Qualitative and Quantitative Analysis of Mycotoxins

Qualitative andQuantitative

Analysis ofMycotoxinsA. Rahmani, S. Jinap, and F. Soleimany

ABSTRACT: Mycotoxin toxicity occurs at very low concentrations, therefore sensitive and reliable methods for theirdetection are required. Consequently, sampling and analysis of mycotoxins is of critical importance because failureto achieve a suitable verified analysis can lead to unacceptable consignments being accepted or satisfactory ship-ments unnecessarily rejected. The general mycotoxin analyses carried out in laboratories are still based on physic-ochemical methods, which are continually improved. Further research in mycotoxin analysis has been establishedin such techniques as screening methods with TLC, GC, HPLC, and LC–MS. In some areas of mycotoxin method de-velopment, immunoaffinity columns and multifunctional columns are good choices as cleanup methods. They areappropriate to displace conventional liquid–liquid partitioning or column chromatography cleanup. On the otherhand, the need for rapid yes/no decisions for exported or imported products has led to a number of new screen-ing methods, mainly, rapid and easy-to-use test kits based on immuno-analytical principles. In view of the fact thatanalytical methods for detecting mycotoxins have become more prevalent, sensitive, and specific, surveillance offoods for mycotoxin contamination has become more commonplace. Reliability of methods and well-defined per-formance characteristics are essential for method validation. This article covers some of the latest activities andprogress in qualitative and quantitative mycotoxin analysis.

IntroductionMycotoxins are secondary metabolites of fungi. Due to the

widespread distribution of fungi in the environment, mycotoxinsare considered to be one of the most important contaminants infoods and feeds. According to the Food and Agriculture Orga-nization (FAO), more than 25% of the world’s agricultural pro-duction is contaminated with mycotoxins, resulting in economiclosses in the grain industry (Cazzaniga and others 2001). Toxiccompounds can contaminate food and feedstuffs and these con-taminated materials may be pathogenic for animals and humans;therefore, one of the most effective measures to protect the publichealth is to establish reasonable regulatory limits of these toxins.Consequently, guidelines regarding the allowed levels of myco-toxins present in food and feed products and in raw materialshave been established by the FAO (FAO 1995).

It is important to develop rapid, sensitive, and reproducibleassays to detect the presence of mycotoxins. The accurate andrapid qualitative and quantitative analysis for mycotoxins hasbeen topic of interest by many researchers. Different analyticalmethods having different sensitivity and accuracy which couldbe used for different purposes have been developed. Commonlyused methods to analyze mycotoxins are thin-layer chromatog-raphy (TLC), high-performance liquid chromatography (HPLC)with UV or fluorescence detection (FD), and enzyme immunoas-says (EIAs). Recently, liquid chromatography–mass spectrometry

MS 20090049 Submitted 1/19/2009, Accepted 4/4/2009. Authors are withCenter of Excellence for Food Safety Research (CEFSR), Faculty of Food Sci-ence and Technology, Univ. Putra Malaysia, 43400 UPM, Serdang, Selangor,Malaysia. Direct inquiries to author Jinap (E-mail: [email protected]).

(LC-MS) and gas chromatography–mass spectrometry (GC-MS)techniques have become accessible for the qualitative and quan-titative determination of mycotoxins.

Although a considerable number of studies have been done,more research on mycotoxin detection is highly needed to pro-vide a sound scientific basis for recommendations for bothpre- and postharvest measures. The Codex Committee on FoodAdditives and Contaminants (CCFAC) has developed codes ofpractice to reduce contamination of food and animal feed withmycotoxins, such as aflatoxins, ochratoxin A (OTA), and patulin(Stuart and Slorach 2002). For public health protection and inter-national trade, more sensitive and accurate analytical methodsfor mycotoxins are needed. Furthermore, there is a concern atnational and international levels to prevent and reduce myco-toxin contamination in food and feedstuffs. This article reviewsthe analytical methods of mycotoxins.

MycotoxinsMycotoxins are toxic substances naturally produced by molds

(fungi) that may contaminate agricultural commodities by grow-ing on them. Despite efforts to control fungal contamination, tox-igenic fungi are everywhere in nature and they can contaminate awide range of agricultural products due to mold infestation bothbefore and after harvest wherever humidity and temperature aresufficient. Thousands of mycotoxins exist, but only a few presentconsiderable food safety hazards. Aspergillus, Fusarium, and Peni-cillium, all known field fungi, are the natural fungal flora asso-ciated with foods. The most prominent mycotoxins are aflatox-ins, deoxynivalenol (DON), zearalenone (ZEA), ochratoxin, fu-monisin, and patulin (Gaag and others 2003). These compounds

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Qualitative and quantitative analysis of mycotoxins . . .

cause adverse health effects such as kidney and liver damage (de-terioration), mutagenic and teratogenic effects, birth defects, andcancers (specially liver cancer) that result in symptoms rangingfrom skin irritation to immuno suppression, neurotoxicity, anddeath (Bennett and Klich 2003). Aflatoxin B1 (AFB1) and fumon-isins are human carcinogens, and patulin is suspected as humancarcinogens. DON and other trichothecenes, as well as AFB1,are likely to exert immunosuppressive effects, and fumonisin B1(FB1) may contribute to neural tube defects. Renal dysfunctiondue to OTA exposure (suspected in Balkan endemic nephropathy)is also a potentially significant problem, especially as this couldexacerbate impaired renal function in individuals with diabetes,a burgeoning worldwide epidemic that is highly likely to grow.There is also uncertainty related to the effects of chronic, low-level, long-term exposure to single and/or multiple mycotoxins,which may be the case even for individuals consuming a diversediet (Lopez-Garcia and others 1999).

The Intl. Agency for Research on Cancer’s (IARC) Monographson the Evaluation of Carcinogenic Risks to Humans and the U.S.Natl. Toxicology program have reviewed hundreds of chemicals,mixtures, and natural products and then graded the cancer riskposed to humans (Abnet 2007). All analytical procedures include3 steps: extraction, purification (if necessary), and determination(Gobel and Lusky 2004; Ren and others 2007).

Analysis of MycotoxinsWith the decrease of restrictive levels of mycotoxins in foods

and feeds defined by the European Union (EU) and other de-veloped countries (EC466 2001; EC472 2002), developmentand validation of more robust analytical methods for the de-termination of mycotoxins are urgently requested. Current an-alytical techniques mainly include fast screening methods andconfirmatory quantification. Standardized methods for aflatox-ins (EN12955 1999; EN14123 2001), ochratoxin A (EN141322003), fumonisins (EN13585 2001; EN14352 2004), and patulin(EN14177 2003) in various foods are available, and methods ofanalysis for trichothecenes in food and various other mycotoxinsin feed are planned to be developed in the near future. A full setof official methods of analysis for mycotoxins has been reportedby Gilbert and Anklam (2002).

SamplingThe obvious reason for sampling of a material is to obtain

a portion for the estimation or observation of attributes of theparticular lot; the sample must be representative of the lot. Basedon the measured sample concentration, some decision is madeabout the edible quality of the bulk lot or the effect of a treatmentor a process on reducing mycotoxins in the lot. Sampling is ageneral requirement for all methods in mycotoxin analysis. Dueto the high heterogeneity of mycotoxins, sampling plans are veryimportant to obtain representative samples (JECFA 2001).

Traditional methods of sampling and sample preparation ofagricultural crops and foodstuffs are usually not adequate formycotoxin analyses because mycotoxin contamination is usuallyheterogeneous, which creates problems in obtaining a represen-tative sample for analysis. Studies on a wide variety of agriculturalproducts such as peanuts and shelled corn indicate that a verysmall percentage (0.1%) of the kernels in the lot is contaminatedand the concentration on a single kernel may be extremely high(Cucullu and others 1966; Johansson and others 2000a).

A common feature of all sampling plans is that the whole pri-mary sample must be ground and mixed so that the analyticaltest portion has the same concentration of toxin as the originalsample. A mycotoxin-sampling plan is defined by a mycotoxintest procedure and a defined accept/reject limit. Sampling for

mycotoxin detection specifies how the sample will be selectedor taken from the bulk lot and the size of the sample. Sampleselection procedures used to take a sample from a bulk lot is ex-tremely important. Every individual item in the lot should have anequal chance of being chosen (called random sampling) (Parkerand others 1982; Hurburgh and Bern 1983).

Two types of mistakes cause inconsistency among mycotoxintest results: First, good lots (in the range of regulatory limits) thatmay be rejected; the so-called sellers’ risk (false-positives). Sec-ond, bad lots (over the regulatory limits) that may be accepted bythe sampling program; the so-called buyers’ risk (false-negatives).A plot of the acceptance probability P(M) compared with the lotconcentration M is called an operating characteristic (OC) curve.As M approaches 0, P(M) approaches 1% or 100%, and as M be-comes large, P(M) approaches zero. The shape of the OC curveis uniquely defined for a particular sampling plan design withdesignated values of sample size, degree of comminution, sub-sample size, analytical method type, number of analyses, andthe accept/reject limit. Increasing the size of a sample decreasesboth the buyers’ and sellers’ risks but it will be very expensive.The best plan will minimize both sellers’ and buyers’ risks (FAO1993; Whitaker and others 1995; EC 1998, 2002; Johansson andothers 2000b, 2000c).

The majority of sampling plans used in the mycotoxins areahave been concerned with the control of aflatoxin concentrationsin peanuts (Whitaker and others 1995), while others have studiedaflatoxins in pistachios (Schatzki 1995), maize (Jewers and others1988), and figs (Sharman and others 1994). Modeling and a sub-sequent simulating study for retail-sampling strategies have beencarried out by MacArthur and others (2006). The number of con-tainers sampled can vary from one-fourth in small lots (less than20 metric tons) to the square root of the total number of contain-ers for large (greater than 20 metric tons) lots (FAO/WHO 2001).The maximum sample result can be 4 to 5 times the lot concen-tration. Therefore, the average of the 10-sample result is the bestestimate of the lot concentration. Furthermore, the distribution ofthe 10-sample result for each lot is not always symmetrical aboutthe lot concentration (Whitaker 2006).

Number of incremental samples to be taken depends on theweight of the lot and kind of food such as cereals and cerealproducts, dried fruits, nuts, and spices that have been tabulatedin EC401/2006. For example in more than 50 tons lot weight ofcereals we need to take 100 incremental samples from sub lotsthat make 10 kg aggregate sample weight; however, for less than50 tons lot weight of cereals we need 3 to 10 incremental samplesdepend on lot weight to make 1- to 10-kg aggregate sample. Theweight of the incremental sample shall be about 300 g in caseof dried figs, groundnuts and nuts. In the case of lots in retailpackings, the weight of the incremental sample depends on theweight of the retail packing (EC401/2006).

The accumulation of many small incremental portions is calleda bulk sample. If the bulk sample is larger than desired, the bulksample should be blended and subdivided until the desired sam-ple size is achieved. The smallest sample size that is subdividedfrom the bulk sample and comminuted in a grinder in the samplepreparation step is called the test sample.

The main economic factors involved with the overall cost of amycotoxin testing program are the cost of sampling, the cost ofsample preparation, the cost for the actual analysis, and in someinstances the cost of sample shipment from the point of samplingto the laboratory that the analysis is performed (Campbell andothers 1986).

Sample preparationExtraction methods. The extraction from a sample depends on

both physicochemical properties of the sample matrix and the

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toxin. Only exceptional methods such as infrared spectroscopictechniques are able to draw data from the ground and homoge-nized sample (Kos and others 2003). In all other cases, the sampleor ground sample should be blended with extraction solvent ina high-speed blender or mechanical shaker. Then the slurry mustbe filtered and will be ready for subsequent purification proce-dures, if necessary. Diatomaceous earth is sometimes includedin the solvent system to enhance the filtration step.

Extraction can be performed by liquid–liquid extraction (LLE)using 2 immiscible liquid-phases or solid phase extraction (SPE)using a solid and a liquid phase. In the extraction step, dependingon the conditions, the analyte (and any compounds with similarproperties) will migrate into the extraction solvent until equilib-rium is established. This way, the desired compounds can beconcentrated in a solvent and interferences can be removed.

In some cases, multiple extractions are necessary for the anal-ysis of mycotoxins. At the end all fractions are pooled for furthertreatment (cleanup). Ideally, the extraction solvent is able to re-move only the mycotoxin of interest from the sample matrix. Dueto the absence of such a completely specific extraction solvent,the solvents chosen are those that can remove as much mycotoxinas possible, while removing as little as possible of any interfer-ing compounds. Also, it should easily be recoverable, nontoxicand nonflammable, and other aspects, such as volatility, stabil-ity, transparency to UV light, and environmental impact of sol-vents are also important. Volatile organic compounds (VOC) maycause ozone depletion for example; previously, chlorofluorocar-bons (CFCs) were the great solvent choice for many market seg-ments due to their effectiveness, low cost, and nonflammability.But today, there are serious restrictions on CFCs and chlorinatedsolvent use due to environmental concerns. Consequently, thesolvent market has changed dramatically over the past decade.Evaluations of extraction techniques for trichothecenes from plantmaterials such as wheat using liquid–liquid extraction (LLE) andSPE procedures have shown that these techniques were compet-itive with those using commercially available high-quality SPEmaterials (Stecher and others 2007). The following are some im-portant methods of extraction.

Liquid extraction. For solid samples like cereals, polar sol-vents can dissolve mycotoxins and extract them from the groundsample. Water is a polar solvent that can be used for extractionof some mycotoxins such as DON (Lisa and others 1999). Po-lar analytes favor polar solvents and pH plays a key role duringextraction. Solvent extraction is also a useful technique for theanalysis of liquid samples. Examples of the use of this techniqueinclude the analysis of aflatoxin M1 in milk (Cavaliere and others2006). The most efficient solvents that have been used for extract-ing mycotoxins are the relatively polar solvents, such as methanol(Juan and others 2005), acetone, acetonitrile (Hinojo and others2006), ethyl acetate, diethyl ether (Hayashi and Yoshizawa 2005),toluene (Sangare-Tigori and others 2006), and chloroform (Saezand others 2004; Ferracane and others 2007), or mixtures of them(Zinedine and others 2006). Small amounts of water will wet thesubstrate and offer higher extraction efficiencies, by increasingpenetration of the solvent (mixture) into the hydrophilic material(Hinojo and others 2006). An acid solution as the aqueous phasecan help the extraction process by breaking interactions betweenthe toxins and sample constituents such as proteins. For exam-ple, Dunne and others (1993) have described a multi-mycotoxinmethod which used hydrochloric acid and dichloromethane forthe extraction of mycotoxins from animal feed. Whereas Barna-Vetro and others (1996) used dichloromethane/citric acid for theextraction of ochratoxin A from cereals and Monbaliu and oth-ers (2009) used ethyl acetate/formic acid for multiextraction oftrichothecenes from sweet pepper. Also, formic acid has beenreported as a good aid for simultaneous extraction of fumonisins

from maize (Zitomer and others 2008). On the other hand, inanother study on co-occurrence of ochratoxin A and aflatoxinB1 in dried figs, higher toxin recovery was reported when al-kaline extraction was used instead of conventionally acidic ex-traction (Senyuva and others 2005). Recently, Reddy and others(2009) used 0.5% KCl in 70% methanol for the extraction afla-toxin B1 from rice before using enzyme-linked immunosorbentassay (ELISA) for mycotoxin detection.

Solid phase extraction. One of the most significant recent im-provements in the purification step is the use of SPE. Test extractsare cleaned up before instrumental analysis (thin-layer or liquidchromatography) to remove co-extracted materials that often in-terfere with the determination of target analytes.

SPE based on molecularly imprinted polymers is an intriguingconcept for specific sample preparation and pre-concentrationand it has been gaining increased interest in the fields of en-vironmental, clinical, and food/beverage analysis. Synthetic re-ceptors for the mycotoxins such as aflatoxin (Egner and others2006), OTA (Stander and others 2000; Jodlbauer and others 2002;Sibanda and others 2002), DON, and ZEA (Weiss and others2003) have been reported for use in solid phase extraction usingthe noncovalent self-assembly imprinting approach. SPE, espe-cially combined polar and nonpolar materials, becomes a pre-ferred technique as a selective and time-saving sample cleanuptechnique enabling almost complete removal of possibly interfer-ing matrices (Stecher and others 2007). Using an SPE cartridgethat contained a polymeric sorbent, aflatoxins B1, G1, B2, G2,and ochratoxin A, were extracted in 1 step (Ventura and others2006; Ferracane and others 2007).

SPE of wine and beer ochratoxin A has been carried out ona C18 cartridge to achieve a 100-fold sample concentration forGC–MS extraction in dichloromethane and derivatization withbis [trimethylsilyl] trifluoroacetamide (Soleas and others 2001).Instead of off-line SPE, online SPE has been introduced and wasable to offer a series of advantages. The use of online SPE tech-niques has made possible the development of faster methodsby reducing the sample preparation time and thus increasingthe sample throughput. Conditioning, washing, and elution stepscan be performed automatically and some systems also permitto extract 1 sample while another one is being analyzed by LC(Rodriguez-Mozaz and others 2007).

Accelerated solvent extraction (ASE). In ASE, solvents areused at relatively high pressure and temperatures at or abovethe boiling point. In this case, parameters like temperature, pres-sure, static time, cell size, and solvent used are very important(Adou and others 2001; Salces and others 2001; Gentili and oth-ers 2004). In this method, a solid sample is placed and sealed ina cell after being filled with an extraction solvent. At static condi-tions, the fluid is held in the cell under elevated temperature andpressure for short periods, then fresh solvent is flushed throughthe cell and compressed gas is used to purge the sample extractfrom the cell into a collection vessel. The high temperature andpressure cause the solvent to be in the liquid state, therefore fastextraction can be achieved (Richter and others 1996). As an ex-ample, Juan and others (2005) used ASE (at 1500 psi, 40 ◦C,and 5 min) with methanol for extraction of ochratoxin A fromrice. A rapid and simple supercritical fluid extraction method hasbeen used for the direct screening of macrocyclic lactone myco-toxins (zearalenone and its derivatives), in maize flour samples,by continuous-flow electrochemical detection after cleanup ona Florisil adsorption cartridge (Zougagh and Rios 2008). Furtherstudies to improve mycotoxin extraction of foods and feedstuffsare still needed.

Cleanup methods. Cleanup of sample is the removal of sub-stances in the sample extract that may interfere with the detectionof the analyte. As a large number of interfering compounds such

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as pigments originally are present in a sample, the primary sam-ple extracts must be cleaned-up in some determination methodsto get more accurate and precise results. A variety of cleanupmethods have been used.

There are a few ways to remove such additional compounds.As an example, for high levels of lipids present in certain com-modities (nuts, cereals), which would interfere with subsequentanalytical procedures, nonpolar solvents such as hexane can beincluded in the original solvent system, or they can be addedafter the homogenization and filtration steps to remove lipidconstituents. Primary extracts in mixtures of acetone with wa-ter contain proteins that can be precipitated with lead acetate.Sometimes various pigments need to be removed from primaryextracts. Cleanup methods which include extract application, awashing step, and application of chromogenic substrate havebeen carried out for cleanup of OTA from high-colored matri-ces such as licorice, ginger, nutmeg, black pepper, white pepper,and Capsicum spp. For spices, tandem immunoassay columnscoupled with simple methanol-based extraction have been used(Goryacheva and others 2007a).

Most of the rapid methods based on immunochemical tech-niques usually do not require any further cleanup or analyte-enrichment steps. Thus, the diluted extracts can be used directlyfor immune-analytical methods, such as ELISA (Barna-Vetro andothers 1997; Krska and Molinelli 2007). Also, there are somemycotoxin determination method with LC–MS/MS, which didnot use cleanup (Delmulle and others 2006).

Liquid–liquid partitioning, SPE, column chromatography,immunoaffinity columns (IAC), and multifunctional cleanupcolumns can be used for the purification of extracts in myco-toxin analysis prior to instrumental analysis.

Liquid–liquid separation. Formerly, liquid–liquid partitioningwas employed to remove unwanted matrix components in thesample extract. It is based on the partition between immisci-ble solvents, one of which contains the analyte. Hayashi andYoshizawa (2005) used diethyl ether for the cleanup of corn andrice. The analyte then migrates into the other phase until equilib-rium has been reached. This step can be performed several timeswith fresh solvent to extract the analyte quantitatively, for exam-ple, the determination of aflatoxin G1 in maize (Castegnaro andothers 2006). Although the method is simple and easy to perform,it is used less frequently nowadays because it is time-consuming,labor-intensive, and large volumes of solvent are required.

Solid phase extraction (SPE). An SPE technique is based onpartitioning of analytes and interfering compounds between amobile and a stationary phase. The stationary phase, containedwithin the cartridge, is composed of a solid adsorbent or animmobilized (bonded) liquid phase. Available bound phases in-clude ethyl (C2), octyl (C8), octadecyl (C18), cyclohexyl (CH),phenyl (PH) cyanopropyl (CN), diol (2OH), aminopropyl (NH2),and a selection of ion exchange phases. C18 is the most prac-tical SPE column for mycotoxin detection (Medina and others2004; Saez and others 2004). SPE is a more rapid, efficient, re-producible, and safer method than the traditional liquid–liquidextraction techniques and offers a wide range of selectivity.

Three different applications have been reported for the SPEprocess: sample cleanup, sample concentration, and matrix re-moval. In the sample cleanup mode, the SPE column retains themycotoxin and allows impurities to pass through the column. Inthe sample concentration mode, large sample volumes are passedthrough the column and the retained mycotoxin is concentratedby eluting it with a small volume of solvent. In the matrix removalmode, it is used to retain interfering impurities and the mycotoxinis allowed to pass through the column (Betina 1993).

A typical SPE sequence starts with a conditioning step (namely,activating it with solvent). Then the aqueous sample extract is

applied to the conditioned column and the analyte is trappedtogether with the matrix. After that, a rinsing step removes matrixcompounds and, finally, the analyte is eluted from the columnwith an organic solvent and a further preconcentration step isemployed by evaporating excess solvent with nitrogen gas.

Ion-exchange columns. Ion-exchange mechanisms are an-other kind of cleanup that are employed, if the analyte canbe made present as an ion (such as moniliformin, MON). An-ionic compounds isolate on strong anion exchange-bonded silicacolumns. The retention is based on the electrostatic attraction ofa charged functional group of the analyte to the charged groupon the silica surface of the column. To elute the analyte thebond to the sorbent must be broken. The electrostatic force isdisrupted and the compound is eluted. Alternatively, a solutionwith high ionic strength is used for elution because of its higheraffinity to the sorbent. It is important to note that the packingshould not dry up between conditioning and sample additionand that, after regeneration, columns can be used again severaltimes. SAX columns can be used for the determination of ochra-toxin A and fumonisin (Betina 1993). In a recent study on themulti-mycotoxin detection of sweet pepper using LC–MS–MS, astrong anion-exchange column was used for cleanup of one splitof extract while the other split was cleaned up by an aminopropylcolumn followed by an octadecyl column (Monbaliu and others2009).

Immunoaffinity columns. Immunoaffinity columns (IACs) forcleanup purposes have become increasingly popular in recentyears because they offer high selectivity (Cahill and others 1999;Abdulkadar and others 2004; Danicke and others 2004; Saezand others 2004; Zinedine and others 2006; Calleri and others2007). They are easy to use for purification of samples which arecontaminated with different mycotoxins. The analyte molecules(the mycotoxins) are bound selectively to the antibodies on thecolumn after a preconditioning step. As matrix components donot interact with the antibodies, a rinsing step removes most ofthe possible interferences and the toxin can be eluted by antibodydenaturation.

IACs feature a higher recovery than standard liquid–liquid par-titioning. There are also commercially available columns for theaflatoxins, fumonisins, and type A and B trichothecenes such asDON and OTA that are used in some experiments; the methodhas been used for cleanup of aflatoxins (B1, B2, G1, and G2),patulin, and ergosterol in dried figs (Karaca and Nas 2006). Se-lectivity of the IAC cleanup was proven by comparison withnonspecific solid phase extraction using octadecylsilica (ODS)sorbent (Mhadhb and others 2006). Regeneration of IACs forreuse in aflatoxin, ochratoxin A, fumonisin, and zearalenoneanalyses has been investigated by (Scott and Trucksess 1997).Columns are prepared by binding antibodies specific for a givenmycotoxin to a specially activated solid phase support and pack-ing the support suspended in aqueous buffer solution into a car-tridge. The mycotoxin in the extract or fluid binds to the antibody,while impurities are removed with water or aqueous solution; andthen the mycotoxin is desorbed with a miscible solvent such asmethanol.

There are many experiments on comparison of IAC to othermethods like SPE (Hu and others 2006) and comparison of differ-ent kinds of IACs. A study of Trucksess and others (2006) showed80% recovery for aflatoxin IAC and 70% by multifunction afla-ochra IAC. Cleanup using IAC was more sensitive than a Mycosepmultifunctional column (MFC) for milk samples (Chen and oth-ers 2005). IAC is a well-known method for cleanup and enrich-ment techniques. The Association of Official Analytical Chemistsand the European Union have validated methods which addresscleanup of few food commodities using conventional and IACapproaches (Scott and Trucksess 1997; Castegnaro and others



2006); however, in some studies SPE was preferred because withlarge amounts of mycotoxins these levels would surpass the ca-pacity of IAC columns (Hinojo and others 2006). Using IACs, evensmall amounts of mycotoxins can be detected with confidence.Visconti and others (1999) stated that the use of immunoaffin-ity chromatography in the purification step provides a numberof advantages over conventional methods, such as clean extractsdue to the high specificity of the antibodies for one toxin or agroup of related toxins, high precision and accuracy over a wideconcentration range of interest, rapidity of the purification step,and reduction in the use of hazardous solvents.

Multifunctional columns for the simultaneous determinationof OTA and ZEA are also available. Wang and others (2008)used AOZ multitoxin method detection based on HPLC in thedetermination of 6 kinds of mycotoxins (aflatoxins B1, B2, G1,and G2, OTA, and ZEA) of air samples. The fact that columnscan only be used once and their relative high costs are majordisadvantages. Columns are commercially available.

MycosepTM columns. Rapid multifunctional Mycosepcolumns remove matrix components efficiently and can producea purified extract within a very short time. The Mycosep multi-functional cleanup columns consist of adsorbents such as char-coal, celite, polymers, and ion-exchange resins which are packedin a plastic tube and used to remove the entire matrix leaving thedesired compound in solution on top of the column (Akiyamaand others 2001; Mateo and others 2002). A rubber flange, aporous frit, and a 1-way valve on the lower end ensure that theextract is forced through the packing material when the columnis inserted into the culture tube. On top of the plastic tube, thepurified extract appears within seconds. Large molecules, pro-teins, fats, carbohydrates, and pigments are all adsorbed on thesolid phase.

Columns are usually suitable for one analyte only, such as My-cosep 229 Ochra column for the determination of OTA (Buttingerand others 2003, 2004) and DON in maize and wheat, and ZEAin maize (Krska and others 2005), and for a range of mycotoxinssuch as DON and other A- and B-trichothecenes (Weingartnerand others 1997).

Qualitative and Quantitative AnalysisSurveillance of foods for mycotoxin contamination has become

more common since analytical methods for detecting mycotox-ins have become more widespread. A mycotoxin analysis methodshould be simple, rapid, robust, accurate, and selective to enablesimultaneous determination. Above all, low tolerance levels infeed and food require sensitive methods. The analytical resultshave to be fit for the purpose and the method has to be chosenaccordingly. Analytical methods for the determination of myco-toxins commonly have the following steps: sampling, homoge-nization, extraction, and cleanup which might include sampleconcentration. The final separation and detection of compoundsof interest is usually achieved by either chromatographic tech-niques followed by various detection methods or by immuno-chemical methods. While immunochemical methods rely onspecific antibodies for each mycotoxin, chromatographic tech-niques can separate a huge number of analytes.

HPLC has become the main method for mycotoxin analysis.Coupled with a variety of detectors, practically all mycotoxinshave been separated and detected by HPLC. Fumonisins, aflatox-ins, ZEA, and OTA are routinely analyzed by HPLC (Shephard1998; Coker 2000).

There are some reports of validated methods for the analysis ofmycotoxins, such as DON, T2 toxin and HT-2 toxin in cereals bygas chromatographic (GC) methods coupled with flame ioniza-tion detector (FID) and mass spectrometry (MS) (Eskola and others

(a) (b) (c) (d)(e) (f)(g) (h)

1930 1980 1990 2000 2010

Figure 1 --- Historical perspective of analytical methods intoxin detection (Hawkins 2005).

2001; Krska and others 2001; Eke and others 2004; Melchert andPabel 2004). An European Committee (EC)-funded project withinthe framework of the SMT-programme was organized by Petters-son and Langseth (2002), in which gas chromatographic methodsfor nivalenol, DON, HT-2, and T-2 toxin were assessed. However,several method problems were identified in that study: higher tri-chothecene response for calibrants in the presence of matrix thanfor pure calibrants, nonlinear calibration curves, drifting responsefor trichothecenes, and carry-over or memory effects from previ-ous samples and matrix interference.

Nowadays, ELISAs (enzyme linked immuno-sorbent assays)have also become widespread in mycotoxin determination. Testkits are available for practically all relevant mycotoxins. Not onlycleanup methods are continuously optimized, but also instru-mental methods.

HPLC–MS/MS has become the most rising analytical tool forthe determination of mycotoxins and their metabolites (Berthillerand others 2007; Spanjer and others 2008). In contrast to GC-based methods, polar compounds are quickly reachable withoutthe need of derivatization. Further advantages include low de-tection limits, the ability to generate structural information of theanalytes, the minimal requirement of sample treatment, and thepossibility to cover a wide range of analytes differing in their po-larities. Finally, mass spectrometers are rather general detectorsthat are not so dependent on chemical characteristics like UVabsorbance or fluorescence.

There are many different methods that have been developed formycotoxin detection: (a) TLC, (b) mouse bioassay, (c) HPLC andGC, (d) protein phosphatase inhibition, (e) HPLC/MS, GC/MS, (f)ELISA, (g) HPLC/MS-MS, (h) PCR (see Figure 1). Summary of someanalytical methods have been tabulated in Table 1.

Colorimetric techniqueFurther separation in mycotoxin detection can be performed

with IAC, followed by liquid chromatographic (LC) quantitation,either off-line or online in an automated system, or by fluorom-etry. Some mycotoxins like aflatoxins, ochratoxins, and citrininhave a conjugated, planar structure that gives them natural flu-orescence ability, which makes it feasible for qualitative andquantitative determination using a fluorometer. Commercial IAC,Aflatest P, is used as the cleanup step in an LC method and in asolution-fluorometry method for corn, peanuts, and peanut but-ter that was adopted as an AOAC Intl. Official Method (Tranthamand Wilson 1984; Scott and Trucksess 1997).

A comparative study of 3 different methods using HPLC, fluo-rometry, and ELISA for the determination of aflatoxins in sesamebutter has been carried out by Nilufer and Boyacioglu (2002).In this study, an immunoaffinity column was used for cleanupand purification of extracts prior to detection by HPLC and flu-orometry. The fluorometric determination method was found tobe highly correlated with the HPLC method (r = 0.978). Bothfluorometry and ELISA methods had high recoveries and lowvariance (Nilufer and Boyacioglu 2002). In addition, this tech-nique allows the high throughput analysis of a large number ofindustrial samples for automation by means of a microplate sys-tem. However, this analysis procedure is one semiquantitative,although it is rapid analysis and low cost for analyzing a largenumber of samples.



Ta

ble

1---

Mu

ltim

yco

tox

ind

ete

cti

on

.

Qu

anti

fica

tio

nT

ype

of

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icle

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eren

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tern

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ns

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rom

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raph

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mas

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met

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for

swee

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per

anal

ysis

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idC

omm

unM

ass

Spe

ctro

m23

(1):

3–11

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toxi

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mpe

titiv

eE

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AR

ice

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dyan

dot

hers

Det

ectio

nof

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ergi

llus

spp.

and

aflat

oxin

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biol

ogy

26:2

7–31

2009

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onis

ins

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idch

rom

atog

raph

y(L

C)

with

fluor

esce

nce

(FD

)an

dm

ass

spec

trom

etry

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tect

ors

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hers

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lysi

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ased

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and

mas

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omet

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istr

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ages

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min

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othe

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ould

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doc

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oxin

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aces

ofar

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din

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dM

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biol

ogy

26:6

5–70

2009

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ugh

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bala

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ess

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ysis

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upda

tefo

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ldM

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nal2

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3–21

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plin

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Det

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):32

1–32

5

2009

Con

tinue

d


CRFSFS: Comprehensive Reviews in Food Science and Food SafetyT

ab

le1

---C

on

tin

ue

d.

Qu

anti

fica

tio

nT

ype

of

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sm

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icle

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eren

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ear

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ter

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ame

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te

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gric

.Foo

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hem

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(9):

3519

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09

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mat

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tran

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atio

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raph

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ithflu

ores

cenc

ede

tect

ion

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hrom

atog

rA

1187

(1-2

):14

5–50

2008

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nsB

1,B

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dG

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hrat

oxin

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titox

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mun

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mn

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eter

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atio

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nalo

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AC

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rnat

iona

l91

(3):

511–

523

2008

Con

tinue

d


Qualitative and quantitative analysis of mycotoxins . . .T

ab

le1

---C

on

tin

ue

d.

Qu

anti

fica

tio

nT

ype

of

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oto

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eth

od

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uth

or

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icle

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eren

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ear

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irect

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t71

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3):1

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figs

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tam

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):47

2–89

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n,pa

tulin

,and

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A

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idch

rom

atog

raph

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mbi

ned

with

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of-fl

ight

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C-T

OF

-MS

)

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ied

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uid

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mat

ogra

phy-

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ight

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ry

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mat

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met

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for

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rmat

ion

JC

hrom

atog

rA

1177

(1):

50–7

2008

T-2

and

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ebst

ein

and

othe

rsD

eter

min

atio

nof

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ince

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sin

clud

ing

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byliq

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mat

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phy

and

fluor

esce

nce

dete

ctio

n

JA

gric

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dC

hem

56(1

3):4

968–

4975

2008

Con

tinue

d



Ta

ble

1---

Co

nti

nu

ed

.

Qu

anti

fica

tio

nT

ype

of

Myc

oto

xin

sm

eth

od

foo

dA

uth

or

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icle

Ref

eren

ceY

ear

Fum

onis

ins

LC-M

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SM

aize

Zito

mer

and

othe

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sing

leex

trac

tion

met

hod

for

the

anal

ysis

byliq

uid

chro

mat

ogra

phy/

tand

emm

ass

spec

trom

etry

offu

mon

isin

san

dbi

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kers

ofdi

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ted

sphi

ngol

ipid

met

abol

ism

intis

sues

ofm

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lBio

anal

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m39

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08

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gan

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-per

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y

Env

iron

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2):1

39–4

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08

For

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ntam

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tect

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with

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ater

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omet

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pes

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and

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apid

mul

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ysis

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gA

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and

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ttro

Pre

mie

rX

E

Wat

ers

App

licat

ions

Not

e20

07V

olum

e:P

age:

5pp

2007

Afla

toxi

ns,o

chra

toxi

n,fu

mon

isin

s,tr

icho

thec

enes

Trop

ical

cere

als

Mag

anan

dA

ldre

dP

osth

arve

stco

ntro

lstr

ateg

ies:

Min

imiz

ing

myc

otox

ins

inth

efo

odch

ain.

IntJ

Foo

dM

icro

biol

2007

Jul3

120

07

Afla

toxi

ns,o

chra

toxi

nA

,fum

onis

ins,

deox

yniv

alen

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dze

aral

enon

e.

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rain

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ulle

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and

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nchi

niS

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lity

ofm

ycot

oxin

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ring

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proc

essi

ngIn

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ood

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robi

ol20

07Ju

l31

2007

Afla

toxi

nsH

PLC

aflat

oxin

sw

ere

quan

tified

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PLC

equi

pped

with

aC

18co

lum

n,a

phot

oche

mic

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acto

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da

fluor

esce

nce

dete

ctor

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icul

tura

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mm

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ple

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ple,

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d,an

din

expe

nsiv

ecl

eanu

pm

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atio

nof

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sin

impo

rtan

tagr

icul

tura

lpr

oduc

tsby

HP

LC

JA

gric

Foo

dC

hem

2007

;55:

2136

–41

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rato

xin

A(O

TA)

and

4-de

oxyn

ival

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(DO

N)

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ults

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cefr

omth

eda

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ther

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gium

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arcz

and

othe

rsIn

take

ofoc

hrat

oxin

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dde

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ival

enol

thro

ugh

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cons

umpt

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inB

elgi

um

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ddit

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tam

,A

ugus

t200

7;24

(8):

910–

6

2007

Sim

ulta

neou

ses

timat

ion

ofafl

atox

inB

(1)

[AF

B(1

)]an

doc

hrat

oxin

A(O

A)

Mem

bran

e-ba

sed

imm

unoa

ssay

cons

istin

gof

am

embr

ane

with

imm

obili

zed

anti-

AF

B(1

)an

dan

ti-O

Aan

tibod

ies

and

afil

ter

pape

rat

tach

edto

apo

lyet

hyle

neca

rdbe

low

the

mem

bran

e

Chi

lisa

mpl

esS

aha

and

othe

rsS

imul

tane

ous

enzy

me

imm

unoa

ssay

for

the

scre

enin

gof

aflat

oxin

B(1

)an

doc

hrat

oxin

Ain

chili

sam

ples

Ana

lChi

mA

cta

2007

Feb

19;

584(

2):3

43–9

2007

Cer

eal

Ber

thill

eran

dot

hers

Chr

omat

ogra

phic

met

hods

for

the

sim

ulta

neou

sde

term

inat

ion

ofm

ycot

oxin

san

dth

eir

conj

ugat

esin

cere

als

IntJ

Foo

dM

icro

biol

2007

Jul3

120

07

Con

tinue

d



Ta

ble

1---

Co

nti

nu

ed

.

Qu

anti

fica

tio

nT

ype

of

Myc

oto

xin

sm

eth

od

foo

dA

uth

or

Art

icle

Ref

eren

ceY

ear

Sim

ulta

neou

safl

atox

ins

(B(1

),B

(2),

G(1

),G

(2))

,och

rato

xin

A,

fum

onis

ins

(B(1

),B

(2))

,de

oxyn

ival

enol

,ze

aral

enon

e,T-

2an

dH

T-2

toxi

ns

Liqu

idch

rom

atog

raph

y/ta

ndem

mas

ssp

ectr

omet

ry-r

ever

sed-

phas

eliq

uid

chro

mat

ogra

phy

coup

led

with

elec

tros

pray

ioni

zatio

ntr

iple

quad

rupo

lem

ass

spec

trom

etry

(LC

/ES

I-M

S/M

S)

usin

g,as

chro

mat

ogra

phic

mob

ileph

ase,

Mai

zeLa

ttanz

ioan

dot

hers

Sim

ulta

neou

sde

term

inat

ion

ofafl

atox

ins,

ochr

atox

inA

and

Fus

ariu

mto

xins

inm

aize

byliq

uid

chro

mat

ogra

phy/

tand

emm

ass

spec

trom

etry

afte

rm

ultit

oxin

imm

unoa

ffini

tycl

eanu

p

Rap

idC

omm

unM

ass

Spe

ctro

m20

07S

ep10

;21(

20):

3253

–61

2007

Afla

toxi

nsafl

atox

ins

(B1,

B2,

G1,

and

G2)

Enz

yme-

linke

dim

mun

osor

bent

assa

y(E

LIS

A).

Ric

ear

tifici

ally

cont

amin

ated

hull,

bran

,pol

ishe

dbr

oken

grai

ns,a

ndpo

lishe

dw

hole

kern

els)

Cas

tells

and

othe

rsD

istr

ibut

ion

ofto

tala

flato

xins

inm

illed

frac

tions

ofhu

lled

rice

JA

gric

Foo

dC

hem

2007

;55:

2760

–420

07

Sim

ulta

neou

sly

aflat

oxin

s,ty

peA

tric

hoth

ecen

es,t

ype

Btr

icho

thec

enes

,O

TA,z

eara

leno

ne,

fum

onis

ins,

and

patu

lin

Com

preh

ensi

veLC

/MS

/MS

ina

sing

leru

nA

naly

sis

ofco

rnfla

keex

trac

tsR

udra

bhat

laan

dot

hers

Mul

ticom

pone

ntm

ycot

oxin

anal

ysis

byLC

/MS

/MS

The

10th

annu

alm

eetin

gof

the

Isra

elA

naly

tical

Che

mis

try

Soc

iety

Con

fere

nce

&E

xhib

ition

,Jan

uary

23–4

2007

Sim

ulta

neou

sly

mea

sure

myc

otox

ins

(NIV

),(D

ON

),A

FG

1,A

FG

2,A

FB

1,A

FB

2,F

B1,

FB

2,D

iace

toxy

scrip

enol

(DA

S),

T2-

Toxi

ne,

Och

rato

xin

A,a

ndZ

EN

LC–M

S/M

Sm

etho

dH

PLC

(The

rmo

Sci

entifi

c,S

anJo

se,C

alif)

.

Cat

tleF

orag

esan

dF

ood

Mat

rices

Hul

san

dot

hers

Ana

lysi

sof

myc

otox

ins

inva

rious

cattl

efo

rage

san

dfo

odm

atric

esw

ithth

eT

SQ

Qua

ntum

Dis

cove

ryM

AX

30M

ass

spec

trom

etry

adve

rtis

ing

supp

lem

entt

heap

plic

atio

nno

tebo

okM

arch

2007

2007

Red

uced

upto

88%

aflat

oxin

B1,

44%

zear

alen

one,

and

29%

for

fum

onis

ins

ochr

atox

in.S

tand

ard

Q/F

ISw

asin

effe

ctiv

ein

redu

cing

DO

Nup

take

Ava

ntag

giat

oan

dot

hers

Ass

essm

ento

fthe

mul

ti-m

ycot

oxin

-bin

ding

effic

acy

ofa

carb

on/

alum

inos

ilica

te-b

ased

prod

ucti

nan

invi

tro

gast

roin

test

inal

mod

el

JA

gric

Foo

dC

hem

2007

May

1920

07

Con

tinue

d



ab

le1

---C

on

tin

ue

d.

Qu

anti

fica

tio

nT

ype

of

Myc

oto

xin

sm

eth

od

foo

dA

uth

or

Art

icle

Ref

eren

ceY

ear

AfB

1,B

2,G

1,G

2,M

1,tr

icho

thec

enes

,DO

Ndi

acet

oxys

cirp

enol

,T-

2to

xin

and

HT-

2to

xin)

,FB

1,B

2,B

3,ag

aric

acid

,erg

otal

kalo

ids,

OTA

,ZE

Apa

tulin

,pho

mop

sins

,st

erig

mat

ocys

tin,

Rev

iew

van

Egm

ond

and

othe

rsR

egul

atio

nsre

latin

gto

myc

otox

ins

info

od:

Per

spec

tives

ina

glob

alan

dE

urop

ean

cont

ext

Ana

lBio

anal

Che

m20

07M

ay17

2007

DO

N,Z

EN

,and

fum

onis

ins

B1

and

B2

(FB

1,F

B2)

HP

LCsy

stem

cons

iste

dof

aP

1000

XR

pum

pH

PLC

–MS

/MS

syst

em.

Cor

nsi

lage

Nid

erko

rnan

dot

hers

Scr

eeni

ngof

ferm

enta

tive

bact

eria

for

thei

rab

ility

tobi

ndan

dbi

otra

nsfo

rmde

oxyn

ival

enol

,ze

aral

enon

ean

dfu

mon

isin

sin

anin

vitr

osi

mul

ated

corn

sila

gem

odel

Foo

dA

ddit

Con

tam

,A

pril

2007

;24

(4):

406–

15

2007

Fum

onis

ins

(FB

1an

dF

B2)

also

anal

yzed

for

aflat

oxin

s(B

1,B

2,G

1,an

dG

2)on

eby

one

FB

1F

B2:

HP

LC/fl

uore

scen

cefo

llow

ing

naph

thal

ene-

2,3

dica

rbox

alde

hyde

(ND

A)

deriv

atiz

atio

nA

Fs

onT

LC)

plat

eun

derU

Vlig

ht

Diff

eren

tcor

n-ba

sed

food

prod

ucts

Cal

das

and

Silv

aM

ycot

oxin

sin

corn

-bas

edfo

odpr

oduc

tsco

nsum

edin

Bra

zil:

anex

posu

reas

sess

men

tfor

fum

onis

ins

JA

gric

Foo

dC

hem

55(1

9):7

974–

8020

07

Afla

toxi

nan

doc

hrat

oxin

Opt

ical

wav

egui

delig

htm

ode

spec

tros

copy

(OW

LS)

tech

niqu

ein

com

petit

ive

and

indi

rect

imm

unoa

ssay

s.

Bar

ley

and

whe

atflo

urA

dany

iand

othe

rsD

evel

opm

ento

fim

mun

osen

sor

base

don

OW

LSte

chni

que

for

dete

rmin

ing

aflat

oxin

B1

and

ochr

atox

inA

Bio

sens

Bio

elec

tron

2007

;22:

797–

802

2007

Afla

toxi

nB

1H

PLC

CIM

disk

was

coup

led

thro

ugh

asw

itchi

ngva

lve

toa

reve

rsed

-pha

seco

lum

n,na

mel

y,C

hrom

olith

Per

form

ance

RP

-18e

.Afu

llyau

tom

ated

HP

LCflu

ores

cenc

ede

tect

ion

Cal

leri

and

othe

rsD

evel

opm

enta

ndin

tegr

atio

nof

anim

mun

oaffi

nity

mon

olith

icdi

skfo

rth

eon

line

solid

phas

eex

trac

tion

and

HP

LCde

term

inat

ion

with

fluor

esce

nce

dete

ctio

nof

aflat

oxin

B1

inaq

ueou

sso

lutio

ns

JP

harm

aB

iom

edA

nal

2007

;44:

396–

403

2007

Ext

ende

dm

ulti-

myc

otox

inm

etho

d,fo

r25

cont

amin

ants

Sep

arat

ion

and

dete

ctio

nw

itha

Wat

ers

Qua

ttro

Pre

mie

rX

Eta

ndem

quad

rupo

lem

ass

spec

trom

eter

Ava

riety

ofsa

mpl

ety

pes

Kok

and

othe

rsR

apid

mul

ti-m

ycot

oxin

anal

ysis

usin

gA

CQ

UIT

YU

PLC

and

Qua

ttro

Pre

mie

rX

E

Wat

ers

App

licat

ions

Not

e20

07,P

age:

5pp

2007

Afla

toxi

nB

i(A

FB

i)H

PLC

isoc

ratic

reve

rse-

phas

eliq

uid

chro

mat

ogra

phy

(HP

LC)

usin

ga

LiC

hros

pher

100

RP

-18

(5m

mco

lum

n25

×4.

6m

mi.d

.)E

coP

ack

(Mer

ck,P

ortu

gal),

with

post

colu

mn

deriv

atis

atio

nco

nfirm

byT

LC

Cat

tlefe

edco

llect

edfr

om7

dair

yco

w’s

farm

sfr

omP

ortu

gal

Mar

tins

and

othe

rsO

ccur

renc

eof

aflat

oxin

Bii

nda

iry

cow

’sfe

edov

er10

yin

Por

tuga

l(19

95to

2004

)

Rev

Iber

oam

Mic

ol20

07;2

4:69

–71

2007

Con

tinue

d



ab

le1

---C

on

tin

ue

d.

Qu

anti

fica

tio

nT

ype

of

Myc

oto

xin

sm

eth

od

foo

dA

uth

or

Art

icle

Ref

eren

ceY

ear

Afla

toxi

nB

1,c

itrin

in,

deox

yniv

alen

ol,

fum

onis

inB

1,

glio

toxi

n,oc

hrat

oxin

A,a

ndze

aral

enon

e

HP

LC–M

S,Z

orba

xS

B-C

18co

lum

n(A

gile

ntTe

chno

logi

es,P

alo

Alto

,U

SA

)w

itha

1m

mO

ptig

uard

C18

prec

olum

n.M

ass

spec

trom

etry

was

perf

orm

edon

aqu

adru

pole

anal

yser

equi

pped

with

elec

tron

spra

yio

niza

tion

(ES

I).

Cor

nsi

lage

Ric

hard

and

othe

rsTo

xige

nic

fung

iand

myc

otox

ins

inm

atur

eco

rnsi

lage

Ava

ilabl

eon

line

22Ju

ne20

0720

07

Och

rato

xin

A(O

TA)

Imm

unoa

ssay

Hig

h-co

lore

dm

atric

esliq

uoric

e,gi

nger

,nu

tmeg

,bla

ckpe

pper

,whi

tepe

pper

Cap

sicu

msp

p.sp

ices

Gor

yach

eva

and

othe

rsR

apid

all-i

n-on

eth

ree-

step

imm

unoa

ssay

for

non-

inst

rum

enta

ldet

ectio

nof

ochr

atox

inA

inhi

gh-c

olou

red

herb

san

dsp

ices

Tala

nta

Vol

ume

72,

Issu

e3,

15M

ay20

07,P

ages

1230

–34

2007

Fus

ariu

mto

xins

fum

onis

ins

(FB

s),

mon

ilifo

rmin

(MO

N),

zear

alen

one

(ZE

A),

and

type

-Aan

d-B

tric

hoth

ecen

es

HP

LCor

GC

inco

mbi

natio

nw

itha

varie

tyof

dete

ctor

sS

cree

ning

myc

otox

ins

ispe

rfor

med

by(T

LC)

ELI

SA

Fee

dsK

rska

and

othe

rsA

naly

sis

ofF

usar

ium

toxi

nsin

feed

Ani

mal

Fee

dS

cien

cean

dTe

chno

logy

137(

3-4)

:241

–64

2007

Afla

toxi

nB

1,c

itrin

in,

deox

yniv

alen

ol,

fum

onis

inB

1,

glio

toxi

n,O

TAan

dze

aral

enon

e

Hig

h-pe

rfor

man

celiq

uid

chro

mat

ogra

phy

coup

led

tom

ass

spec

trom

etry

(HP

LC–M

S)

Cor

nsi

lage

Toxi

geni

cfu

ngia

ndm

ycot

oxin

sin

mat

ure

corn

sila

ge

2007

Afla

toxi

ns;o

chra

toxi

ns;

fum

onis

ins,

deox

yniv

alen

ol;

zear

alen

one

Ana

lyze

dby

HP

LCoc

hrat

oxin

Aan

dafl

atox

inB

1w

aspe

rfor

med

usin

ga

reve

rsed

phas

eS

ymm

etry

C18

colu

mn

(15

cm_

4.6

mm

,5I

mpa

rtic

les)

prec

eded

bya

Rhe

odyn

egu

ard

0.5

Imfil

ter.

The

fluor

esce

nce

dete

ctor

emis

sion

for

ochr

atox

inA

emis

sion

for

aflat

oxin

B1.

Abl

end

ofna

tura

llyco

ntam

inat

edgr

ains

Ava

ntag

giat

oan

dot

hers

Ass

essm

ento

fthe

mul

ti-m

ycot

oxin

-bin

ding

effic

acy

ofa

carb

on/

alum

inos

ilica

te-b

ased

prod

ucti

nan

invi

tro

gast

roin

test

inal

mod

el

JA

gric

Foo

dC

hem

2007

;55:

4810

–920

07

Fus

ario

toxi

nan

alys

isD

ON

,ZE

A,F

B1,

....

Liqu

idch

rom

atog

ra-

phy/

elec

tros

pray

ioni

zatio

nta

ndem

mas

ssp

ectr

omet

ry(L

C/E

SI-

MS

/MS

),

Mai

zem

eal

Cav

alie

rean

dot

hers

Myc

otox

ins

prod

uced

byF

usar

ium

genu

sin

mai

ze:

dete

rmin

atio

nby

scre

enin

gan

dco

nfirm

ator

ym

etho

dsba

sed

onliq

uid

chro

mat

ogra

phy

tand

emm

ass

spec

trom

etry

Foo

dC

hem

105(

2):7

00–1

020

07

Con

tinue

d



ab

le1

---C

on

tin

ue

d.

Qu

anti

fica

tio

nT

ype

of

Myc

oto

xin

sm

eth

od

foo

dA

uth

or

Art

icle

Ref

eren

ceY

ear

Och

rato

xin

A(O

TA)

Cle

anup

tand

emim

mun

oass

ayco

lum

nG

inge

r,nu

tmeg

,bla

ckpe

pper

,and

whi

tepe

pper

Rap

idal

l-in-

one

3-st

epim

mun

oass

ayfo

rno

n-in

stru

men

tald

etec

tion

ofoc

hrat

oxin

Ain

high

-col

oure

dhe

rbs

and

spic

es

Tala

nta

Vol

.72,

Issu

e3,

15M

ay20

07;

1230

–4

2007

Sim

ulta

neou

sde

tect

ion

ofafl

atox

inB

1an

doc

hrat

oxin

A

Tand

emim

mun

oass

ay1

mL

colu

mn

with

1cl

eanu

pla

yer

and

two

dete

ctio

nim

mun

olay

ers

ELI

SA

Res

ults

confi

rmed

byH

PLC

-flu

ores

cenc

ede

tect

ion.

LC–M

S/M

Sw

ithim

mun

oaffi

nity

colu

mn

clea

nup

Spi

ces

Gin

ger,

pepp

er,

chili

Gor

yach

eva

and

othe

rsS

imul

tane

ous

noni

nstr

umen

tal

dete

ctio

nof

aflat

oxin

B1

and

ochr

atox

inA

usin

ga

clea

nup

tand

emim

mun

oass

ayco

lum

n

Ana

lChi

mA

cta

2007

;59

0:11

8–24

2007

Afla

toxi

nB

1(A

FB

1),

citr

inin

(CIT

)an

doc

hrat

oxin

A(O

TA)

HP

LCw

ithflu

orim

etry

dete

ctio

neq

uipp

edw

ithan

inje

ctor

20μ

Llo

op,a

C18

sphe

risor

bco

lum

n(3

lmC

18,0

.46

∗25

cm),

and

aflu

ores

cenc

ede

tect

or(S

pect

raph

ysic

2000

),w

asus

ed.D

iffer

ente

xcita

tion

and

emis

sion

fluor

esce

nce

para

met

ers

Ric

eN

guye

nan

dot

hers

Occ

urre

nce

ofafl

atox

inB

1,ci

trin

inan

doc

hrat

oxin

Ain

rice

in.v

epr

ovin

ces

ofth

ece

ntra

lreg

ion

ofV

ietn

am

Foo

dC

hem

2007

;10

5:42

–720

07

Con

tam

inan

tsw

ithth

ehi

ghes

tle

velo

fevi

denc

ein

clud

eafl

atox

in,a

lcoh

olic

beve

rage

s,2,

3,7,

8-te

trac

holo

rdib

enzo

-p-d

ioxi

n

Abn

etC

arci

noge

nic

food

cont

amin

ants

Can

cer

Inve

st20

07A

pr–M

ay;

25(3

):18

9–96

.

2007

Afla

toxi

nM

1(A

FM

1)

and

ochr

atox

inA

(OTA

)

Raw

bulk

milk

Bou

dra

and

othe

rsA

flato

xin

M1

and

ochr

atox

inA

inra

wbu

lkm

ilkfr

omfr

ench

dair

yhe

rds

JD

airy

Sci

2007

;90

:319

7–20

120

07

Sim

ulta

neou

sde

term

inat

ion

oftr

icho

thec

enes

(NIV

,D

ON

,F-X

,T-2

Ro-

A,

Ve-

A)

HP

LCco

uple

dto

UV

and

mas

ssp

ectr

omet

ric(M

S)

dete

ctio

n.

Pla

ntm

ater

ials

uch

asw

heat

,whe

atS

tech

eran

dot

hers

Eva

luat

ion

ofex

trac

tion

met

hods

for

the

sim

ulta

neou

san

alys

isof

sim

ple

and

mac

rocy

clic

tric

hoth

ecen

es

Tala

nta

2007

;73:

251–

720

07

Zea

rale

none

,a-

and

b-ze

aral

enol

s,fu

mon

isin

B1

Hig

h-pe

rfor

man

celiq

uid

chro

mat

ogra

phy

coup

led

with

mas

ssp

ectr

osco

py(H

PLC

/MS

)LC

anal

ysis

byV

aria

nsy

stem

,2pu

mps

,po

lar

mod

ified

RP

-18

colu

mn

Mai

zeA

deju

mo

and

othe

rsS

urve

yof

mai

zefr

omso

uth-

wes

tern

Nig

eria

for

zear

alen

one,

α-

and

β-z

eara

leno

ls,f

umon

isin

B1

and

enni

atin

spr

oduc

edby

Fus

ariu

msp

ecie

s

Foo

dA

ddit

Con

tam

,S

epte

mbe

r20

07;

24(9

):99

3–10

00

2007

Con

tinue

d



ab

le1

---C

on

tin

ue

d.

Qu

anti

fica

tio

nT

ype

of

Myc

oto

xin

sm

eth

od

foo

dA

uth

or

Art

icle

Ref

eren

ceY

ear

Afla

toxi

nsan

doc

hrat

oxin

A.

wer

ede

term

ined

byT

LCan

dH

PLC

met

hods

Pou

ltry

feed

sFr

aga

and

othe

rsP

oten

tialA

flato

xin

and

Och

rato

xin

Apr

oduc

tion

byA

sper

gillu

ssp

ecie

sin

poul

try

feed

proc

essi

ng

Vet

Res

Com

mun

,Vol

ume

31,

Num

ber

3-/3

43-5

3/23

Dec

2006

2007

Sim

ulta

neou

sde

term

inat

ion

ofafl

atox

inB

1(A

FB

1)an

doc

hrat

oxin

A(O

TA)

HP

LCco

lum

nw

asB

io-s

ilC

18H

L90

-5S

(5m

m,4

.6∗

150

mm

)20

0ng

/gw

itha

corr

espo

ndin

glim

itof

dete

ctio

n

Oliv

eoi

lF

erra

cane

and

othe

rsS

imul

tane

ous

dete

rmin

atio

nof

aflat

oxin

B1

and

ochr

atox

inA

and

thei

rna

tura

loc

curr

ence

inM

edite

rran

ean

virg

inol

ive

oil

Foo

dA

ddit

Con

tam

,V

ol.2

4.2:

173–

8020

07

Sim

ulta

neou

s,afl

atox

ins

(AF

L),i

.e.,

B1

(AF

B1)

,B2

(AF

B2)

,G1

(AF

G1)

,an

dG

2(A

FG

2),a

ndoc

hrat

oxin

A(O

TA)

AF

reve

rsed

-pha

seliq

uid

chro

mat

ogra

phy

(RP

LC)

with

fluor

esce

nce

dete

ctio

naf

ter

post

colu

mn

UV

phot

oche

mic

alde

rivat

izat

ion.

OTA

was

sepa

rate

dan

dde

term

ined

byR

PLC

with

fluor

esce

nce

dete

ctio

n.

Gin

seng

and

ging

erTr

ucks

ess

and

othe

rsU

seof

mul

titox

inim

mun

oaffi

nity

colu

mns

for

dete

rmin

atio

nof

aflat

oxin

san

doc

hrat

oxin

Ain

gins

eng

and

ging

er.

JA

OA

CIn

t200

7Ju

lto

Aug

;90(

4):1

042–

920

07

Afla

toxi

nsor

ochr

atox

ins

Rev

iew

Tree

nuts

(alm

onds

,pi

stac

hios

,and

wal

nuts

)

Mol

yneu

xan

dot

hers

Myc

otox

ins

ined

ible

tree

nuts

IntJ

Foo

dM

icro

biol

2007

Jul3

120

07

Afla

toxi

ns,

deox

yniv

alen

ol,

fum

onis

ins,

zear

alen

one,

T-2

toxi

n,oc

hrat

oxin

and

cert

ain

ergo

tal

kalo

ids

Rev

iew

Cro

ppl

ants

Ric

hard

Som

em

ajor

myc

otox

ins

and

thei

rm

ycot

oxic

oses

:an

over

view

.

IntJ

Foo

dM

icro

biol

2007

Jul3

120

07

Afla

toxi

nB

1,ci

trin

in,

deox

yniv

alen

ol,

fum

onis

inB

1,gl

ioto

xin,

ochr

atox

inA

and

zear

alen

one

Hig

h-pe

rfor

man

celiq

uid

chro

mat

ogra

phy

coup

led

tom

ass

spec

trom

etry

(HP

LC–M

S).

Cor

nsi

lage

myc

otox

ins

onnu

trie

ntag

arR

icha

rdan

dot

hers

Toxi

geni

cfu

ngia

ndm

ycot

oxin

sin

mat

ure

corn

sila

ge

Foo

dC

hem

Toxi

col

(200

7)Ju

n22

2007

13tr

icho

thec

enes

,(S

CIR

P),

15-

mon

oace

toxy

scir

peno

l,4,

15-

diac

etox

ysci

rpen

ol,

T-2

tetr

aol,

HT-

2to

xin,

(DO

N),

15-,

3-ac

etyl

DO

N,Z

EA

,α

-an

dβ

-ZO

L

Gas

chro

mat

ogra

phy/

mas

ssp

ectr

omet

ry,z

eara

leno

ne(Z

EA

),α

-an

dβ

-zea

rale

nol

(α-

and

β-Z

OL)

byhi

gh-p

erfo

rman

celiq

uid

chro

mat

ogra

phy

(HP

LC)

with

fluor

esce

nce

and

UV

-det

ectio

n.

Who

lebe

ans,

roas

ted

soy

nuts

,flou

ran

dfla

kes,

text

ured

soy

prot

ein,

tofu

,pr

otei

niso

late

incl

udin

gin

fant

form

ulas

and

ferm

ente

dpr

oduc

ts(s

oysa

uce)

Sch

olle

nber

ger

and

othe

rsN

atur

aloc

curr

ence

ofF

usar

ium

toxi

nsin

soy

food

mar

kete

din

Ger

man

y

IntJ

Foo

dM

icro

biol

2007

;113

:142

–6

Con

tinue

d



ab

le1

---C

on

tin

ue

d.

Qu

anti

fica

tio

nT

ype

of

Myc

oto

xin

sm

eth

od

foo

dA

uth

or

Art

icle

Ref

eren

ceY

ear

Afla

toxi

ns,t

ype

Atr

icho

thec

enes

,typ

eB

tric

hoth

ecen

es,

Och

rato

xin

A,

Zea

rale

none

Fum

onis

ins,

and

Pat

ulin

LC/M

S/M

SC

orn

flake

Mul

ticom

pone

ntm

ycot

oxin

anal

ysis

byLC

/MS

/MS

The

10th

annu

alm

eetin

gof

the

Isra

elan

alyt

ical

chem

istr

yso

ciet

y20

07

2007

Myc

otox

ins

with

in12

min

utes

:(N

IV),

(DO

N),

AfG

1,A

FG

2,A

FB

1,A

fB2,

FB

1,F

B2,

Dia

ceto

xysc

ripen

ol(D

AS

),T

2-To

xine

,O

TA,a

nd(Z

EN

)

HP

LCLC

–MS

/MS

met

hod

for

the

dete

rmin

atio

nof

myc

otox

ins

Var

ious

cattl

efo

rage

s.A

naly

sis

ofm

ycot

oxin

sin

vario

usca

ttle

Mas

ssp

ectr

omet

ry20

07

Zea

rale

none

,gl

ucos

ides

,m

alon

ylgl

ucos

ides

,di

-hex

ose-

and

hexo

se–p

ento

sedi

sacc

harid

esof

zear

alen

one,

and

_-an

d_-

zear

alen

ol,

wer

ede

tect

ed

LCco

uple

dto

tand

emm

ass

spec

trom

etry

(LC

–MS

/MS

).an

alys

isby

(HP

LC)-

MS

/MS

.A

quas

ilC

18co

lum

n(1

00_4

.6m

m,3

mm

)

Usi

ngth

em

odel

plan

tra

bido

psis

thal

iana

.A

fter

trea

tmen

tof

plan

tsee

dlin

gs

Ber

thill

eran

dot

hers

Liqu

idch

rom

atog

raph

yco

uple

dto

tand

emm

ass

spec

trom

etry

(LC

–MS

/MS

)de

term

inat

ion

ofph

ase

IIm

etab

olite

sof

the

myc

otox

inze

aral

enon

ein

the

mod

elpl

antA

rabi

dops

isth

alia

na

Foo

dA

dditi

ves

and

Con

tam

inan

ts,

Nov

embe

r20

06;

23(1

1):1

194–

1200

2006

Afla

toxi

nsH

PLC

-fluo

resc

ence

dete

ctio

n(F

LD)

with

post

colu

mn

elec

troc

hem

ical

deriv

atiz

atio

nin

aK

obra

cell.

Chi

lipo

wde

r,gr

een

bean

,and

blac

kse

sam

e.

Hu

and

othe

rsD

eter

min

atio

nof

aflat

oxin

sin

high

-pig

men

tcon

tent

sam

ples

bym

atrix

solid

phas

edi

sper

sion

and

high

-per

form

ance

liqui

dch

rom

atog

raph

y

JA

gric

Foo

dC

hem

2006

,54,

4126

–30

2006

Afla

toxi

nB

1,fu

mon

isin

B1,

zear

alen

one,

ochr

atox

inA

Afla

toxi

nB

1,fu

mon

isin

B1,

zear

alen

one

usin

gim

mun

oass

ays,

and

ochr

atox

inA

usin

ga

valid

ated

HP

LCm

etho

dw

ithflu

ores

cenc

ede

tect

or

Ric

e,m

aize

and

pean

uts

San

gare

-Tig

oria

ndot

hers

Co-

occu

rren

ceof

aflat

oxin

B1,

fum

onis

inB

1,oc

hrat

oxin

Aan

dze

aral

enon

ein

cere

als

and

pean

uts

from

Cot

ed’

Ivoi

re

Foo

dA

dditi

ves

and

Con

tam

inan

ts,

Oct

ober

2006

;23

(10)

:100

0–10

07

2006

Afla

toxi

nsE

LIS

AH

PLC

All

posi

tive

sam

ples

wer

eal

soan

alyz

edan

dco

nfirm

edby

HP

LC.

Red

scal

ed,r

edan

dbl

ack

pepp

er.

Col

akan

dot

hers

Det

erm

inat

ion

ofafl

atox

inco

ntam

inat

ion

inre

d-sc

aled

,re

dan

dbl

ack

pepp

erby

ELI

SA

and

HP

LC

Jour

nalo

fFoo

dan

dD

rug

Ana

lysi

s,V

ol.

14,N

o.3,

2006

,P

ages

292–

96

2006

Tric

hoth

ecen

es,

ochr

atox

ins,

zear

alen

one,

fum

onis

ins,

aflat

oxin

s,en

niat

ins,

mon

ilifo

rmin

Atm

osph

eric

pres

sure

ioni

satio

n(A

PI)

tech

niqu

esin

the

late

80s,

LC/M

Sha

sbe

com

ea

rout

ine

tech

niqu

eal

soin

food

anal

ysis

Zol

lner

and

May

er-H

elm

JC

hrom

atog

rA

2006

Nov

420

06

Con

tinue

d



Ta

ble

1---

Co

nti

nu

ed

.

Qu

anti

fica

tio

nT

ype

of

Myc

oto

xin

sm

eth

od

foo

dA

uth

or

Art

icle

Ref

eren

ceY

ear

Afla

toxi

n;O

chra

toxi

nA

;P

atul

in; F

usar

ium

toxi

ns

PC

Rre

view

Pat

erso

nId

entifi

catio

nan

dqu

antifi

catio

nof

myc

otox

igen

icfu

ngib

yP

CR

Pro

cess

Bio

chem

istr

yV

olum

e41

,Iss

ue7,

July

2006

,Pag

es14

67–7

4

2006

Tric

hoth

ecen

es,

ochr

atox

ins,

zear

alen

one,

fum

onis

ins,

aflat

oxin

s,en

niat

ins,

mon

ilifo

rmin

LC–(

AP

I)M

Sre

view

Trac

em

ycot

oxin

anal

ysis

inco

mpl

exbi

olog

ical

and

food

mat

rices

byliq

uid

chro

mat

ogra

phy–

atm

osph

eric

pres

sure

ioni

satio

nm

ass

spec

trom

etry

Jour

nalo

fC

hrom

atog

raph

yA

Vol

ume

1136

,Iss

ue2,

Pag

es12

3–69

2006

Afla

toxi

nM

1in

milk

and

B1

infe

edE

LIS

Aim

mun

oass

ay,u

sed

assc

reen

ing

test

,pos

itive

sam

ples

confi

rmed

byH

PLC

Milk

and

feed

Dec

aste

llian

dot

hers

Afla

toxi

nsoc

curr

ence

inm

ilkan

dfe

edin

Nor

ther

nIta

lydu

ring

2004

to20

05

Ava

ilabl

eon

line

27O

ctob

er20

0620

06

Afla

toxi

nsB

1,G

1,B

2,G

2an

doc

hrat

oxin

AU

ltra-

perf

orm

ance

liqui

dch

rom

atog

raph

y/ta

ndem

mas

ssp

ectr

omet

ry(U

PLC

/MS

/MS

),m

ass

spec

trom

eter

used

anel

ectr

ospr

ayio

niza

tion

sour

ceop

erat

edin

the

posi

tive

mod

eto

dete

ctafl

atox

ins

and

inth

ene

gativ

em

ode

tode

tect

ochr

atox

in

Bee

rG

uille

nan

dot

hers

Ultr

a-pe

rfor

man

celiq

uid

chro

mat

ogra

phy/

tand

emm

ass

spec

trom

etry

for

the

sim

ulta

neou

san

alys

isof

aflat

oxin

sB

1,G

1,B

2,G

2an

doc

hrat

oxin

Ain

beer

Rap

idC

omm

unic

atio

nsin

Mas

sS

pect

rom

etry

Vol

ume

20,I

ssue

21,

Pag

es31

99–2

04

2006

Myc

otox

ins

OTA

,DO

N,

AF

B1,

and

FB

wer

ede

tect

edsi

mul

tane

ousl

y

ELI

SA

Foo

dsa

mpl

eR

apid

dete

ctio

nof

food

born

eco

ntam

inan

tsus

ing

anA

rray

Bio

sens

or

Sen

sors

and

Act

uato

rsB

113

(200

6)59

9–60

7

2006

Rev

iew

Mal

iran

dot

hers

Mon

itorin

gth

em

ycot

oxin

sin

food

and

thei

rbi

omar

kers

inth

eC

zech

Rep

ublic

.

Mol

Nut

rF

ood

Res

2006

Jun;

50(6

):51

3–8

2006

AF

Lan

doc

hrat

oxin

A(O

TA)

Liqu

idch

rom

atog

raph

icse

para

tion,

and

fluor

esce

nce

dete

ctio

n

Gin

seng

and

othe

rse

lect

edbo

tani

cal

root

s

Truc

kses

san

dot

hers

Det

erm

inat

ion

ofafl

atox

ins

and

ochr

atox

inA

ingi

nsen

gan

dot

her

bota

nica

lroo

tsby

imm

unoa

ffini

tyco

lum

ncl

eanu

pan

dliq

uid

chro

mat

ogra

phy

with

fluor

esce

nce

dete

ctio

n

JA

OA

CIn

t200

6M

ay-J

un;

89(3

):62

4–30

2006

Con

tinue

d



Ta

ble

1---

Co

nti

nu

ed

.

Qu

anti

fica

tio

nT

ype

of

Myc

oto

xin

sm

eth

od

foo

dA

uth

or

Art

icle

Ref

eren

ceY

ear

Ana

lysi

sof

myc

otox

ins

anal

ysis

ofth

ree

myc

otox

ins.

Afla

toxi

ns(A

Fs)

:A

flato

xin

G1

Afla

toxi

nG

1ha

sbe

ende

tect

edby

liqui

d-liq

uid

part

ition

ing

met

hods

with

HP

LCde

tect

ion

asfa

lse-

posi

tive

inso

me

mai

zeF

umon

isin

s(F

B):

Com

poun

dsin

terf

erin

gw

ithth

eF

B’s

antib

odie

sw

ere

also

obse

rved

whi

lean

alys

ing

brea

kfas

tcer

eals

lead

ing

toun

dere

stim

atio

nof

FB

.Och

rato

xin

A(O

TA)

Mai

zeC

aste

gnar

oan

dot

hers

Adv

anta

ges

and

draw

back

sof

imm

unoa

ffini

tyco

lum

nsin

anal

ysis

ofm

ycot

oxin

sin

food

Mol

Nut

rF

ood

Res

2006

May

;50

(6):

480–

7

2006

Och

rato

xin

(OT

)an

dafl

atox

in(A

F)

Bar

ley

root

lets

(BR

)R

ibei

roan

dot

hers

Influ

ence

ofw

ater

activ

ity,

tem

pera

ture

,and

time

onm

ycot

oxin

spr

oduc

tion

onba

rley

root

lets

.

Lett

App

lMic

robi

ol20

06F

eb;

42(2

):17

9–84

2006

Tric

hoth

ecen

es,

ochr

atox

ins,

zear

alen

one,

fum

onis

ins,

aflat

oxin

s,en

niat

ins,

mon

ilifo

rmin

and

seve

ralo

ther

myc

otox

ins

LC–(

AP

I)M

SR

evie

wTr

ace

myc

otox

inan

alys

isin

com

plex

biol

ogic

alan

dfo

odm

atric

esby

liqui

dch

rom

atog

raph

y–at

mos

pher

icpr

essu

reio

nisa

tion

mas

ssp

ectr

omet

ry

Jour

nalo

fC

hrom

atog

raph

yA

Vol

ume

1136

,Iss

ue2,

15D

ecem

ber

2006

,Pag

es12

3–69

2006

Sim

ulta

neou

sly

NIV

,D

ON

,ZE

N,

diac

etox

ysci

rpen

ol,

T-2

toxi

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rruc

arol

,ve

rruc

arin

A,

neos

olan

iol,

ster

igm

atoc

ystin

,ro

ridin

A,O

TA,A

FB

1,A

FB

2,A

FG

1,A

FG

2

HP

LCflu

ores

cenc

ede

tect

or,

inje

ctor

,gra

dien

tand

data

hand

ling

capa

bilit

yis

requ

ired.

The

fluor

esce

nce

dete

ctor

setti

ngs:

exci

tatio

n31

5nm

,em

issi

on>

415

nmliq

uid

chro

mat

ogra

phy/

tand

emm

ass

spec

trom

etry

(LC

/MS

/MS

)m

etho

d

Two

fung

alm

edia

wer

eus

edas

sam

ples

Del

mul

lean

dot

hers

Dev

elop

men

tofa

liqui

dch

rom

atog

raph

y/ta

ndem

mas

ssp

ectr

omet

rym

etho

dfo

rth

esi

mul

tane

ous

dete

rmin

atio

nof

16m

ycot

oxin

son

cellu

lose

filte

rsan

din

fung

alcu

lture

s

Rap

idC

omm

unM

ass

Spe

ctro

m.2

006;

20(5

):77

1–6

2006

Afla

toxi

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chra

toxi

nA

;P

atul

in; F

usar

ium

toxi

ns

PC

RF

ood

stuf

frev

iew

Iden

tifica

tion

and

quan

tifica

tion

ofm

ycot

oxig

enic

fung

iby

PC

R

Pro

cess

Bio

chem

istr

yV

olum

e41

,Iss

ue7,

July

2006

,Pag

es14

67–7

4

2006

Con

tinue

d



ab

le1

---C

on

tin

ue

d.

Qu

anti

fica

tio

nT

ype

of

Myc

oto

xin

sm

eth

od

foo

dA

uth

or

Art

icle

Ref

eren

ceY

ear

Och

rato

xin

A(O

TA)

Ext

ract

sw

ere

subs

eque

ntly

anal

ysed

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gre

vers

e-ph

ase

high

-per

form

ance

liqui

dch

rom

atog

raph

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ores

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ede

tect

ion

with

post

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mn

amm

onia

tion

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prov

eth

elim

itof

dete

ctio

n.

Win

ean

dbe

erV

arel

isan

dot

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Qua

ntita

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anal

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hrat

oxin

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win

ean

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ing

solid

phas

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trac

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high

-per

form

ance

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atog

raph

y–flu

ores

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ede

tect

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Foo

dA

dditi

ves

and

Con

tam

inan

ts,

Dec

embe

r20

06;

23(1

2):1

308–

15

2006

Afla

toxi

ns(B

1,B

2,G

1,an

dG

2),p

atul

inan

der

gost

erol

one

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e

HP

LC(A

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s,U

SA

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uipp

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itha

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ctor

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lent

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ries,

US

A)

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mun

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nity

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mn

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am,W

ater

tow

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A,

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A)

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dfig

sK

arac

aan

dN

asA

flato

xins

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ulin

and

ergo

ster

olco

nten

tsof

drie

dfig

sin

Turk

ey

Foo

dA

dditi

ves

and

Con

tam

inan

ts,M

ay,

2006

;23(

5):5

02–0

8

2006

Tric

hoth

ecen

es,

ochr

atox

ins,

zear

alen

one,

fum

onis

ins,

aflat

oxin

s,en

niat

ins,

mon

ilifo

rmin

,and

seve

ralo

ther

myc

otox

ins

App

licat

ion

ofLC

–(A

PI)

MS

atm

osph

eric

pres

sure

ioni

satio

n(A

PI)

tech

niqu

es

Trac

em

ycot

oxin

anal

ysis

inco

mpl

exbi

olog

ical

and

food

mat

rices

byliq

uid

chro

mat

ogra

phy–

atm

osph

eric

pres

sure

ioni

satio

nm

ass

spec

trom

etry

bD

epar

tmen

tofC

linic

alP

harm

acol

ogy,

Med

ical

Uni

vers

ityof

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nna,

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ringe

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20,A

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tria

2006

AF

M1

Thi

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yer

chro

mat

ogra

phy

for

dete

rmin

ing

AF

M1.

com

pa-

red

with

HP

LCflu

ores

cenc

ede

tect

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Raw

,pas

teur

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ultr

ahig

htr

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mpe

ratu

re(U

HT

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ilk

Shu

ndo

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ino

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toxi

nM

1in

milk

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mun

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nity

colu

mn

clea

nup

with

TLC

/HP

LCde

term

inat

ion

Bra

zilia

nJo

urna

lof

Mic

robi

olog

y(2

006)

37:1

64–6

7

2006

Och

rato

xin

A(O

TA)

and

aflat

oxin

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(AF

B1)

one

byon

e

Med

iterr

anea

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ores

.Ith

asa

rect

angu

lar

shap

ew

ith10

.452

km2

area

.OTA

was

dete

cted

and

quan

tified

byre

vers

ed-p

hase

HP

LC.

auto

sam

pler

(Agi

lent

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1313

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LS)

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aflu

ores

cenc

ede

tect

orA

sele

cted

RP

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mn

HP

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etho

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inB

1an

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Win

e-gr

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bano

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lture

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ium

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hour

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nce

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chra

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prod

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bane

segr

apes

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atox

ina

cont

enti

nm

usts

and

finis

hed

win

esdu

ring

2004

JA

gric

Foo

dC

hem

2006

,54,

8977

–82

2006

Con

tinue

d



ab

le1

---C

on

tin

ue

d.

Qu

anti

fica

tio

nT

ype

of

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oto

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od

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uth

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icle

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dhbi

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atio

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clon

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cyst

ins

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licat

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toim

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and

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ffini

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mpl

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ior

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alys

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liqui

dch

rom

atog

raph

yan

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006)

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ates

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and

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amin

atio

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llect

edfr

omdi

ffere

ntst

ates

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dia:

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ultic

entr

est

udy

Foo

dA

dditi

ves

and

Con

tam

inan

ts,A

pril,

2006

;(23

)4:4

11–1

4

2006

enzy

me

linke

dim

mun

osor

bent

assa

ys(E

LIS

A),

flow

thro

ugh

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says

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rom

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raph

icte

chni

ques

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eic

acid

ampl

ifica

tion

assa

ys,

bios

enso

rs,a

ndm

icro

arra

ysfo

rde

tect

ion

ofm

olds

and

myc

otox

ins.

Foo

ng-C

unni

ngha

man

dot

hers

Rap

idde

tect

ion

ofm

ycot

oxig

enic

mol

dsan

dm

ycot

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sin

frui

tjui

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letin

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ulTe

chni

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vers

ityV

OLU

ME

54,N

UM

BE

R4

2006

AF

B1

and

OTA

one

byon

eQ

uant

itate

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HP

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llus

para

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kan

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ekor

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biol

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23(2

006)

612–

2120

06

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toxi

nsH

igh-

perf

orm

ance

liqui

dch

rom

atog

raph

y(H

PLC

)-flu

ores

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ede

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(FD

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ioni

zatio

n(E

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m20

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Con

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le1

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on

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ue

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Qu

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and

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dw

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ical

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Pu

2006

Nov

;24

(6):

581–

420

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PLC

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mal

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KM

ITL

Sci

.Tec

h.J.

Vol

.6

No.

1Ja

n.–J

un.

2006

2006

Afla

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urin

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gner

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ifica

tion

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1-N

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mat

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spec

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mR

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tam

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ts,

Aug

ust2

006;

23(8

):81

6–25

2006

Con

tinue

d



Ta

ble

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nti

nu

ed

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tio

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oto

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icle

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chro

mat

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buck

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nce

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tail

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n

JF

ood

Pro

t.20

06Ju

n;69

(6):

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2006

Sim

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T-2

toxi

n,ne

osol

anio

l,m

onoa

ceto

xysc

ir-pe

nol,

diac

etox

ysci

rpen

ol,

T-2

trio

l,an

dT-

2te

trao

l

Liqu

idch

rom

atog

raph

y-el

ectr

ospr

ayio

niza

tion

tand

emm

ass

spec

trom

etry

(LC

-ES

I-M

S/M

S)

Whe

atan

doa

tsam

ples

Klo

tzel

and

othe

rsD

eter

min

atio

nof

12Ty

peA

and

Btr

icho

thec

enes

ince

real

sby

liqui

dch

rom

atog

raph

y-el

ectr

ospr

ayio

niza

tion

tand

emm

ass

spec

trom

etry

JA

gric

Foo

dC

hem

2005

,53:

8904

–10

2005

Whi

tlow

and

othe

rsM

ycot

oxin

sin

dair

yca

ttle:

occu

rren

ce,t

oxic

ity,

prev

entio

nan

dtr

eatm

ent

Whi

tlow

and

Hag

ler,

2005

.Pro

c.S

outh

wes

tNut

r.C

onf.:

124–

38

2005

FU

M1

LCM

SYu

and

othe

rsD

evel

opin

ga

gene

ticsy

stem

for

func

tiona

lman

ipul

atio

nsof

FU

M1,

apo

lyke

tide

synt

hase

gene

for

the

bios

ynth

esis

offu

mon

isin

sin

Fus

ariu

mve

rtic

illio

ides

FE

MS

Mic

robi

olog

yLe

tters

Vol

ume

248,

Issu

e2,

15Ju

ly20

05,P

ages

257–

64

2005

OTA

,α-Z

EA

,β-Z

EA

zear

alan

ol(t

aler

anol

),F

B1,

FB

2,T-

2to

xin,

HT-

2to

xin,

T-2

trio

l,di

acet

oxys

cirp

enol

(DA

S),

15-

mon

oace

toxy

scir

peno

l(M

AS

),(D

ON

),3-

acet

ylde

oxyN

IV(3

-AcD

ON

),15

-ac

etyl

deox

yNIV

(15-

AcD

ON

),de

epox

y-D

ON

(DO

M-1

)an

dA

FM

1

LC_M

S/M

SLi

quid

chro

mat

ogra

phic

/tand

emm

ass

spec

trom

etric

met

hods

usin

gpn

eum

atic

ally

assi

sted

elec

tros

pray

ioni

satio

n(L

C–E

SI-

MS

/MS

)

Milk

Sør

ense

nan

dE

lbæ

kD

eter

min

atio

nof

myc

otox

ins

inbo

vine

milk

byliq

uid

chro

mat

ogra

phy

tand

emm

ass

spec

trom

etry

JC

hrom

atog

rB

,820

(200

5)18

3–96

2005

Con

tinue

d



Ta

ble

1---

Co

nti

nu

ed

.

Qu

anti

fica

tio

nT

ype

of

Myc

oto

xin

sm

eth

od

foo

dA

uth

or

Art

icle

Ref

eren

ceY

ear

Fus

ariu

mm

ycot

oxin

sN

IV,D

ON

,fu

sare

non-

X,3

-ac

etyl

deox

yniv

alen

ol,

3-ac

etyl

-DO

Nan

d15

-ace

tyl-D

ON

,di

acet

oxy-

scir

peno

l,H

T-2

toxi

n,T-

2to

xin,

ZE

N

RP

-LC

with

atm

osph

eric

pres

sure

chem

ical

ioni

zatio

ntr

iple

quad

rupo

lem

ass

spec

trom

etry

(LC

–AP

CI–

MS

/MS

).LC

–MS

/MS

anal

ysis

was

perf

orm

ed

Mai

zeB

erth

iller

and

othe

rsR

apid

sim

ulta

neou

sde

term

inat

ion

ofm

ajor

type

A-

and

B-t

richo

thec

enes

asw

ella

sze

aral

enon

ein

mai

zeby

high

-per

form

ance

liqui

dch

rom

atog

raph

y–ta

ndem

mas

ssp

ectr

omet

ry

Jour

nalo

fC

hrom

atog

raph

yA

,10

62(2

005)

209–

16

2005

Co-

occu

rren

ceof

ochr

atox

inA

and

aflat

oxin

B1

one

byon

e

Drie

dfig

sS

enyu

vaan

dot

hers

Sur

vey

for

co-o

ccur

renc

eof

ochr

atox

inA

and

aflat

oxin

B1

indr

ied

figs

inTu

rkey

usin

ga

sing

lela

bora

tory

-val

idat

edal

kalin

eex

trac

tion

met

hod

for

ochr

atox

inA

.

JF

ood

Pro

t200

5Ju

l;68

(7):

1512

–520

05

Afla

toxi

nM

1E

nzym

eim

mun

oass

ayco

mpa

red

with

are

fere

nce

high

-per

form

ance

liqui

dch

rom

atog

raph

ym

etho

dw

itha

fluor

esce

ntde

tect

or.

Milk

Mag

liulo

and

othe

rsD

evel

opm

enta

ndva

lidat

ion

ofan

ultr

asen

sitiv

ech

emilu

min

esce

nten

zym

eim

mun

oass

ayfo

rafl

atox

inM

1in

milk

JA

gric

Foo

dC

hem

2005

,53,

3300

–05

2005

DO

N,A

flato

xins

,O

chra

toxi

nA

,Z

eara

leno

nean

dF

umon

isin

HP

LCan

dpo

stco

lum

nde

rivat

izat

ion

colu

mn:

MY

CO

TOX

TM

reve

rsed

-pha

seC

18,

4.6

×25

0m

m

Aliq

uoto

fthe

beve

rage

Ofit

sero

vaan

dot

hers

Mul

tires

idue

myc

otox

inan

alys

issi

ngle

run

anal

ysis

ofde

oxyn

ival

enol

,afl

atox

ins,

ochr

atox

ina,

zear

alen

one

and

fum

onis

inby

HP

LCan

dpo

stco

lum

nde

rivat

izat

ion

ww

w.p

icke

ringl

abs.

com

2005

Afla

toxi

nM

1,afl

atox

inB

1,an

doc

hrat

oxin

A.

HP

LCpu

mp

Mod

el22

48to

geth

erw

itha

Low

Pre

ssur

eM

ixer

Flu

ores

cenc

ede

tect

ion:

.

Ana

lyze

123

sam

ples

of24

-hdi

ets

Siz

ooan

dV

anE

gmon

dA

naly

sis

ofdu

plic

ate

24-h

diet

sam

ples

for

aflat

oxin

B1,

aflat

oxin

M1

and

ochr

atox

inA

Foo

dA

dditi

ves

and

Con

tam

inan

ts,

Feb

ruar

y20

05;

22(2

):16

3–72

2005

Afla

toxi

nsB

1,B

2,G

1an

dG

2(A

FB

1,A

FB

2,A

FG

1,A

FG

2)an

doc

hrat

oxin

A(O

TA)

one

byon

e

high

-per

form

ance

liqui

dch

rom

atog

raph

y(H

PLC

)flu

ores

cenc

ede

tect

or

Spi

cegr

ound

red

pepp

er,6

blac

kpe

pper

,5w

hite

pepp

er,5

spic

em

ix,

and

5ch

ili

Faze

kas

and

othe

rsA

flato

xin

and

ochr

atox

inA

cont

ento

fspi

ces

inH

unga

ry

Foo

dA

dditi

ves

&C

onta

min

ants

,V

olum

e22

,Iss

ue9

Sep

tem

ber

2005

,pa

ges

856–

63

2005

Con

tinue

d



ab

le1

---C

on

tin

ue

d.

Qu

anti

fica

tio

nT

ype

of

Myc

oto

xin

sm

eth

od

foo

dA

uth

or

Art

icle

Ref

eren

ceY

ear

Sim

ulta

neou

sde

term

inat

ion

ofT-

2an

dH

T-2

toxi

ns

HP

LC-

fluor

esce

nce

quan

tified

byre

vers

ed-p

hase

HP

LCw

ithflu

orom

etric

dete

ctio

n(e

xcita

tion

wav

elen

gth

381

nm,e

mis

sion

wav

elen

gth

470

nm)

afte

rde

rivat

izat

ion

with

1-A

N.

Cer

ealg

rain

sLa

ttanz

ioan

dot

hers

Ana

lysi

sof

T-2

and

HT-

2to

xins

ince

real

grai

nsby

imm

unoa

ffini

tycl

eanu

pan

dliq

uid

chro

mat

ogra

phy

with

fluor

esce

nce

dete

ctio

n

Jour

nalo

fC

hrom

atog

raph

yA

,10

75(2

005)

151–

58

2005

Och

rato

xin

A(O

TA)

ELI

ZA

Roa

sted

coffe

eLo

beau

and

othe

rsD

evel

opm

ento

fane

wcl

eanu

pta

ndem

assa

yco

lum

nfo

rth

ede

tect

ion

ofoc

hrat

oxin

Ain

roas

ted

coffe

e

Ana

lytic

aC

him

ica

Act

aV

olum

e53

8,Is

sues

1-2,

4M

ay20

05,

Pag

es57

–61

2005

Sim

ulta

neou

sly

aflat

oxin

sB

1,B

2,G

1,G

2an

dM

1,oc

hrat

oxin

A,

myc

ophe

nolic

acid

,pe

nici

llic

acid

and

roqu

efor

tine

Csi

mul

tane

ousl

y

HP

LC_M

SB

lue

and

whi

tem

old

chee

ses

Kok

kone

nan

dot

hers

Det

erm

inat

ion

ofse

lect

edm

ycot

oxin

sin

mou

ldch

eese

sw

ithliq

uid

chro

mat

ogra

phy

coup

led

tota

ndem

with

mas

ssp

ectr

omet

ry

Foo

dA

dditi

ves

and

Con

tam

inan

ts,M

ay20

05;2

2(5)

:449

–56

2005

Och

rato

xin

A(O

TA)

anal

ysis

(LC

)w

ithflu

ores

cenc

ede

tect

ion

(FD

),(E

LIS

A)

kits

,us

ing

anti-

OTA

antib

odie

s(e

lect

roch

emic

alim

mun

osen

sors

,flu

ores

cenc

epo

laris

atio

n,la

tera

lflow

devi

ces,

enzy

me-

base

dflo

wth

roug

hm

embr

anes

,and

surf

ace

plas

mon

reso

nanc

ebi

osen

sors

)Li

quid

chro

mat

ogra

phy-

mas

ssp

ectr

omet

ryre

pres

ents

anad

equa

teal

tern

ativ

eto

LC-F

D

Cer

eals

,cof

fee,

win

e,an

dbe

er.

Vis

cont

iand

De

giro

lam

oF

itnes

sfo

rpu

rpos

e–oc

hrat

oxin

Aan

alyt

ical

deve

lopm

ents

Foo

dA

dditi

ves

and

Con

tam

inan

ts,

Sup

plem

ent1

2005

:37–

44

2005

Afla

toxi

nM

1(A

FM

1)

and

ochr

atox

inA

(OA

)

Qua

ntifi

catio

nby

high

-per

form

ance

liqui

dch

rom

atog

raph

y(H

PLC

)w

ithflu

ores

cenc

ede

tect

ion.

Hum

anM

ilkB

ank

Nav

asan

dot

hers

Afla

toxi

nM

1an

doc

hrat

oxin

Ain

ahu

man

milk

bank

inth

eci

tyof

Sao

Pau

lo,B

razi

l

Foo

dA

dditi

ves

&C

onta

min

ants

,V

olum

e22

,Iss

ue5

May

2005

,pag

es45

7–62

2005

Och

rato

xin

A(O

TA)

LC–M

Ssy

stem

Alc

ohol

icbe

vera

ges,

win

ean

dbe

erB

acal

onia

ndot

hers

Aut

omat

edon

line

solid

phas

eex

trac

tion-

liqui

dch

rom

atog

raph

y-el

ectr

ospr

ayta

ndem

mas

ssp

ectr

omet

rym

etho

dfo

rth

ede

term

inat

ion

ofoc

hrat

oxin

ain

win

ean

dbe

er

JA

gric

Foo

dC

hem

2005

,53,

5518

–25

2005

Con

tinue

d



ab

le1

---C

on

tin

ue

d.

Qu

anti

fica

tio

nT

ype

of

Myc

oto

xin

sm

eth

od

foo

dA

uth

or

Art

icle

Ref

eren

ceY

ear

Afla

toxi

nsin

anu

mbe

rof

com

mod

ities

,oc

hrat

oxin

A(O

TA)

inw

heat

,de

oxyn

ival

enol

(DO

N)

inm

aize

and

whe

at,a

ndZ

EA

inm

aize

Rev

iew

artic

leA

flato

xins

ina

num

ber

ofco

mm

oditi

es,

ochr

atox

inA

(OTA

)in

whe

at,

deox

yniv

alen

ol(D

ON

)in

mai

zean

dw

heat

,and

ZE

Ain

mai

ze

Krs

kaan

dot

hers

Adv

ance

sin

the

anal

ysis

ofm

ycot

oxin

san

dits

qual

ityas

sura

nce

Foo

dA

dditi

ves

and

Con

tam

inan

ts,

Vol

ume

22,N

umbe

r4,

Apr

il20

05,p

p.34

5–53

(9)

2005

Afla

toxi

n(A

F)

oroc

hrat

oxin

A(O

TA)

one

byon

e

HP

LCfo

rA

FO

TAby

(ELI

SA

)S

eed-

,pul

ses-

,and

cere

al-fl

ours

and

star

ches

Bay

dar

and

othe

rsA

flato

xin

and

ochr

atox

inin

vario

usty

pes

ofco

mm

only

cons

umed

reta

ilgr

ound

sam

ples

inA

nkar

a,Tu

rkey

Ann

Agr

icE

nviro

nM

ed.

2005

;12(

2):1

93–7

2005

Afla

toxi

n,oc

hrat

oxin

A,

Ana

lyze

dfo

rth

em

ycot

oxin

sby

RH

MTe

chno

logy

.usi

nghi

gh-p

erfo

rman

celiq

uid

chro

mat

ogra

phy

(HP

LC).

Spi

ces

Sur

vey

ofsp

ices

for

aflat

oxin

san

doc

hrat

oxin

AF

ood

Sur

vey

Info

rmat

ion

She

ets

onth

eW

WW

:http

://w

ww

.fo

od.g

ov.u

k/sc

ienc

e/su

rvei

llanc

e

2005

Fum

onis

inB

1an

dB

2,T

2to

xin,

DO

Non

eby

one

HP

LCw

ithflu

ores

cenc

ede

tect

orfo

rfu

mon

isin

san

dw

ithva

riabl

ew

avel

engt

hU

Vde

tect

orfo

rT

2to

xin

and

DO

N

161

cere

alan

dce

real

prod

ucts

115

med

icin

alan

dhe

rbal

tea

spec

imen

s11

2ce

real

and

puls

epr

oduc

ts

Om

urta

gan

dot

hers

Are

view

onfu

mon

isin

and

tric

hoth

ecen

em

ycot

oxin

sin

food

sco

nsum

edin

Turk

ey

AR

IThe

Bul

letin

ofth

eIs

tanb

ulTe

chni

cal

Uni

vers

ityV

olum

e54

,Num

ber

4

2005

Fum

onis

inB

1,fu

mon

isin

B2,

zear

alen

one

and

ochr

atox

inA

one

byon

e

HP

LCsy

stem

(Var

ian,

US

A)

with

fluor

esce

nce

dete

ctio

n.M

aize

Dom

ijan

and

othe

rsF

umon

isin

B1,

fum

onis

inB

2,ze

aral

enon

ean

doc

hrat

oxin

Aco

ntam

inat

ion

ofm

aize

inC

roat

ia

Foo

dA

dditi

ves

and

Con

tam

inan

ts,J

uly

2005

;22(

7):6

77–8

0

2005

Och

rato

xin

A(O

TA)

and

aflat

oxin

sB

1,B

2,G

1an

dG

2

TLC

and

confi

rmat

ion

byH

PLC

extr

acts

byH

PLC

with

fluor

esce

ntde

tect

ion.

Bee

polle

nG

onza

lez

and

othe

rsO

ccur

renc

eof

myc

otox

inpr

oduc

ing

fung

iin

bee

polle

n

IntJ

Foo

dM

icro

biol

105

(200

5)1–

920

05

Fus

ariu

mm

ycot

oxin

s(t

richo

thec

enes

Type

Aan

dB

,ze

aral

enon

e)si

mul

tane

ousl

y

Liqu

idch

rom

atog

raph

yw

ithta

ndem

mas

ssp

ectr

omet

ry(L

C-E

SI-

MS

/MS

).H

PLC

Cer

eals

and

cere

al-b

ased

sam

ples

Bis

elli

and

Hum

mer

tD

evel

opm

ento

fam

ultic

ompo

nent

met

hod

for

Fus

ariu

mto

xins

usin

gLC

–MS

/MS

and

itsap

plic

atio

ndu

ring

asu

rvey

for

the

cont

ento

fT-2

toxi

nan

dde

oxyn

ival

enol

inva

rious

feed

and

food

sam

ples

Foo

dA

dditi

ves

and

Con

tam

inan

ts,

Aug

ust2

005;

22(8

):75

2–60

2005

Con

tinue

d



ab

le1

---C

on

tin

ue

d.

Qu

anti

fica

tio

nT

ype

of

Myc

oto

xin

sm

eth

od

foo

dA

uth

or

Art

icle

Ref

eren

ceY

ear

Afla

toxi

n-fu

mon

isin

sD

eoxy

niva

leno

lZ

eara

leno

neon

eby

one.

HP

LCan

dLC

MS

for

AF

Fum

onis

ins

ELI

SA

for

AF

and

Fum

onis

ins

45co

mm

erci

alco

rn(m

aize

)hy

brid

sA

bbas

and

othe

rsA

flato

xin

and

fum

onis

inco

ntam

inat

ion

ofco

mm

erci

alco

rn( Z

eam

ays )

hybr

ids

inM

issi

ssip

pi

JA

gric

Foo

dC

hem

2002

,50,

5246

–54

2005

Och

rato

xin

A(O

TA)

Com

petit

ive

dire

cten

zym

e-lin

ked

imm

unos

orbe

ntas

say

(cdE

LIS

A)

and

aco

mpe

titiv

ein

dire

ctE

LIS

A(c

iELI

SA

)w

ere

used

effic

acy

ofcd

ELI

SA

was

also

confi

rmed

byth

ehi

ghpe

rfor

man

celiq

uid

chro

mat

ogra

phy

met

hod

Soy

bean

sam

ples

Yuan

dot

hers

Dev

elop

men

tofa

sens

itive

enzy

me-

linke

dim

mun

osor

bent

assa

yfo

rth

ede

term

inat

ion

ofoc

hrat

oxin

A

JA

gric

Foo

dC

hem

2005

,53,

6947

–53

2005

AF

M1

HP

LC-fl

uore

scen

ce,A

FM

1qu

antifi

edby

HP

LCta

ndem

mas

ssp

ectr

omet

ryw

ithne

gativ

eel

ectr

ospr

ayio

niza

tion.

Who

lem

ilk,l

owfa

tm

ilk,m

ilkpo

wde

rC

hen

and

othe

rsD

eter

min

atio

nof

aflat

oxin

M1

inm

ilkan

dm

ilkpo

wde

rus

ing

high

-flow

solid

phas

eex

trac

tion

and

liqui

dch

rom

atog

raph

y-ta

ndem

mas

ssp

ectr

omet

ry

JA

gric

Foo

dC

hem

2005

,53,

8474

–80

2005

(DO

N),

(ZE

N),

fum

onis

inB

1(F

B1)

and

mon

ilifo

rmin

(MO

N)

Cel

lcul

ture

sse

nsiti

vece

lllin

esfo

rpr

elim

inar

ysc

reen

ing

ofD

ON

,ZE

N,

and

MO

Nco

ntam

inat

edfe

edan

dfo

odex

trac

ts

Chi

nese

ham

ster

ovar

yce

lls(C

HO

-K1)

mos

tse

nsiti

vefo

rD

ON

and

FB

1w

ithIC

50va

lues

Cet

inan

dB

ulle

rman

Cyt

otox

icity

ofF

usar

ium

myc

otox

ins

tom

amm

alia

nce

llcu

lture

sas

dete

rmin

edby

the

MT

Tbi

oass

ay

Foo

dan

dC

hem

ical

Toxi

colo

gyV

olum

e43

,Iss

ue5,

May

2005

,Pag

es75

5–64

2005

OTA

Liqu

idch

rom

atog

raph

yco

uple

dw

itha

fluor

esce

nce

dete

ctor

and

confi

rmed

bym

ethy

lest

erde

rivat

izat

ion.

Ric

esa

mpl

esJu

anan

dot

hers

AS

Eof

ochr

atox

inA

from

rice

sam

ples

JA

gric

Foo

dC

hem

2005

,53,

9348

–51

2005

Aan

dB

type

tric

hoth

ecen

es,

nam

ely

4,15

-di

acet

oxy-

scir

peno

l,T

2-to

xin,

deox

yniv

alen

ol(D

ON

)an

dni

vale

nol

(NIV

).A

fter

deriv

atiz

atio

nw

ithN

,N-d

imet

hyl-

trim

ethy

lsily

l-ca

rbam

ate

Gas

chro

mat

ogra

phy

with

flam

eio

niza

tion

(GC

-FID

)or

mas

sse

lect

ive

dete

ctio

n(G

C–M

SD

)

Sem

olin

aan

dco

rngr

itsE

kean

dot

hers

Sim

ulta

neou

sde

tect

ion

ofA

and

Btr

icho

thec

enes

byga

sch

rom

atog

raph

yw

ithfla

me

ioni

zatio

nor

mas

sse

lect

ive

dete

ctio

n

Mic

roch

emJ

78(2

004)

211–

620

04

Con

tinue

d



Ta

ble

1---

Co

nti

nu

ed

.

Qu

anti

fica

tio

nT

ype

of

Myc

oto

xin

sm

eth

od

foo

dA

uth

or

Art

icle

Ref

eren

ceY

ear

Asi

gnifi

cant

decr

ease

inth

ere

lativ

ew

eigh

toft

hebu

rsa

ofFa

bric

ius

was

note

dat

the

high

estc

once

ntra

tion

ofA

F(2

mg/

kg)

and

com

bina

tions

of1

and

2m

g/kg

AF

and

2an

d4

mg/

kgO

A

Bro

ilers

Ver

ma

and

othe

rsE

ffect

ofgr

aded

leve

lsof

aflat

oxin

,och

rato

xin

and

thei

rco

mbi

natio

nson

the

perf

orm

ance

and

imm

une

resp

onse

ofbr

oile

rs

Br

Pou

ltS

ci20

04A

ug;

45(4

):51

2–8

2004

Och

rato

xin

A(O

TA)

Usi

ngR

P-H

PLC

with

aflu

ores

cenc

ede

tect

ion

Cer

eals

,red

win

e,ra

isin

san

dgr

een

coffe

e

But

tinge

ran

dot

hers

Per

form

ance

ofne

wcl

eanu

pco

lum

nfo

rth

ede

term

inat

ion

ofoc

hrat

oxin

Ain

cere

als

and

food

stu.

sby

HP

LC-F

LD

Foo

dA

dditi

ves

and

Con

tam

inan

ts,V

ol.

21,N

o.11

(Nov

embe

r20

04),

pp.1

107–

14

2004

Fus

ariu

m-t

oxin

-de

oxyn

ival

enol

and

zear

alen

one

one

byon

e

HP

LCD

ON

inw

heat

and

diet

anal

ysed

by(H

PLC

)w

ithdi

ode

arra

yde

tect

ion

(DA

D)

Whe

atfo

rdu

ckdi

etD

anic

kean

dot

hers

Effe

cts

ofgr

aded

leve

lsof

Fus

ariu

m-t

oxin

-co

ntam

inat

edw

heat

inP

ekin

duck

diet

son

perf

orm

ance

,hea

lthan

dm

etab

olis

mof

deox

yniv

alen

olan

dze

aral

enon

e

Brit

ish

Pou

ltry

Sci

ence

Vol

ume

45,N

umbe

r2

(Apr

il20

04),

pp.2

64–7

2

2004

Thr

eety

peA

(dia

ceto

xysc

irpe

nol,

T-2

toxi

n,H

T-2

toxi

n)an

dfiv

ety

peB

tric

hoth

ecen

es[d

eoxy

niva

leno

l(D

ON

),ni

vale

nol,

fusa

reno

n-X

,3-

acet

ylde

oxyn

ival

enol

,15

-ac

etyl

deox

yniv

alen

ol].

Sim

ulta

neou

sLC

–fluo

resc

ence

dete

ctio

n(F

LD)

dete

rmin

atio

n

Fin

ely

grou

ndce

real

sD

all’A

sta

and

othe

rsS

imul

tane

ous

liqui

dch

rom

atog

raph

y–flu

ores

cenc

ean

alys

isof

type

Aan

dty

peB

tric

hoth

ecen

esas

fluor

esce

ntde

rivat

ives

via

reac

tion

with

coum

arin

-3-c

arbo

nyl

chlo

ride

JC

hrom

atog

rA

,104

7(2

004)

241–

720

04

Och

rato

xin

A(O

TA)

and/

orci

trin

in(C

IT)

and/

orafl

atox

inB

(AF

B)

HP

LCco

uple

dto

aflu

ores

cenc

ede

tect

orO

live

ElA

dlou

nian

dot

hers

Pre

limin

ary

data

onth

epr

esen

ceof

myc

otox

ins

(och

rato

xin

A,c

itrin

in,a

ndafl

atox

inB

1)in

blac

kta

ble

oliv

es“G

reek

styl

e”of

Mor

occa

nor

igin

Foo

dC

ontr

olV

olum

e15

,Iss

ue7,

Oct

ober

2004

,Pag

es54

3–48

2004

Afla

toxi

n,oc

hrat

oxin

,ze

aral

enon

ean

dde

oxyn

ival

enon

eon

eby

one

wiy

hdi

ffere

ntm

obil

phas

e

HP

LCW

ater

s60

0pu

mp

with

diod

ear

ray

and

aflu

ores

cenc

ede

tect

orlin

ked

with

IBM

com

pute

rw

asus

ed

Var

ious

food

prod

ucts

:ce

real

and

cere

alpr

oduc

ts,n

uts

and

nutp

rodu

cts,

spic

es,

dry

frui

tsan

dbe

vera

ges

Abd

ulka

dar

and

othe

rsM

ycot

oxin

sin

food

prod

ucts

avai

labl

ein

Qat

arF

ood

Con

trol

Vol

ume

15,I

ssue

7,O

ctob

er20

04,P

ages

543–

8

2004

Och

rato

xin

Aan

dafl

atox

ins

B1,

B2,

G1,

and

G2

HP

LCan

alyt

ical

met

hod

and

fluor

esce

nce

dete

ctio

nA

irsa

mpl

esw

orkp

lace

sof

aco

ffee

fact

ory

Tarı

n,an

dot

hers

Use

ofhi

gh-p

erfo

rman

celiq

uid

chro

mat

ogra

phy

toas

sess

airb

orne

myc

otox

ins.

Afla

toxi

nsan

doc

hrat

oxin

A.

JC

hrom

atog

rA

2004

Aug

27;

1047

(2):

235–

40

2004

Con

tinue

d



ab

le1

---C

on

tin

ue

d.

Qu

anti

fica

tio

nT

ype

of

Myc

oto

xin

sm

eth

od

foo

dA

uth

or

Art

icle

Ref

eren

ceY

ear

Bue

noan

dO

liver

Det

erm

inat

ion

ofafl

atox

ins

and

zear

alen

one

indi

ffere

ntcu

lture

med

ia

Met

hods

Mol

Bio

l20

04:1

33–7

2004

Fum

onis

inB

1(F

B1)

and

B2

(FB

2)

Flo

w-t

hrou

ghen

zym

eim

mun

oass

ayre

sults

com

pare

dw

ithva

lidat

edH

PLC

met

hod

Mai

zeP

aepe

nsan

dot

hers

Aflo

w-t

hrou

ghen

zym

eim

mun

oass

ayfo

rth

esc

reen

ing

offu

mon

isin

sin

mai

ze

Ana

lytic

aC

him

ica

Act

aV

olum

e52

3,Is

sue

2,11

Oct

ober

2004

,P

ages

229–

35

2004

Och

rato

xin

ALi

quid

chro

mat

ogra

phy

with

fluor

esce

nce

dete

ctio

nB

eepo

llen

for

cont

rol

purp

oses

corn

,w

heat

and

rice

grai

ns,a

ndel

even

liqui

dm

edia

Med

ina

and

othe

rsB

eepo

llen,

asu

bstr

ate

that

stim

ulat

esoc

hrat

oxin

apr

oduc

tion

byA

sper

gillu

sO

chra

ceus

wilh

.

Sys

tem

.App

l.M

icro

biol

.27,

261–

67(2

004)

2004

Afla

toxi

nsB

1,B

2,G

1,

G2

and

ochr

atox

inA

(OTA

)

HP

LCco

nditi

ons

ingr

adie

ntel

utio

nan

da

wav

elen

gth

prog

ram

for

the

sepa

ratio

nflu

orim

etric

quan

titat

ion

Bee

polle

nG

arci

a-V

illan

ova

and

othe

rsS

imul

tane

ous

imm

unoa

ffini

tyco

lum

ncl

eanu

pan

dH

PLC

anal

ysis

ofafl

atox

ins

and

ochr

atox

ina

insp

anis

hbe

epo

llen

JA

gric

Foo

dC

hem

,52

(24)

,723

5–72

39,

2004

2004

Afla

toxi

ns(A

fB1,

AfB

2,A

fG1,

AfG

2)an

dZ

eara

leno

ne(Z

EN

)O

TA,F

B1,

FB

2,Tr

icho

tece

nes:

one

byon

e

TLC

for

AF

and

ZE

Nan

dTr

icho

tece

nes:

HP

LCfo

rO

TAA

ndF

B1

FB

2

Med

icin

alhe

rbs,

Riz

zoan

dot

hers

Ass

essm

ento

ftox

igen

icfu

ngi

onA

rgen

tinea

nm

edic

inal

herb

s

Mic

robi

olog

ical

Res

earc

h15

9(2

004)

113–

20

2004

AF

B1

noni

nstr

umen

tal

imm

unofi

ltrat

ion-

base

das

say

devi

ceco

nsis

tsof

mem

bran

estr

ips,

with

antib

ody-

imm

obili

zed

zone

s,at

tach

edto

apo

lyet

hyle

neca

rd

Gro

undn

ut,c

orn,

whe

at,c

hees

e,an

dch

ili

Pal

and

Dha

rA

nan

alyt

ical

devi

cefo

ron

-site

imm

unoa

ssay

.de

mon

stra

tion

ofits

appl

icab

ility

inse

miq

uant

itativ

ede

tect

ion

ofaf

b1in

aba

tch

ofsa

mpl

esw

ithul

trah

igh

sens

itivi

ty

Ana

l.C

hem

.200

4,76

,98–

104

2004

Afla

toxi

nan

doc

hrat

oxin

one

byon

e

HP

LCR

awin

gred

ient

s,fin

ishe

dba

kery

prod

ucts

,equ

ipm

ent

surf

ace

swab

s,w

orke

rs’g

love

s,w

ater

used

inpr

oces

sing

lines

and

air

Al-Z

enki

1an

dot

hers

Eva

luat

ion

ofm

icro

bial

haza

rds

asso

ciat

edw

ithbr

ead

man

ufac

turin

gin

the

Sta

teof

Kuw

ait

2004

IFT

Ann

ual

Mee

ting,

July

12–1

6-

Las

Veg

as,

NV

2004

Sim

ulta

neou

sely

Afla

toxi

n,O

chra

toxi

nA

and

Zea

rale

none

Liqu

idch

rom

atog

raph

yw

ithflu

ores

cenc

ede

tect

ion

Rye

and

rice

Gob

elan

dLu

sky

Sim

ulta

neou

sde

term

inat

ion

ofafl

atox

in,o

chra

toxi

nA

and

zear

alen

one

ingr

ains

byne

wim

unoa

ffini

tyco

lum

n/liq

uid

chro

mat

ogra

phy

Jof

AO

AC

Int8

7(2)

411–

6M

ar-a

pr20

04

Con

tinue

d



ab

le1

---C

on

tin

ue

d.

Qu

anti

fica

tio

nT

ype

of

Myc

oto

xin

sm

eth

od

foo

dA

uth

or

Art

icle

Ref

eren

ceY

ear

Sim

ulta

neou

sde

tect

ion

ofafl

atox

ins

(AF

)an

doc

hrat

oxin

A(O

A)

Aut

omat

edH

PLC

met

hod

aque

ous

extr

acts

wer

eth

entr

ansf

erre

dto

anA

SP

EC

HP

LCsy

stem

for

auto

mat

edcl

eanu

pus

ing

Afla

Och

raim

mun

oaffi

nity

colu

mns

.OA

and

AF

wer

equ

antifi

edus

ing

HP

LCw

ithflu

ores

cenc

ede

tect

ion,

with

aru

ntim

eof

appr

oxim

atel

y40

min

.

Mai

zece

real

prod

ucts

and

pean

utbu

tter

Cha

nan

dot

hers

Sim

ulta

neou

sde

term

inat

ion

ofafl

atox

ins

and

ochr

atox

inA

info

odus

ing

afu

llyau

tom

ated

imm

unoa

ffini

tyco

lum

ncl

eanu

pan

dliq

uid

chro

mat

ogra

phy-

fluor

esce

nce

dete

ctio

n.

JC

hrom

atog

rA

2004

Dec

3;10

59(1

–2):

13–6

2004

Sim

ulta

neou

sde

tect

ion

ofth

eF

usar

ium

myc

otox

ins

fusa

prol

iferin

and

seve

ntr

icho

thec

enes

(GC

–MS

)G

rain

sJe

stoi

and

othe

rsA

naly

sis

ofth

eF

usar

ium

Myc

otox

ins

fusa

prol

iferin

and

tric

hoth

ecen

esin

grai

nsus

ing

gas

chro

mat

ogra

phy-

mas

ssp

ectr

omet

ry

JA

gric

Foo

dC

hem

2004

,52,

1464

–920

04

Och

rato

xin

A(O

TA)

and

fum

onis

inB

1(F

B1)

thre

edi

ffere

ntce

ll-lin

es,C

6gl

iom

ace

lls,C

aco-

2ce

llsan

dV

ero

cells

Cre

ppy

and

othe

rsS

yner

gist

icef

fect

sof

fum

onis

inB

1an

doc

hrat

oxin

A:a

rein

vitr

ocy

toto

xici

tyda

tapr

edic

tive

ofin

vivo

acut

eto

xici

ty?

Toxi

colo

gy20

1(2

004)

115–

2320

04

Tric

hoth

ecen

esD

ON

,N

IV,3

-ace

tylD

ON

and

Fus

aren

one

X

LC–M

Sm

etho

dsT

LCG

CLC

ELI

SA

Mol

ecul

arim

prin

ted

poly

mer

s(M

IP)

Cre

al,c

offe

eTr

icho

thec

enes

with

asp

ecia

lfo

cus

onD

ON

Sum

mar

yR

epor

tofa

Wor

ksho

phe

ldin

Sep

tem

ber

2003

ILS

IE

urop

eR

epor

tS

erie

s

2004

Cyc

lopi

azon

icac

id,

myc

ophe

nolic

acid

,te

nuaz

onic

acid

,and

ochr

atox

inA

HP

LCC

ornfl

ake

Are

sta

and

othe

rsS

imul

tane

ous

dete

rmin

atio

nof

ochr

atox

inA

and

cycl

opia

zoni

c,m

ycop

heno

lic,a

ndte

nuaz

onic

acid

sin

corn

flake

sby

solid

phas

em

icro

extr

actio

nco

uple

dto

HP

LC

JA

gric

Foo

dC

hem

2003

,51,

5232

–720

03

Sim

ulta

neou

sde

term

inat

ion

ofB

-tric

hoth

ecen

esan

dth

em

ajor

met

abol

ites

ofN

IV,

(DO

N),

(15-

AcD

ON

,(3

-AcD

ON

),fu

sare

non

X(F

us-X

)an

dde

-ep

oxyd

eoxy

niva

leno

l(D

OM

-1)

Hig

h-pe

rfor

man

celiq

uid

chro

mat

ogra

phy

(HP

LC),

com

bine

dw

ithat

mos

pher

icpr

essu

rech

emic

alio

nisa

tion

(AP

CI)

,mas

ssp

ectr

omet

ry(M

S),

Dex

amet

haso

ne(D

ex)

was

used

asin

tern

alst

anda

rd

Pig

urin

ean

dm

aize

sam

ples

Raz

zazi

-Faz

elia

ndot

hers

Sim

ulta

neou

sde

term

inat

ion

ofm

ajor

B-t

richo

thec

enes

and

the

de-e

poxy

-met

abol

iteof

deox

yniv

alen

olin

pig

urin

ean

dm

aize

usin

ghi

gh-p

erfo

rman

celiq

uid

chro

mat

ogra

phy–

mas

ssp

ectr

omet

ry

JC

hrom

atog

rB

,796

(200

3)21

–33

2003

Con

tinue

d



ab

le1

---C

on

tin

ue

d.

Qu

anti

fica

tio

nT

ype

of

Myc

oto

xin

sm

eth

od

foo

dA

uth

or

Art

icle

Ref

eren

ceY

ear

Afla

toxi

nB

1(A

fB1)

Rad

ioim

mun

oass

aay

(RIA

)A

ntia

flato

xin

B1

seru

mw

asra

ised

in-h

ouse

usin

gA

fB1-

bovi

nese

rum

albu

min

conj

ugat

eas

imm

unog

en

Agr

icul

tura

lco

mm

oditi

esR

ice

Whe

atS

oybe

an

Kor

dean

dot

hers

Dev

elop

men

tofa

radi

oim

mun

oass

aypr

oced

ure

for

aflat

oxin

B1

mea

sure

men

t

JA

gric

Foo

dC

hem

2003

,51:

843–

620

03

Och

rato

xin

AH

PLC

MS

anal

yzed

ona

narr

ow-b

ore

reve

rsed

-pha

seC

18H

PLC

colu

mn

with

acet

onitr

ile/

wat

er(0

.1%

form

icac

id)

(40:

60)

asm

obile

phas

ean

dqu

antifi

edw

itha

fluor

esce

nce

dete

ctor

OTA

was

confi

rmed

bysi

ngle

-qua

drup

leM

Sus

ing

anel

ectr

ospr

ayio

niza

tion

sour

ce

Gre

enan

dro

aste

dco

ffee

Ven

tora

and

othe

rsA

naly

sis

ofoc

hrat

oxin

Ain

coffe

eby

solid

phas

ecl

eanu

pan

dna

rrow

-bor

eliq

uid

chro

mat

ogra

phy-

fluor

esce

nce

dete

ctor

-mas

ssp

ectr

omet

ry

JA

gric

Foo

dC

hem

2003

,51:

7564

–67

2003

AF

B1,

ZE

N,O

TA,D

ON

,an

dfu

mun

osin

B1

Imm

obili

satio

non

the

CM

5se

nsor

surf

ace

took

plac

eus

ing

am

odi.c

atio

nof

the

stan

dard

ED

C–N

HS

reac

tion

Adi

amin

esp

acer

was

coup

led

toa

ED

C–N

HS

activ

ated

CM

5-se

nsor

chip

afte

rw

hich

ED

C–N

HS

activ

ated

a.at

oxin

orze

aral

enon

ew

ere

inje

cted

.G

C,H

PLC

Gaa

gan

dot

hers

Bio

sens

ors

and

mul

tiple

myc

otox

inan

alys

isF

ood

Con

trol

14(2

003)

251–

5420

03

Fum

onis

ins

Bio

assa

ysre

view

Fun

galc

ultu

res,

cere

als

Gut

leb

and

othe

rsC

ytot

oxic

ityas

says

for

myc

otox

ins

prod

uced

byF

usar

ium

stra

ins:

are

view

Env

ironm

enta

lTo

xico

logy

and

Pha

rmac

olog

yV

olum

e11

,Iss

ues

3-4,

July

2002

,P

ages

309–

20

2002

Mai

nty

peA

-tric

hoth

ecen

essu

chas

T-2

Toxi

n,H

T-2

Toxi

n,ac

etyl

T-2

Toxi

n,di

acet

oxys

cirp

enol

,m

onoa

ceto

xysc

ir-pe

nol(

15-

acet

oxys

cirp

enol

)an

dne

osol

anio

l

HP

LCliq

uid

chro

mat

ogra

phy

and

atm

osph

eric

pres

sure

chem

ical

ioni

zatio

nm

ass

spec

trom

etry

coup

ling

ofLC

–MS

Oat

s,m

aize

,bar

ley,

and

whe

atsa

mpl

esR

azza

zi-F

azel

iand

othe

rsS

imul

tane

ous

quan

tifica

tion

ofA

-tric

hoth

ecen

em

ycot

oxin

sin

grai

nsus

ing

liqui

dch

rom

atog

raph

y–at

mos

pher

icpr

essu

rech

emic

alio

niza

tion

mas

ssp

ectr

omet

ry

968

(200

2)12

9–42

JC

hrom

atog

rA

,20

02

Con

tinue

d



ab

le1

---C

on

tin

ue

d.

Qu

anti

fica

tio

nT

ype

of

Myc

oto

xin

sm

eth

od

foo

dA

uth

or

Art

icle

Ref

eren

ceY

ear

Och

rato

xin

Aan

dze

aral

enon

eH

PLC

fluor

esce

nce

dete

ctio

n.W

heat

,rye

,bar

ley,

and

oat

Esk

ola

and

othe

rsA

pplic

atio

nof

man

uala

ndau

tom

ated

syst

ems

for

purifi

catio

nof

ochr

atox

inA

and

zear

alen

one

ince

real

sw

ithim

mun

oaffi

nity

colu

mns

JA

gric

Foo

dC

hem

2002

,50:

41–7

2002

Och

rato

xin

A(O

A)

and

T-2

toxi

nM

embr

ane-

base

dflo

w-t

hrou

ghen

zym

eim

mun

oass

ayre

sults

confi

rmed

byH

PLC

-flu

ores

cenc

ean

dby

GC

_MS

Cer

eals

(whe

at,r

ye,

mai

ze,b

arle

y)D

eS

aege

ran

dot

hers

Aco

llabo

rativ

est

udy

tova

lidat

eno

velfi

eld

imm

unoa

ssay

kits

for

rapi

dm

ycot

oxin

dete

ctio

n

IntJ

Foo

dM

icro

biol

Vol

.75,

Issu

es1–

2,P

ages

135–

42

2002

Afla

toxi

nF

ully

auto

mat

edta

ndem

MS

,w

ithau

tosa

mpl

eran

din

ject

ion

atat

mos

pher

icpr

essu

re,w

asav

aila

ble.

Pea

nut

Sch

atzk

iand

Had

don

Rap

id,n

onde

stru

ctiv

ese

lect

ion

ofpe

anut

sfo

rhi

ghafl

atox

inco

nten

tby

soak

ing

and

tand

emm

ass

spec

trom

etry

JA

gric

Foo

dC

hem

2002

,50,

3062

–69

2002

Afla

toxi

nsH

PLC

,fluo

rom

etry

,ELI

SA

Tahi

ni,a

sesa

me

butte

rN

ilufe

ran

dB

oyac

iogl

uC

ompa

rativ

eS

tudy

ofT

hree

Diff

eren

tMet

hods

for

the

Det

erm

inat

ion

ofA

flato

xins

inTa

hini

JA

gric

Foo

dC

hem

2002

,50:

3375

–79

2002

Afla

toxi

nsan

doc

hrat

oxin

AT

hin-

laye

rch

rom

atog

raph

y,an

dth

enqu

antifi

edw

ithflu

ores

cenc

e.

Pea

nuts

and

itspr

oduc

ts,n

uts,

mai

ze,o

atan

d/or

whe

atpr

oduc

ts,r

ice

and

bean

s

Cal

das

and

othe

rsA

flato

xins

and

ochr

atox

inA

info

odan

dris

ksto

hum

anhe

alth

Rev

Sau

deP

ublic

a.20

02Ju

n;36

(3):

319–

23

2002

Afla

toxi

nR

apid

fluor

esce

nce

pola

rizat

ion

(FP

)as

say

com

pare

dw

ithH

PLC

resu

lts.

Gra

ins

corn

,sor

ghum

,pe

anut

butte

r,an

dpe

anut

past

e

Nas

iran

dJo

lley

Dev

elop

men

tofa

fluor

esce

nce

pola

rizat

ion

assa

yfo

rth

ede

term

inat

ion

ofafl

atox

ins

ingr

ains

JA

gric

Foo

dC

hem

2002

,50,

3116

–21

2002

Och

rato

xin

A(O

A)

Mem

bran

e-ba

sed

flow

-thr

ough

enzy

me

imm

unoa

ssay

flow

-thr

ough

enzy

me

imm

unoa

ssay

and

HP

LCm

etho

ds.

Roa

sted

coffe

eS

iban

daan

dot

hers

Dev

elop

men

tofa

solid

phas

ecl

eanu

pan

dpo

rtab

lera

pid

flow

-thr

ough

enzy

me

imm

unoa

ssay

for

the

dete

ctio

nof

ochr

atox

inA

inro

aste

dco

ffee

JA

gric

Foo

dC

hem

2002

,50:

6964

–67

2002

Afla

toxi

nsB

1,B

2,G

1an

dG

2,ze

aral

enon

e,ci

trin

in,

deox

yniv

alen

ol,a

ndoc

hrat

oxin

A

Mul

ti-m

ycot

oxin

thin

-laye

rch

rom

atog

raph

ysc

reen

ing

met

hod

and

toxi

nsw

ere

quan

tiR©

edby

high

-per

form

ance

liqui

dch

rom

atog

raph

y.

Bre

wed

alco

holic

beve

rage

s,be

erO

dhav

and

Nai

cker

Myc

otox

ins

inS

outh

Afr

ican

trad

ition

ally

brew

edbe

ers

Foo

dA

dditi

ves

and

Con

tam

inan

ts,2

002,

Vol

.19,

No.

1,55

–61

2002

Con

tinue

d



ab

le1

---C

on

tin

ue

d.

Qu

anti

fica

tio

nT

ype

of

Myc

oto

xin

sm

eth

od

foo

dA

uth

or

Art

icle

Ref

eren

ceY

ear

OTA

Thi

n-la

yer

chro

mat

ogra

phic

(TLC

)sc

reen

ing

met

hod

dete

ctio

nby

visu

ales

timat

ion

offlu

ores

cenc

ein

tens

ityun

der

aU

Vla

mp

at36

6nm

.Con

firm

byby

aqu

antit

ativ

eim

mun

oaffi

nity

/HP

LCm

etho

d.

Gre

enco

ffee

Pitt

etan

dR

oyer

Rap

id,l

owco

stth

in-la

yer

chro

mat

ogra

phic

scre

enin

gm

etho

dfo

rth

ede

tect

ion

ofoc

hrat

oxin

ain

gree

nco

ffee

ata

cont

roll

evel

of10

μg/

kg

JA

gric

Foo

dC

hem

2002

,50,

243–

4720

02

AF

M1

ELI

SA

Hig

h-tit

erra

bbit

poly

clon

alan

tibod

ies

toafl

atox

inM

1w

ere

prod

uced

byut

ilizi

ngA

FM

1-bo

vine

seru

mal

bum

in(B

SA

)co

njug

ate

asan

imm

unog

en.

Milk

Dev

iand

othe

rsD

evel

opm

enta

ndap

plic

atio

nof

anin

dire

ctco

mpe

titiv

een

zym

e-lin

ked

imm

unoa

ssay

for

aflat

oxin

M1

inm

ilkan

dm

ilk-b

ased

conf

ectio

nery

JA

gric

Foo

dC

hem

2002

,50:

933–

720

02

Val

idat

ion

ofan

alyt

ical

met

hods

for

dete

rmin

ing

myc

otox

ins

info

odst

uffs

tren

dsin

anal

ytic

alch

emis

try,

vol.

21,

no.6

+7,

2002

2002

Afla

toxi

nsan

dF

usar

ium

toxi

nson

eby

one

Afla

toxi

nsby

HP

LC(a

Jasc

oP

U-9

80pu

mp

with

aJa

sco

AS

-950

auto

sam

pler

)w

itha

Shi

mad

zuR

F-1

0X

Lspe

ctro

fluor

omet

erw

ithex

cita

tion/

emis

sion

wav

elen

gths

253

nm/4

15nm

afte

rde

rivat

izat

ion

with

trifl

uoro

acet

icac

id.

Shi

mad

zuG

C/M

S-Q

P50

00w

ithse

lect

edio

nm

onito

ring

for

Tric

hoth

ecen

es.

Zea

rale

none

was

anal

yzed

byH

PLC

fluor

esce

nce

dete

ctor

Cor

nQ

inLi

and

othe

rsA

flato

xins

and

Fum

onis

ins

inco

rnfr

omth

ehi

gh-in

cide

nce

area

for

hum

anhe

pato

cellu

lar

carc

inom

ain

Gua

ngxi

,C

hina

JA

gric

Foo

dC

hem

2001

,49:

4122

–26

2001

Afla

toxi

nB

1an

doc

hrat

oxin

AR

IAm

etho

dR

adio

Imm

iuno

chem

ical

met

hod

Whe

atan

dba

rely

Sed

mik

ova

and

othe

rsP

oten

tialh

azar

dof

sim

ulta

neou

soc

curr

ence

ofafl

atox

inB

1an

doc

hrat

oxin

A

Vet

Med

–C

zech

46,

2001

(6):

169–

7420

01

AF

B1

Mai

zean

imal

Lem

kean

dot

hers

Dev

elop

men

tofa

mul

titie

red

appr

oach

toth

ein

vitr

opr

escr

eeni

ngof

clay

-bas

eden

tero

sorb

ents

Ani

mal

Fee

dS

cien

cean

dTe

chno

logy

Vol

ume

93,I

ssue

s1–

2,17

Pag

es17

–29

2001

Con

tinue

d



ab

le1

---C

on

tin

ue

d.

Qu

anti

fica

tio

nT

ype

of

Myc

oto

xin

sm

eth

od

foo

dA

uth

or

Art

icle

Ref

eren

ceY

ear

Sim

ulta

neou

sac

etyl

T-2

toxi

n,T-

2to

xin,

HT-

2to

xin,

T-2

trio

l,T-

2te

trao

l,ne

osol

anio

l,is

o-ne

osol

anio

l,sc

irpe

ntrio

l,4,

15-

diac

etox

ysci

rpen

ol,

15-a

ceto

xysc

irpe

nol,

4-ac

etox

ysci

rpen

trio

l,N

IV,f

usar

enon

-X,

DO

N,1

5-ac

etyl

-DO

Nan

d3-

acet

yl-D

ON

GC

sim

ulta

neou

sfu

llsc

anan

dta

ndem

mas

ssp

ectr

omet

ricde

tect

ion

nega

tive

ion

chem

ical

ioni

satio

n(N

ICI)

GC

–MS

for

mol

ecul

arm

ass

dete

rmin

atio

nve

rifica

tion

Fun

galc

ultu

res

Nie

lsen

and

Thr

ane

Fast

met

hods

for

scre

enin

gof

tric

hoth

ecen

esin

fung

alcu

lture

sus

ing

gas

chro

mat

ogra

phy–

tand

emm

ass

spec

trom

etry

Jour

nalo

fC

hrom

atog

raph

yA

Vol

ume

929,

Issu

es1–

2,21

Sep

tem

ber

2001

,Pag

es75

–87

2001

Sim

ulta

neou

sde

term

inat

ion

ofafl

atox

ins

(G1,

G2,

B1,

B2)

citr

inin

ean

doc

hrat

oxin

A

Rev

erse

d-ph

ase

HP

LCse

para

tion

with

tand

emm

ass

spec

trom

etric

iden

tifica

tion

and

quan

tifica

tion

usin

gel

ectr

ospr

ayio

nisa

tion

ona

quad

rupo

leio

ntr

apm

ass

anal

yser

(ES

I-M

S-M

S).

The

HP

LCse

para

tion

was

run

onlin

ew

ithth

eE

SI-

MS

-MS

dete

ctio

n

Tuom

iand

othe

rsD

etec

tion

ofafl

atox

ins

(G(1

-2),

B(1

-2))

,st

erig

mat

ocys

tin,c

itrin

ine,

and

ochr

atox

inA

insa

mpl

esco

ntam

inat

edby

mic

robe

s

Ana

lyst

2001

Sep

;12

6(9)

:154

5–50

2001

Afla

toxi

nsB

1,B

2,G

1,G

2,ze

aral

enon

e,an

dfu

mon

isin

B1

In-h

ouse

valid

ated

met

hods

Unp

roce

ssed

corn

sam

ples

Var

gas

and

othe

rsC

o-oc

curr

ence

ofafl

atox

ins

B1,

B2,

G1,

G2,

zear

alen

one

and

fum

onis

inB

1in

Bra

zilia

nco

rn

Foo

dA

ddit

Con

tam

.20

01N

ov;1

8(11

):98

1–6

2001

Afla

toxi

nM

1an

doc

hrat

oxin

A(O

TA)

Det

erm

inat

ion

byH

PLC

fluor

esce

nce

dete

ctor

Milk

Sur

vey

ofm

ilkfo

rm

ycot

oxin

s(n

r17

/01)

Foo

dS

urve

yIn

form

atio

nS

heet

Frid

ay14

Sep

tem

ber

2001

2001

Och

rato

xin

A(O

TA)

HP

LCon

aC

18co

lum

nw

ithgr

adie

ntel

utio

nan

dqu

antit

atio

nat

333

nmby

mea

nsof

aph

otod

iode

arra

yde

tect

or.s

econ

dm

etho

dut

ilize

dga

sch

rom

atog

raph

yw

ithm

ass

sele

ctiv

ede

tect

ion

mon

itorin

gei

ghts

peci

ficio

ns

Win

esan

dbe

ers,

Sol

eas

and

othe

rsA

ssay

ofoc

hrat

oxin

Ain

win

ean

dbe

erby

high

-pre

ssur

eliq

uid

chro

mat

ogra

phy

phot

odio

dear

ray

and

gas

chro

mat

ogra

phy

mas

sse

lect

ive

dete

ctio

n

JA

gric

Foo

dC

hem

2001

,49:

2733

–40

2001

Con

tinue

d



ab

le1

---C

on

tin

ue

d.

Qu

anti

fica

tio

nT

ype

of

Myc

oto

xin

sm

eth

od

foo

dA

uth

or

Art

icle

Ref

eren

ceY

ear

Afla

toxi

nB

1(A

FT

B1)

,an

dfu

mon

isin

B1

(FB

1)on

eby

one

AF

TB

1T

LC,a

ndF

B1

leve

lsby

aB

ond-

Elu

tSA

Xca

rtrid

gean

dH

PLC

.TLC

Whi

tean

dye

llow

corn

.M

arty

nez

and

Mar

tyne

zM

old

occu

rren

cean

dafl

atox

inB

1an

dfu

mon

isin

B1

dete

rmin

atio

nin

corn

sam

ples

inV

enez

uela

JA

gric

Foo

dC

hem

2000

,48:

2833

–36

2000

Och

rato

xin

A(O

TA)

Con

firm

edby

HP

LCw

ithflu

ores

cenc

ede

tect

ion

Mic

robi

alm

edia

Sta

nder

and

othe

rsS

cree

ning

ofco

mm

erci

alhy

drol

ases

for

the

degr

adat

ion

ofoc

hrat

oxin

a

JA

gric

Foo

dC

hem

2000

,48:

5736

–39

2000

T-2

toxi

nM

embr

aneb

ased

flow

-thr

ough

enzy

me

imm

unoa

ssay

Imm

unod

yne

AB

Cm

embr

ane

was

coat

edw

ith2

ILof

goat

anti-

hors

erad

ish

pero

xida

se(H

RP

)ra

bbit

anti-

mou

se(t

ests

pot)

(und

ilute

d)im

mun

oglo

bulin

s,an

dth

efr

eebi

ndin

gsi

tes

wer

ebl

ocke

d.In

addi

tion

toth

ean

tibod

y-co

ated

Imm

unod

yne

AB

Cm

embr

ane

Cer

eals

Sib

anda

and

othe

rsD

etec

tion

ofT-

2to

xin

indi

ffere

ntce

real

sby

flow

-thr

ough

enzy

me

imm

unoa

ssay

with

asi

mul

tane

ous

inte

rnal

refe

renc

e

JA

gric

Foo

dC

hem

2000

,48:

5864

–67

2000

P.ci

trin

um(2

5is

olat

es)

citr

inin

and

tanz

awai

cac

idA

, P.

stec

kii (

18is

olat

es)

isoc

hrom

anto

xins

(exc

ept2

)ta

nzaw

aic

acid

E, P

.siz

ovae

tanz

awai

cac

idA

,P.

cory

loph

ilum

(10

isol

ates

)ci

treo

isoc

oum

arin

ol,

P.su

mat

rens

e(1

5is

olat

es)

curv

ular

in

Car

boxy

licac

ids

and

the

benz

opyr

anw

ere

iden

tified

onth

eba

sis

ofm

ass

spec

trom

etry

,and

one

and

two

dim

ensi

onal

NM

Rsp

ectr

osco

pic

tech

niqu

es

Sec

onda

rym

etab

olite

sch

arac

teris

ticof

Pen

icill

ium

citr

inum

,Pen

icill

ium

stec

kii,

and

rela

ted

spec

ies

Phy

toch

emis

try

Vol

ume

54,I

ssue

3,1

June

2000

,Pag

es30

1–9

2000

Afla

toxi

nsB

1,B

2,G

1an

dG

2,oc

hrat

oxin

A,z

eara

leno

nean

dfu

mon

isin

sB

1,B

2an

dB

3

Ful

lyva

lidat

edan

alyt

ical

HP

LCm

etho

dsR

awm

aize

asre

ceiv

edat

port

sor

atm

ajor

mai

zem

ills

Scu

dam

ore

and

Pat

elS

urve

yfo

rafl

atox

ins,

ochr

atox

inA

,zea

rale

none

and

fum

onis

ins

inm

aize

impo

rted

into

the

Uni

ted

Kin

gdom

.

Foo

dA

ddit

Con

tam

.20

00M

ay;1

7(5)

:407

–16

2000

Och

rato

xin

A(O

A)

Enz

yme-

linke

dim

mun

osor

bent

assa

y(E

LIS

A),

and

dete

cted

OA

conc

entr

atio

nsup

to0.

1ng

/mL.

Chi

lies,

Thi

rum

ala-

Dev

iand

othe

rsP

rodu

ctio

nof

poly

clon

alan

tibod

ies

agai

nst

ochr

atox

inA

and

itsde

tect

ion

inch

ilies

byE

LIS

A

JA

gric

Foo

dC

hem

2000

,48:

5079

–82

2000

Con

tinue

d



ab

le1

---C

on

tin

ue

d.

Qu

anti

fica

tio

nT

ype

of

Myc

oto

xin

sm

eth

od

foo

dA

uth

or

Art

icle

Ref

eren

ceY

ear

Afla

toxi

nsB

1,B

2,an

dG

1an

dth

ech

oler

ato

xin

A-s

ubun

it

Cap

illar

yel

ectr

okin

etic

chro

mat

ogra

phy

with

mul

tipho

ton-

exci

ted

fluor

esce

nce

Wei

and

othe

rsD

eter

min

atio

nof

biol

ogic

alto

xins

usin

gca

pilla

ryel

ectr

okin

etic

chro

mat

ogra

phy

with

mul

tipho

ton-

exci

ted

fluor

esce

nce

Ana

lChe

m20

00,

72:1

360–

6320

00

Afla

toxi

nan

dfu

mon

isin

one

byon

eA

flato

xins

B1,

B2,

G1,

and

G2

by(T

LC),

FB

1,F

B2

byH

PLC

fluor

esce

nce

Sor

ghum

daS

ilva

and

othe

rsM

ycofl

ora

and

occu

rren

ceof

aflat

oxin

B1

and

fum

onis

inB

1du

ring

stor

age

ofB

razi

lian

sorg

hum

JA

gric

Foo

dC

hem

2000

,48:

4352

–56

2000

Och

rato

xin

Aan

dci

trin

inE

nzym

eim

mun

oass

ays

(EIA

),O

chra

toxi

nA

-pos

itive

resu

ltsw

ere

confi

rmed

byH

PLC

afte

rim

mun

oaffi

nity

chro

mat

ogra

phy

Cer

eals

ampl

esS

ampl

ing

incl

uded

food

s(w

heat

,cor

n)an

dfe

eds

(bar

ley,

oats

,whe

atbr

an)

Vra

bche

vaan

dot

hers

Co-

occu

rren

ceof

ochr

atox

ina

and

citr

inin

ince

real

sfr

omB

ulga

rian

villa

ges

with

ahi

stor

yof

Bal

kan

ende

mic

neph

ropa

thy

JA

gric

Foo

dC

hem

2000

,48:

2483

–88

2000

8-ke

totr

icho

thec

enes

,(Z

EA

),an

dfu

mon

isin

s,in

clud

ing

FB

1,F

B2,

FB

3,D

ON

),15

-ace

tyld

eoxy

NIV

(15-

AD

ON

),3-

acet

ylde

oxyN

IV,(

3-A

DO

N),

niva

leno

l(N

IV),

and

4-ac

etyl

NIV

(4-A

NIV

),

Cor

nS

ohn

and

othe

rsC

o-oc

curr

ence

ofF

usar

ium

myc

otox

ins

inm

ould

yan

dhe

alth

yco

rnfr

omK

orea

Foo

dA

ddit

Con

tam

.19

99A

pr;1

6(4)

:153

–8

1999

Och

rato

xin

A(O

TA)

and

aflat

oxin

s(A

Fs)

Rev

erse

d-ph

ase

liqui

dch

rom

atog

raph

y(L

C)

with

fluor

esce

nce

dete

ctio

n

Japa

nese

beer

sam

ples

Nak

ajim

aan

dot

hers

Asu

rvey

ofoc

hrat

oxin

Aan

dafl

atox

ins

indo

mes

tican

dim

port

edbe

ers

inJa

pan

byim

mun

oaffi

nity

and

liqui

dch

rom

atog

raph

y.

JA

OA

CIn

t199

9Ju

l-Aug

;82

(4):

897–

902.

1999

Zea

rale

none

,de

oxyn

ival

enol

and

aflat

oxin

s,fu

mon

isin

son

eby

one

Zea

rale

none

,deo

xyni

vale

nol

and

aflat

oxin

sby

TLC

and

fum

onis

ins

(FB

1,F

B2,

and

FB

3)by

HP

LC

Cor

n-ba

sed

food

sS

olov

eyan

dot

hers

Asu

rvey

offu

mon

isin

s,de

oxyn

ival

enol

,ze

aral

enon

ean

dafl

atox

ins

cont

amin

atio

nin

corn

-bas

edfo

odpr

oduc

tsin

Arg

entin

a

1999

Afla

toxi

nsfu

mon

isin

str

icho

thec

enes

and

zear

alen

one

(ZE

A)

HP

LC,G

C_M

SC

orn

sam

ples

Ali

and

othe

rsN

atur

alco

-occ

urre

nce

ofafl

atox

ins

and

Fus

ariu

mm

ycot

oxin

s(f

umon

isin

s,de

oxyn

ival

enol

,niv

alen

olan

dze

aral

enon

e)in

corn

from

Indo

nesi

a.

Foo

dA

ddit

Con

tam

.19

98M

ay-

Jun;

15(4

):37

7–84

1998

Con

tinue

d



ab

le1

---C

on

tin

ue

d.

Qu

anti

fica

tio

nT

ype

of

Myc

oto

xin

sm

eth

od

foo

dA

uth

or

Art

icle

Ref

eren

ceY

ear

Afla

toxi

nA

vaila

ble

AO

AC

Met

hods

swith

slig

htm

odifi

catio

nsfo

rth

ere

cove

ryof

aflat

oxin

sU

sing

the

HP

LCan

dpo

stco

lum

nde

rivat

izat

ion

proc

edur

e

Dat

epa

lmA

hmed

and

Rob

inso

nS

elec

tion

ofa

suita

ble

met

hod

for

anal

ysis

ofafl

atox

ins

inda

tefr

uits

JA

gric

Foo

dC

hem

1998

,46:

580–

419

98

(DO

N),

3-ac

etyl

DO

N,

15-

acet

ylD

ON

,fu

sare

none

X(F

X),

T-2

Toxi

n(T

-2),

diac

etox

ysci

rpen

ol(D

AS

),(Z

EA

),fB

1,A

FB

1,O

TA,a

ndci

trin

in(C

T)

Ana

lyze

dby

enzy

me

imm

unoa

ssay

s3,

15-d

iace

tylD

ON

was

dete

cted

inso

me

sam

ples

byH

PLC

-EIA

anal

ysis

Whe

atm

aize

asfe

edC

urtu

iand

othe

rsA

surv

eyon

the

occu

rren

ceof

myc

otox

ins

inw

heat

and

mai

zefr

omw

este

rnR

oman

ia.

Myc

opat

holo

gia

1998

;14

3(2)

:97–

103

1998

Afla

toxi

ns,f

umon

isin

B1,

and

zear

alen

one

one

byon

e

Sor

ghum

,mai

ze,

pean

uts,

pean

utbu

tter,

puls

es(c

owpe

asbe

ans)

Sia

me

and

othe

rsO

ccur

renc

eof

aflat

oxin

s,fu

mon

isin

B1,

and

zear

alen

one

info

ods

and

feed

sin

Bot

swan

a.

JF

ood

Pro

t.19

98D

ec;6

1(12

):16

70–3

1998

AF

B1,

B2,

G1,

G2,

OTA

,Z

EA

,T2-

toxi

n,P

enic

ilic

acid

TLC

with

pre-

coat

edgl

ass

plat

es(2

0×

20cm

ofsi

lica

gelD

.G.6

0M

erck

,D

arm

stad

t)

Med

icin

alpl

ant

sam

ples

and

spic

esA

ziz

and

othe

rsC

onta

min

atio

nof

som

eco

mm

onm

edic

inal

plan

tsa

mpl

esan

dsp

ices

byfu

ngi

and

thei

rm

ycot

oxin

s

Azi

zet

al.o

Med

icin

alpl

ant,

spic

es,B

otB

ull

Aca

dS

in(1

998)

39:2

79–8

5

1998

Afla

toxi

nsB

1,B

2,G

1an

dG

2,oc

hrat

oxin

sA

and

B,c

itrin

in,

cycl

opia

zoni

cac

id,

zea,

ster

igm

atoc

ystin

,D

ON

,niv

ltog

ethe

rw

ithse

ven

rela

ted

richo

thec

ene

myc

otox

ins,

fum

onis

ins

B1

and

B2

mon

ilifo

rmin

Ana

lytic

alm

etho

dsM

aize

glut

enan

dot

her

mai

zepr

oduc

tsus

edin

the

anim

alfe

edin

dust

ry

Scu

dam

ore

and

othe

rsM

ycot

oxin

sin

ingr

edie

nts

ofan

imal

feed

ing

stuf

fs:I

I.D

eter

min

atio

nof

myc

otox

ins

inm

aize

and

mai

zepr

oduc

ts.

Foo

dA

ddit

Con

tam

.19

98Ja

n;15

(1):

30–5

5

1998

Afla

toxi

ns,o

chra

toxi

nA

,and

fum

onis

ins.

zear

alen

one,

and

deox

yniv

alen

ol.

Fur

ther

sepa

ratio

nca

nbe

perf

orm

edw

ithIA

C,

follo

wed

byliq

uid

chro

mat

ogra

phic

(LC

)qu

antit

atio

n,ei

ther

off-

line

oron

line

inan

auto

mat

edsy

stem

,or

byflu

orom

etry

.

10gr

ains

Reg

ener

atio

nof

IAC

sfo

rre

use

inafl

atox

in,o

chra

toxi

nA

,fum

onis

in,a

ndze

aral

enon

ean

alys

esha

sbe

enin

vest

igat

ed

Sco

ttan

dTr

ucks

ess

App

licat

ion

ofim

mun

oaffi

nity

colu

mns

tom

ycot

oxin

anal

ysis

JA

OA

CIn

t199

7S

ep–O

ct;

80(5

):94

1–9

1997

Fum

onis

inB

1an

dafl

atox

inB

1.on

eby

one

FB

1:(H

PLC

)on

are

vers

e-ph

ase

colu

mn

AF

B1

:de

rivat

izat

ion

with

trifl

uoro

acet

icac

id.T

hede

rivat

ive

was

dete

cted

byH

PLC

anal

ysis

B1

Rai

n-af

fect

edso

rghu

m,

rain

-affe

cted

mai

ze,

norm

alm

aize

,no

rmal

sorg

hum

,and

poul

try

feed

She

ttyan

dB

hat

Nat

ural

occu

rren

ceof

fum

onis

inB

1an

dits

co-o

ccur

renc

ew

ithafl

atox

inB

1in

indi

anso

rghu

m,

mai

ze,a

ndpo

ultr

yfe

eds

JA

gric

Foo

dC

hem

1997

,45:

2170

–173

1997

Con

tinue

d



Ta

ble

1---

Co

nti

nu

ed

.

Qu

anti

fica

tio

nT

ype

of

Myc

oto

xin

sm

eth

od

foo

dA

uth

or

Art

icle

Ref

eren

ceY

ear

Afla

toxi

nB

1C

apill

ary

elec

trop

hore

sis

(CE

)C

Em

etho

dw

asco

mpa

red

toan

esta

blis

hed

HP

LCm

etho

d

Cor

nM

arag

os∗

and

Gre

erA

naly

sis

ofafl

atox

inB

1in

corn

usin

gca

pilla

ryel

ectr

opho

resi

sw

ithla

ser-

indu

ced

fluor

esce

nce

dete

ctio

n

JA

gric

Foo

dC

hem

1997

,45:

4337

–41

1997

Afla

toxi

nsB

1,B

2,G

1an

dG

2an

doc

hrat

oxin

A,

fum

onis

ins

B1

and

B2

sim

ulta

neou

sde

term

inat

ion

ofafl

atox

ins

and

ochr

atox

inA

HP

LCD

ryce

real

-bas

edpe

tfo

ods

and

wild

bird

food

Scu

dam

ore

and

othe

rsD

eter

min

atio

nof

myc

otox

ins

inpe

tfoo

dsso

ldfo

rdo

mes

ticpe

tsan

dw

ildbi

rds

usin

glin

ked-

colu

mn

imm

unoa

ssay

clea

nup

and

HP

LC

Foo

dA

ddit

Con

tam

.19

97F

eb-

Mar

;14(

2):1

75–8

6

1997

Och

rato

xin

A(O

A)

and

aflat

oxin

sA

naly

sis

was

perf

orm

edby

high

-per

form

ance

liqui

dch

rom

atog

raph

y(H

PLC

),w

ithflu

ores

cenc

ede

tect

ion

and

acet

onitr

ile/w

ater

/ace

ticac

idm

obile

phas

e(b

ased

onm

etho

dby

Sha

rman

etal

.199

2)

Cer

eals

and

ava

riety

ofre

tail

prod

ucts

Sur

vey

ofafl

atox

ins

and

ochr

atox

ina

ince

real

san

dre

tail

prod

ucts

Foo

dsu

rvei

llanc

ein

form

atio

nsh

eet

No.

130

Nov

embe

r19

97

1997

Fum

onis

ins

Cor

nliv

eran

dki

dney

ofra

tN

orre

dan

dot

hers

Tim

e-an

ddo

se-r

espo

nse

effe

cts

ofth

em

ycot

oxin

,fu

mon

isin

B1

onsp

hing

oid

base

elev

atio

nsin

prec

isio

n-cu

trat

liver

and

kidn

eysl

ices

Toxi

colo

gyin

Vitr

oV

olum

e10

,Iss

ue3,

June

1996

,Pag

es34

9–58

1996

Afla

toxi

nsan

doc

hrat

oxin

AM

aize

-bas

edgr

uels

Oye

lam

iand

othe

rsA

flato

xins

and

ochr

atox

inA

inth

ew

eani

ngfo

odof

Nig

eria

nch

ildre

n.

Ann

Trop

Pae

diat

r.19

96Ju

n;16

(2):

137–

40

1996

Och

rato

xin

A(O

A)

Com

petit

ive

enzy

me-

linke

dim

mun

osor

bent

assa

y(E

LIS

A)

with

mon

oclo

nal

antib

ody

HP

LCflu

ores

cenc

ede

tect

orto

confi

rm

Diff

eren

tcer

eals

.B

arna

-Vet

roan

dot

hers

Sen

sitiv

eE

LIS

Ate

stfo

rde

term

inat

ion

ofoc

hrat

oxin

A

JA

gric

Foo

dC

hem

1996

,44:

4071

–74

1996

Afla

toxi

nsS

cien

tifica

llyop

erat

edch

arge

-cou

pled

devi

ce(C

CD

)hi

gh-p

erfo

rman

ceth

in-la

yer

chro

mat

ogra

phic

(HP

TLC

)F

luor

esce

nce

exci

tatio

nof

the

aflat

oxin

sw

asac

com

plis

hed

with

anul

trav

iole

ttra

nsill

umin

ator

,w

hich

caus

edth

ean

alyt

esof

inte

rest

toem

itin

the

blue

gree

npo

rtio

nof

the

visi

ble

spec

trum

Pea

nutb

utte

rsa

mpl

esLi

ang

and

othe

rsQ

uant

itativ

ean

alys

isof

aflat

oxin

sby

high

-per

form

ance

thin

-laye

rch

rom

atog

raph

yut

ilizi

nga

scie

ntifi

cally

oper

ated

char

ge-c

oupl

edde

vice

dete

ctor

Ana

lChe

m19

96,

68:3

885–

9119

96

Con

tinue

d



Ta

ble

1---

Co

nti

nu

ed

.

Qu

anti

fica

tio

nT

ype

of

Myc

oto

xin

sm

eth

od

foo

dA

uth

or

Art

icle

Ref

eren

ceY

ear

Och

rato

xin

A(O

TA)

Imm

unoa

ffini

tyco

lum

n/H

PLC

proc

edur

eM

odel

420

dual

pist

onpu

mp,

aM

odel

460

auto

sam

pler

,aS

FM

25flu

ores

cenc

ede

tect

or,

Gre

enco

ffee

bean

s,ro

aste

dco

ffee

bean

s,an

dso

lubl

e(in

stan

t)co

ffee

Pitt

etan

dot

hers

Liqu

idch

rom

atog

raph

icde

term

inat

ion

ofoc

hrat

oxin

ain

pure

and

adul

tera

ted

solu

ble

coffe

eus

ing

anim

mun

oaffi

nity

colu

mn

clea

nup

proc

edur

e

JA

gric

Foo

dC

hem

1996

,44:

3564

–69

1996

Fum

onis

ins

and

aflat

oxin

sH

PLC

Cor

nsa

mpl

esYo

shiz

awa

and

othe

rsO

ccur

renc

eof

fum

onis

ins

and

aflat

oxin

sin

corn

from

Tha

iland

.

Foo

dA

ddit

Con

tam

.19

96F

eb–

Mar

;13(

2):1

63–8

1996

Am

aran

thgr

ains

ondi

chlo

ran-

chlo

r-am

phen

icol

-pep

tone

agar

(DC

PA)

and

dich

lora

n-18

%gl

ycer

olag

ar(D

G18

).

Myc

otox

in-p

rodu

cing

pote

ntia

lof

fung

iiso

late

dfr

omam

aran

thse

eds

inA

rgen

tina

IntJ

Foo

dM

icro

biol

Vol

ume

25,I

ssue

1,M

arch

1995

,Pag

es10

1–8

1995

Afla

toxi

nsB

1,B

2,G

1,an

dG

2,oc

hrat

oxin

A,z

eara

leno

nean

dst

erig

mat

ocys

tin

Thi

n-la

yer

chro

mat

ogra

phy

36sa

mpl

eof

stor

edm

aize

Hen

nige

nan

dot

hers

Inci

denc

ean

dab

unda

nce

ofm

ycot

oxin

sin

mai

zein

Rio

Gra

nde

doS

ul,B

razi

l.

Foo

dA

ddit

Con

tam

1995

Sep

–O

ct;1

2(5)

:677

–81

1995

Tric

hoth

ecen

esan

dfu

mon

isin

s)an

dafl

atox

inB

1(A

FB

1)on

eby

one

tric

hoth

ecen

es(N

IV),

(DO

N),

and

T-2

toxi

n(T

-2)

(GC

/MS

);fu

mon

isin

sB

1(F

B1)

,B2

(FB

2),a

ndB

3(F

B3)

by(H

PLC

)w

itha

flour

esce

nce

dete

ctor

;and

AF

B1

byan

dE

LIS

Aki

tbas

edon

am

onoc

lona

lant

ibod

y

Cor

nW

ang

and

othe

rsN

atur

alco

-occ

urre

nce

ofF

usar

ium

toxi

nsan

dafl

atox

inB

1in

corn

for

feed

inno

rth

Vie

tnam

.

Nat

Toxi

ns19

95;3

(6):

445–

919

95

Afla

toxi

nsB

1,B

2,G

1an

dG

2,oc

hrat

oxin

Aan

dze

aral

enon

e

The

liqui

dch

rom

atog

raph

icm

etho

dde

velo

ped

for

the

sepa

ratio

nof

the

six

myc

otox

ins

invo

lves

grad

ient

elut

ion

with

are

vers

ed-p

hase

C18

colu

mn

and

fluor

esce

nce

dete

ctio

n

Ani

mal

feed

ingr

edie

nts

Dun

nean

dot

hers

Mul

ti-m

ycot

oxin

dete

ctio

nan

dcl

eanu

pm

etho

dfo

rafl

atox

ins,

ochr

atox

inan

dze

aral

enon

ein

anim

alfe

edin

gred

ient

sus

ing

high

-per

form

ance

liqui

dch

rom

atog

raph

yan

dge

lpe

rmea

tion

chro

mat

ogra

phy.

JC

hrom

atog

r19

93Ja

n22

;629

(2):

229–

3519

93

AF

DO

NU

sing

biol

ogic

alsp

ecie

sre

view

Ani

mal

feed

sP

anig

rahi

Bio

assa

yof

myc

otox

ins

usin

gte

rres

tria

land

aqua

tic,

anim

alan

dpl

ants

peci

es

Foo

dan

dC

hem

ical

Toxi

colo

gyV

olum

e31

,Iss

ue10

,Pag

es76

7–90

1993

Con

tinue

d



Ta

ble

1---

Co

nti

nu

ed

.

Qu

anti

fica

tio

nT

ype

of

Myc

oto

xin

sm

eth

od

foo

dA

uth

or

Art

icle

Ref

eren

ceY

ear

Afla

toxi

nsB

1,B

2,G

1,G

2no

rst

erig

mat

ocys

tin,

zear

alen

one,

oroc

hrat

oxin

B

Gra

insa

mpl

esof

oats

,w

heat

,rye

,bar

ley,

and

mai

ze

Jusz

kiew

icz

and

Pis

kors

ka-

Plis

zczy

nska

Occ

urre

nce

ofm

ycot

oxin

sin

anim

alfe

eds.

(Pol

and)

JE

nviro

nP

atho

lTox

icol

Onc

ol.1

992

Jul–

Aug

;11(

4):2

11–5

1992

Och

rato

xin

A,a

flato

xin

B1

and

T-2

toxi

nM

onoc

lona

lant

ibod

ies

spec

ific

for

Cer

ealg

rain

Lace

yan

dot

hers

Imm

unoa

ssay

ofoc

hrat

oxin

and

othe

rm

ycot

oxin

sfr

oma

sing

leex

trac

tofc

erea

lgr

ains

utili

zing

mon

oclo

nal

antib

odie

s.

IAR

CS

ciP

ubl1

991;

(115

):97

–103

1991

Afla

toxi

nsB

1,B

2,G

1,an

dG

,och

rato

xin

A,

citr

inin

,zea

rale

none

and

vom

itoxi

non

eby

one

Thi

n-la

yer

chro

mat

ogra

phy

(TLC

)F

eeds

tuffs

,mai

ze,

whe

at,w

heat

bran

,be

ans,

rice

germ

,ric

ege

rmca

ke,

broi

lers

feed

,egg

feed

,milk

feed

;ye

llow

mai

zeso

yabe

ans,

whe

atso

yam

eal,

rice

crac

k,se

edca

ke,fi

shm

eal

Abd

elha

mid

Occ

urre

nce

ofso

me

myc

otox

ins

(afla

toxi

n,oc

hrat

oxin

A,c

itrin

in,

zear

alen

one

and

vom

itoxi

n)in

vario

usE

gypt

ian

feed

s.

Arc

hT

iere

rnah

r.19

90Ju

l;40(

7):6

47–6

419

90

Sim

ulta

neou

sde

term

inat

ion

ofafl

atox

ins,

ochr

atox

inA

,ste

rigm

atoc

ystin

,an

dze

aral

enon

e

TLC

Ric

e,be

ans,

drie

dbe

ans,

corn

prod

ucts

,cas

sava

flour

Soa

res

and

othe

rsS

urve

yof

aflat

oxin

s,oc

hrat

oxin

A,z

eara

leno

ne,

and

ster

igm

atoc

ystin

inso

me

Bra

zilia

nfo

ods

usin

gm

ultit

oxin

thin

-laye

rch

rom

atog

raph

icm

etho

d

JA

ssoc

Off

Ana

lC

hem

.198

9Ja

n-F

eb;7

2(1)

:22–

6

1989

Det

ectio

nof

aw

ide

rang

eof

tric

hoth

ecen

es,

incl

udin

gth

em

ost

pola

ron

esc

irpe

ntrio

l,ni

vale

nol

and

15-

mon

oace

toxy

scir

pend

iolG

asch

rom

atog

raph

y-m

ass

spec

trom

etry

with

sele

cted

ion

mon

itorin

g,or

gas

chro

mat

ogra

phy

with

elec

tron

-cap

ture

dete

ctio

n

Sor

ghum

Bla

ckan

dot

hers

Det

ectio

nof

trac

ele

vels

oftr

icho

thec

ene

myc

otox

ins

inen

viro

nmen

talr

esid

ues

and

food

stuf

fsus

ing

gas

chro

mat

ogra

phy

with

mas

ssp

ectr

omet

ricor

elec

tron

-cap

ture

dete

ctio

n.

JC

hrom

atog

r19

87F

eb13

;388

(2):

365–

7819

87

afB

1,B

2,G

1,G

2,O

TA,

citr

inin

,pen

icill

inac

id,v

iom

elle

in,

peni

trem

A,p

atul

in,

ster

igm

atoc

ystin

,al

tern

ario

l,,

Hig

h-pe

rfor

man

celiq

uid

chro

mat

ogra

phy

(HP

LC)

with

anal

kylp

heno

nere

tent

ion

inde

xan

dph

otod

iode

-arr

ayde

tect

ion

com

bine

dw

ithth

in-la

yer

chro

mat

ogra

phy

(TLC

)in

two

diffe

rent

elue

nts

Fris

vad

and

Thr

ane

Sta

ndar

dize

dhi

gh-p

erfo

rman

celiq

uid

chro

mat

ogra

phy

of18

2m

ycot

oxin

san

dot

her

fung

alm

etab

olite

sba

sed

onal

kylp

heno

nere

tent

ion

indi

ces

and

UV

-VIS

spec

tra

(dio

dear

ray

dete

ctio

n).

JC

hrom

atog

r19

87A

ug28

;404

(1):

195–

214

1987

Pro

duct

sof

Pen

icill

ium

spec

ies

Sta

ndar

dize

dth

in-la

yer

chro

mat

ogra

phic

(TLC

)P

ater

son

Sta

ndar

dize

don

e-an

dtw

o-di

men

sion

alth

in-la

yer

chro

mat

ogra

phic

met

hods

for

the

iden

tifica

tion

ofse

cond

ary

met

abol

ites

inpe

nici

llium

and

othe

rfu

ngi

Jour

nalo

fC

hrom

atog

raph

yA

Vol

ume

368,

1986

,P

ages

249–

64

1986

Con

tinue

d



ab

le1

---C

on

tin

ue

d.

Qu

anti

fica

tio

nT

ype

of

Myc

oto

xin

sm

eth

od

foo

dA

uth

or

Art

icle

Ref

eren

ceY

ear

Sec

onda

rym

etab

olite

sof

Pen

icill

ium

)an

dot

her

fung

iid

entifi

catio

nof

prod

ucts

ofP

enic

illiu

msp

ecie

s

Sta

ndar

dize

dth

in-la

yer

chro

mat

ogra

phic

(TLC

)m

etho

dsfo

rth

eid

entifi

catio

nof

seco

ndar

ym

etab

olite

sin

peni

cilli

uman

dot

her

fung

i

Jour

nalo

fC

hrom

atog

raph

yA

Vol

ume

368,

1986

,P

ages

249–

64

1986

Sim

ulta

neou

sde

tect

ion

ofth

e11

myc

otox

ins

af(B

1,B

2,G

1,G

2),

OTA

,ZE

Ast

erig

mat

ocys

tin,

citr

inin

,pen

icill

icac

id,T

-2to

xin

and

rubr

atox

inB

Cer

eals

peci

es(r

ye,

barle

y,w

heat

,oat

s,an

dco

rn)

Gra

bark

iew

icz-

Szc

zesn

aan

dot

hers

Myc

otox

ins

ince

real

grai

n.P

artX

I.S

impl

em

ultid

etec

tion

proc

edur

efo

rde

term

inat

ion

of11

myc

otox

ins

ince

real

s.

Nah

rung

1985

;29

(3):

229–

4019

85

AF

ls,

ster

igm

atoc

ystin

s,ve

rsic

olor

ins,

OT

s,ru

brat

oxin

s,pa

tulin

,pe

nici

llic

acid

,...

..

Two-

dim

ensi

onal

TLC

,hi

gh-p

erfo

rman

ceT

LC(H

PT

LC),

quan

titat

ion

and

prep

arat

ive

TLC

(PLC

).S

peci

alap

plic

atio

nsof

TLC

deal

with

mul

ti-m

ycot

oxin

anal

yses

Bet

ina

Thi

n-la

yer

chro

mat

ogra

phy

ofm

ycot

oxin

s.J

Chr

omat

ogr

1985

Nov

15;3

34(3

):21

1–76

1985

Afla

toxi

ns,o

chra

toxi

nA

,zea

rale

none

,T-2

toxi

n

Myc

otox

ins

wer

ese

para

ted

bybi

dim

ensi

onal

thin

-laye

rch

rom

atog

raph

y

Foo

dstu

ffsa

mpl

esTa

pia

Aqu

antit

ativ

eth

in-la

yer

chro

mat

ogra

phy

met

hod

for

the

anal

ysis

ofafl

atox

ins,

ochr

atox

inA

,zea

rale

none

,T-

2to

xin

and

ster

igm

atoc

ystin

info

odst

uffs

Rev

Arg

entM

icro

biol

.19

85;1

7(4)

:183

–619

85

Mul

ti-m

ycot

oxin

met

hod

aflat

oxin

s,oc

hrat

oxin

A,z

eara

leno

ne,

seca

loni

cac

idD

,and

vom

itoxi

n

Afla

toxi

nsan

doc

hrat

oxin

wer

equ

antit

ated

byflu

ores

cenc

em

easu

rem

ento

nsi

lica

thin

-laye

rch

rom

atog

raph

icpl

ates

.The

othe

rm

ycot

oxin

sw

ere

quan

titat

edaf

ter

clea

nup

byre

vers

e-ph

ase

liqui

dch

rom

atog

raph

yan

dul

trav

iole

tdet

ectio

n

Gra

indu

st.

Ehr

lich

and

Lee

Myc

otox

ins

ingr

ain

dust

:m

etho

dfo

ran

alys

isof

aflat

oxin

s,oc

hrat

oxin

A,

zear

alen

one,

vom

itoxi

n,an

dse

calo

nic

acid

D.

JA

ssoc

Off

Ana

lChe

m19

84S

ep-O

ct;

67(5

):96

3–7

1984

Sim

ulta

neou

sde

term

inat

ion

ofafl

atox

inB

1an

doc

hrat

oxin

A

Thi

n-la

yer

chro

mat

ogra

phy

Bla

ckol

ives

LeTu

tour

and

othe

rsS

imul

tane

ous

thin

-laye

rch

rom

atog

raph

icde

term

inat

ion

ofafl

atox

inB

1an

doc

hrat

oxin

Ain

blac

kol

ives

JA

ssoc

Off

Ana

lChe

m19

84M

ay-J

un;

67(3

):61

1–2

1984

Con

tinue

d



Ta

ble

1---

Co

nti

nu

ed

.

Qu

anti

fica

tio

nT

ype

of

Myc

oto

xin

sm

eth

od

foo

dA

uth

or

Art

icle

Ref

eren

ceY

ear

Deo

xyni

vale

nol,

T-2

toxi

n,ze

aral

enon

e,an

dafl

atox

in.O

neby

one

Zea

rale

none

-TLC

Deo

xyni

vale

nol-G

C_M

SA

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Chromatographic techniqueChromatography analysis is based on distribution or partition

of a sample solute between 2 phases: stationary phase and mobilephase. Most common chromatography techniques used today inthe field of food analysis are gas chromatography (GC), HPLC,and supercritical fluid chromatography (SFC). These methods,when connected to another instrument such as mass spectrom-eter, work as a separation method. In the 1980s and the earlyof 1990s, various reviews on the chromatography of mycotoxinswere published (Betina 1993).

TLC technique. Thin-layer chromatography (TLC) is a techniquethat can be used for the separation, purity assessment, and iden-tification of organic compounds. First reports of this techniquewere in the 1930s and after that it becomes a very useful andeasy technique for the analysis of a wide range of compounds(Betina 1993). TLC also identified as flat-bed chromatography orplanar chromatography, is one of the most widely used separationtechniques in aflatoxin analysis. Since 1990, it has been consid-ered as an AOAC official method and the method of choice toidentify and quantify aflatoxins at levels as low as 1 ng/g. Accord-ing to reports and articles, mycotoxins were easily separated byTLC using several solvents (Odhav and Naicker 2002), assessedin the multitoxin detection part of this article.

Normal-phase TLC consists of a stationary phase like silica,alumina, and cellulose immobilized on a glass or plastic plateand a solvent as the mobile phase (Betina 1993). The sample,either liquid or dissolved in solvent, is deposited as a spot onthe stationary phase. The constituent of a sample can be iden-tified by simultaneously running standards with the unknownspot. Then one edge of the plate is vertically placed in a sol-vent tank and the solvent moves up the plate by capillary ac-tion. After the solvent reaches other edge, the plate is removedfrom tank and the separated spots (because of different parti-tioning behavior of the components) are visualized by UV, flu-orescence, MS, or other techniques. Pittet and Royer (2002)used this method for the determination of ochratoxin A in greencoffee.

Sometimes the plate is dried after first-development and ro-tated through 90◦ and developed in another solvent. This modelis called 2-dimensional TLC and is used for better resolution orremoval of interfering compounds (Betina 1985). A further devel-opment in TLC is high-performance thin-layer chromatography(HPTLC). Reduction of layer thickness (down to 100 microns)and particle size (2 to 10 microns) of the stationary phase leadsto an improved separation within a shorter time. Modern HP-TLCis a precise and accurate analytical tool with efficiency, which iscomparable to that of HPLC and ELISA methods. Therefore, quan-titative and qualitative analysis of aflatoxins has been developedusing multidimensional–HPTLC–fluorescence excitation, such asapplied in peanut butter samples by Liang and others (1996). Re-cently, Toteja and others (2006) determined aflatoxin B1 of ricesamples, using HPTLC after extraction with water/chloroform andsilica gel column cleanup.

The overpressured-layer chromatography (OPLC) method hasthe advantages of the HPTLC and HPLC methods. The linearOPLC is a forced flow technique, using external pressure on chro-matoplate sealed on the edges and a pump system for the admis-sion of mobile phase into the stationary phase. Comparing withthe HPLC, it requires less mobile phase, using off-line method,and allows faster examination with the possibility of parallel anal-ysis. OPLC is more efficient than TLC, providing better resolutionand more compact spots. OPLC methods were developed for themeasurement of aflatoxin (B1, B2, G1, and G2) contaminationin various foodstuffs (maize, wheat, peanut, fish meat, rice, sun-flower seeds, and red paprica) (Otta and others 2000; Papp andothers 2002; Moricz and others 2007).

For the chemical confirmation of mycotoxins, there are 2 treat-ment methods. First, TLC plates were formerly impregnated withacidic-organic solution; second, the TLC plates, with the de-veloped chromatogram, were exposed to vapors of pyridine oracetic anhydride or dipped into aluminum chloride reagent. Afterthese treatments, mycotoxins were converted into new fluores-cent compounds, and then the TLC plates were observed under365 nm light. The combination of TLC with mass spectrometry(MS) has been carried out without an adsorbent elution step (Scott1993).

TLC was an extremely powerful, rapid, and low-cost separationtechnique in mycotoxicology before HPLC techniques becamepopular. Several TLC methods were developed for mycotoxinquantitation (Le-Tutor and Tantaoui Elaraki 1984; Liang and oth-ers 1996; Aziz and others 1998; Odhav and Naicker 2002; Rizzoand others 2004; Caldas and Silva 2007) and qualitative deter-mination (Grabarkiewicz-Szczesna and others 1985; Liang andothers 1996; Abrunhosa and others 2001; Odhav and Naicker2002). Alhough there are some reports on comparable resultsbetween TLC and HPLC for the dtermination of aflatoxin M1 inraw, pasteurized, and UHT milk (recovery values ranged from85.83% to 73.86% at levels of 0.010 to 0.50 μg/L) (Shundo andSabino 2006) and aflatoxins (B1, B2, G1, and G2) in productswith quantification limit (LOQ) of 2 μg/kg, these TLC methodsare generally suitable for qualitative analysis at best (Caldas andSilva 2007).

Liquid chromatography. Liquid chromatography methods forthe determination of mycotoxins in foods include normal-phaseLC (NPLC), reversed-phase LC (RPLC) with pre- or before-columnderivatization (BCD), RPLC followed by postcolumn derivatiza-tion (PCD), and RPLC with electrochemical detection (Calleriand others 2007). Pre- and postcolumn derivatizations are usedfor improvement of sensitivity (Hu and others 2006). LC canbe classified into 3 parts, column chromatography, mini-columnchromatography, and HPLC. Column chromatography is used forcleanup. Many factors like particle size, particle size distribution,and surface area, packing density, pH, and many other factors af-fect its performance. Therefore, columns have been replaced bycommercial prepacked cartridges. Mini-columns were used forscreening of different mycotoxins (usually aflatoxins, ochratoxinA, and ZEA). After first publishing about the application of HPLC(Betina 1993), the same researcher stated that the usage of HPLChas increased and it has been used for separation, detection, andquantification of mycotoxins.

High-performance liquid chromatography. HPLC is the mostpopular method for the analysis of mycotoxins in foods andfeeds. Actually it is a quantitative technique that is suited foronline cleanup of sample extract and could be combined withdifferent detectors. During the last decades, several reviews havebeen written in this area. There are some reports of successfulapplication of HPLC techniques for the analysis of mycotoxinsin grains (Li and others 2001, 2006; Razzazi-Fazeli and oth-ers 2002, 2003; Eke and others 2004; Gobel and Lusky 2004;Klotzel and others 2005; Visconti and others 2005), fungal cul-tures (Delmulle and others 2006), cheese (Kokkonen and others2005), milk (Sorensen and Elbaek 2005), bee pollen (Garcia-Villanova and others 2004), cereal products (Aresta and others2003; Chan and others 2004; Biselli and Hummert 2005), beerand wine (Soleas and others 2001), and feeds (Vrabcheva and oth-ers 2000; Biselli and Hummert 2005; Martins and others 2007;Krska and others 2007). These HPLC methods differed signifi-cantly in the choice of normal-phase or reversed-phase columnsof different types, elution mixtures and gradients, detection meth-ods, and sample preparation and purification procedures. Amongthose, most chromatography techniques were performed in theform of reversed-phase based on acidic mobile phase with



ortho-phosphoric acid and fluorescence detection (FD) (Odhavand Naicker 2002; Abdulkadar and others 2004; Saez and others2004; Gonzalez and others 2005; Zinedine and others 2006; Cal-leri and others 2007; Sobolev 2007), or UV detection (Hayashiand Yoshizawa 2005); the ion pair techniques with UV detection.HPLC in a normal phase mode on a buffered silica gel columnwas also proposed.

Calleri and others (2007) determined aflatoxin B1 by anti-aflatoxin B1 immunoaffinity monolithic disk. Polyclonal anti-AFB1 was covalently immobilized in batch on an epoxy-activatedmonolithic Convective Interaction Media (CIM) disk by a 1-stepreaction via epoxy groups of the polymer surface. A weight of0.96 mg of antibody was immobilized and the CIM disk wascoupled through a switching valve to a reversed-phase column.The fully automated HPLC method with fluorescence detectionhas a limit of detection of 50 ng/mL (S/N = 3) and a limit ofquantitation of 100 ng/mL (Calleri and others 2007).

HPLC–UV technique. The reversed-phase HPLC–UV tech-nique was an early method used for the determination of my-cotoxins in grains (Cahill and others 1999), which was estab-lished based on an acidic mobile phase with phosphoric acid.However, even using the same type of columns, the retentiontimes were highly variable. In sequence, a general method (Fris-vad and Thrane 1987) for mycotoxin analysis was developed,based on HPLC with an alkyl phenone retention index andphotodiode-array (PDA) detection in 2 different eluents. Appli-cation of the PDA technique allowed the simultaneous qualita-tive detection and identification of multi-mycotoxins. By analyz-ing the organic solvent extracts of fungal cultures, this systemwas found effective for comparison of chemotaxonomic data andfor precise identification of fungi. Based on RP–HPLC–UV–PDAtechniques, multi-mycotoxin estimations were further developedusing linear gradient elution with an acetonitrile/water solventsystem (Kuronen 1989). The toxins were characterized by reten-tion times and online UV spectra produced by a diode arraydetector (DAD). In a simple method, DON in cereal was ex-tracted using methanol, then the solvent was evaporated, andthe residue was re-dissolved with water; the extract was thencleaned up by immunoaffinity column and DON was determinedusing HPLC-UV. The limits of detection (LOD) and quantifica-tion (LOQ) were 10 and 50 ng/g, respectively (Czerwiecki andWilczynska 2003). In another study for the investigation of DONin wheat, HPLC–DAD has been used after sample cleaning withimmunoaffinity column. The detection limit was 0.03 ng/g andrecovery was almost 90% (Danicke and others 2004). Abdulka-dar and others (2004) used HPLC–UV for the determination ofDON in foods after extraction by acetonitrile : water (15:85). Also,Briones-Reyes and others (2007) developed and optimized an RP-HPLC-UV method for determination of zearalenone in corn forhuman consumption. In this method, zearalenon was extractedby methanol : water (85:15) and cleaned up by Florisil column,defatted by n-hexane and re-extracted by chloroform. Recov-ery was 90% and LOD was 0.7 ng/g (Briones-Reyes and others2007).

HPLC-fluorescence technique. HPLC with fluorescence de-tection (FD) becomes the method of choice because of the avail-able short and high-resolution columns and of the sensitivity offluorescence detectors, and its potential for automation (Hol-comb and others 1992; Valenta 1998). Extraction is normallyperformed in acetonitrile-water, methanol-water, or even chlo-roform. An effective cleanup of the raw extract is required forpurification of the analytes.

An early RP–HPLC–FD method coupled with solid phase ex-traction (SPE) cleanup and concentration procedure was devel-oped for the analysis of citrinin from hydrolyzed human urine(Orti and others 1986). By this method, the detection limit for cit-

rinin was achieved to a level of 10 ng/g. Liquid chromatographyusing reversed-phase columns and fluorescence detection waseffectively used to quantify different mycotoxins in grains (Ab-dulkadar and others 2004; Medina and others 2004; Hinojo andothers 2006; Zinedine and others 2006), feeds (Charoenpornsookand Kavisarasai 2006), beverages (Abdulkadar and others 2004;Saez and others 2004; Varelis and others 2006), high-pigment-content samples such as chili powder, green bean, black sesame,and other spices (Fazekas and others 2005; Hu and others 2006),nuts (Abdulkadar and others 2004), coffee (Ventura and others2003), ginseng and ginger (Trucksess and others 2008), and beepollen (Gonzalez and others 2005).

Optimizations for selective separations were generally done us-ing ternary or even quaternary eluent systems. Water, methanol,and acetonitrile were mostly used as a ternary system. The reten-tion of mycotoxins depended on the content of water, whereasthe composition and ratio of methanol and acetonitrile deter-mined the elution order and resolution of mycotoxin with otheranalytes. To obtain fine peak forms and resolution, RP-ion-pairHPLC techniques have also been applied for the determination ofmycotoxins. Later, an improved ion pair RP–HPLC coupled withpostcolumn fluorometric detection technique for mycotoxin de-termination was developed. Spectroscopic studies demonstratedthat the fluorescence of this metabolite was influenced by thepH of the environment. In the meantime, another ion-pair RP–HPLC procedure coupled with a postcolumn technique and time-resolved luminescence (TRL) detection were developed (Vazquezand others 1996).

Some of the mycotoxins such as fumonisins are not fluores-cent, so, prior derivatization of these compounds is needed tomake fluorescent derivatives (Caldas and Silva 2007). To thisaim, different reagents can be used for derivatization, such asfluorescamine, o-phthaldialdehyde (OPA) (Sydenham and oth-ers 1990; Stroka and others 2002; Hinojo and others 2006), 4-fluoro-7-nitrobenzofurazan (NBD-F) (Scott and Lawrence 1994;Jimenez and Mateo 1997), 9-fluorenilmethyl chloroformate (Hol-comb and others 1993), or naphthalene 2,3-dicarboaldehyde(Bennett and Richard 1994). Fumonisins (FB1 and FB2) weredetermined in different corn-based food products using HPLC-fl with quantification limit (LOQ) of 0.020 mg/kg (Caldas andSilva 2007). Trebstein and others (2008) developed an HPLC-flourescence method for the determination of T-2 toxin and HT-2toxin in different cereals and cereal products after derivatizationwith 1-anthroylnitrile.

Liquid chromatography with fluorescence detection (LC–FLD)is one of the most widely used techniques for the analysis ofmycotoxins. LC using other detection methods, such as pho-todiode array (Danicke and others 2004) or mass spectrome-try (LC–MS–MS) (Delmulle and others 2006; Tanaka and others2006; Lattanzio and others 2007; Sulyok and others 2007) hasalso been reported. However, these 2 detection methods are lesssensitive than FLD in some cases but can aid as confirmativetools (Saez and others 2004). On the other hand, in contrast toHPLC-UV methods, GC-ECD enables the determination of sev-eral trichothecenes, even in complex food matrices, in the lowermilligram per kilogram range. However, reversed-phase ion-pairHPLC provides good peaks, whereas those in the native fluores-cence of mycotoxins were somewhat lost. In that way, the sen-sitivity and selectivity of this detection method were decreased.This weakness can be solved by acidifying the eluate from theHPLC column before fluorescence detection. So, RP-HPLC iswidely used because of its advantages instead of conventionalnormal-phase HPLC.

Although these RP–HPLC–fluorescence detection methodshave relatively good sensitivity and recovery, in practice, ap-plication of all these methods to various complex matrices was



considered boring and time-consuming. Extensive cleanup pro-cedures were generally necessary, and sometimes deficient inspecificity. Some problems, such as low reproducible LC reten-tion times still existed when normal-phase columns were used(Dick and others 1988; Zimmerli and others 1989), and decreasedsensitivity and accuracy resulting from stability of citrinin in or-ganic eluents, ion-pair, reagents, and acid environment.

Chromatography and mass spectrometrycombination technique

LC–MS technique. Coupling of LC and MS provides a great op-portunity for the analysis of mycotoxins. HPLC with MS detectioneliminates the need for sample derivatization for fluorescence ac-tivity enhancement. Furthermore, the use of LC and tandem massspectrometry enables a very selective and sensitive detection. Liq-uid chromatography tandem mass spectrometry (LC–MS/MS) is auseful technique for identification and quantification of chemi-cals such as mycotoxins. Before mass spectrometer, HPLC willseparate the sample to chemical compounds. Then mass spec-trometer will ionize molecules and sort, and identify them ac-cording to their mass-to-charge ratio (m/z).

The first LC–MS methods for the determination of tri-chothecenes were based on fast-atom bombardment (FAB), ther-mospray, and plasmaspray ionization (Kostiainen 1991). Later,soft-ionization techniques such as atmospheric pressure chem-ical ionization (APCI), electrospray ionization (ESI), and at-mospheric pressure photo-ionization (APPI) were widely used,which are suitable for different molecular weights and polarity ofcompounds.

APCI is more practical for low to medium molecular massand low to medium polar analytes, but ESI is more helpful formedium to high molecular mass and medium to high polar ana-lytes. However, there are some reports in using both of these ion-izers in mycotoxin detection literatures. For instance, APCI havebeen used in the determination of trichothecenes (Berger andothers 1999; Razzazi-Fazeli and others 2002, 2003; Berthillerand others 2005) and Zollner and Mayer-Helm (2006) reviewedtrace mycotoxin analysis using APCI. Also, ESI have been used byBerthiller and others (2006) for zearalenone and by Delmulle andothers (2006) for simultaneous determination of 16 mycotoxinsin fungal cultures and by Ventura and others (2006) for simultane-ous determination of aflatoxins and OTA in beer. Lau and others(2000) have determined ochratoxin A (OTA) in coffee samplesusing 3 different quantitative approaches (standard method addi-tion, internal standard, and external standard methods) by meansof ESI-MS–MS detection. As well, LC–ESI-MS–MS determinationin combination with C18 SPE has been reported as a valid alter-native to liquid chromatography-fluorescence protocols for thedetection of OTA in wine samples at trace levels (Leitner and oth-ers 2002). Due to its higher sensitivity in comparison with APCI,ESI-MS–MS detection was proposed for quantitative analysis atlow levels (Biselli and others 2004; Klotzel and others 2005).

Only a few LC–MS methods for the simultaneous determinationof both type A and B trichothecenes exist in the literature (Biselliand others 2004; Dall’Asta and others 2004). LC–tandem-MS hasbeen also proposed as a valid technique for the determination ofmycotoxins in contaminated foodstuffs and beverages (Lau andothers 2000; Leitner and others 2002).

In addition, there are many types of mass analyzers such asquadrupole, time-of-flight, ion-trap, and Fourier transform-ioncyclotron resonance (FT-ICR); however, for mycotoxin analysisthe most important mass analyzers are the triple quadrupole andthe ion-trap and time of flight.

Triple quadrupole consists of 3 parts for 3 important func-tions. The first quadrupole acts as an ion filter. Then the massseparated ions pass into the collision cell and change to frag-

ments. Finally, the selected fragment ions pass into the thirdquadrupole that is for detection. Lattanzio and others (2007) ap-plied a double extraction approach, using a phosphate-bufferedsolution followed by methanol, for the simultaneous detectionof 11 mycotoxins (aflatoxins (B1, B2, G1, G2), ochratoxin A,and fumonisins (B1, B2), DON, zearalenone, and T-2 and HT-2toxins) having quite different polarities and chemical structures.A new multitoxin immunoaffinity column containing antibod-ies for all these mycotoxins was used to clean up the extract,and a liquid chromatography/tandem mass spectrometry methodwas developed. Reversed-phase liquid chromatography coupledwith electrospray ionization triple quadrupole mass spectrom-etry (LC/ESI–MS/MS) using a linear gradient of methanol/watercontaining 0.5% acetic acid and 1 mM ammonium acetate, aschromatographic mobile phase, achieved recoveries higher than79% in maize. Limits of detection in maize ranged from 0.3 to4.2 μg/kg (Lattanzio and others 2007).

An extended multi-mycotoxin method for 25 contaminants ina variety of sample types has been carried out by separation anddetection using tandem quadrupole mass spectrometry (Kok andothers 2007). Furthermore, fully automated tandem MS, with in-jection at atmospheric pressure, has been applied to examineaflatoxins in peanuts (Schatzki and Haddon 2002). In addition,mycotoxins [NIV, DON, AFG1, AFG2, AFB1, AFB2, FB1, FB2, di-acetoxyscripenol (DAS), T2-toxine, ochratoxin A, and ZEN] weresimultaneously measured in cattle forages and food matrices bythe LC–MS/MS method. The MS analysis was carried out on aTSQ Quantum Discovery MAXTM triple-stage quadrupole massspectrometer with a heated electrospray ionization (H-ESI) probein the positive ionization mode. TSQ Quantum Discovery MAXoffers the unique capability of highly selective reaction mon-itoring (H-SRM) (Huls and others 2007). Monbaliu and others(2009) have developed a multi-mycotoxin method using a liquidchromatography/tandem mass spectrometry method for the si-multaneous determination of trichothecenes (nivalenol, DON,3-acetyldeoxynivalenol, 15-acetyldeoxynivalenol, neosolaniol,fusarenon-X, diacetoxyscirpenol, HT-2 toxin, T-2 toxin), afla-toxins (aflatoxin-B1, aflatoxin-B2, aflatoxin-G1, and aflatoxin-G2), alternaria toxins (alternariol, alternariol methyl ether,and altenuene), fumonisins (fumonisin-B1, fumonisin-B2, andfumonisin-B3), ochratoxin A, zearalenone, beauvericin, andsterigmatocystin in sweet pepper.

In addition, simultaneous determination of aflatoxins, type Atrichothecenes, type B trichothecenes, OTA, zearalenone, fumon-isins, and patulin have been done on corn flake extracts with nosample cleanup in a single run by comprehensive LC/MS/MS(Rudrabhatla and others 2007). In another study, Niderkorn andothers (2007) used an HPLC–MS/MS system for the determina-tion of DON, ZEN, and fumonisins B1 and B2 (FB1, FB2) in cornsilage after separation by C18 reversed-phase columns. On theother hand, HPLC–MS analysis was performed using a C18 col-umn with a C18 precolumn for the detection of aflatoxin B1,citrinin, DON, fumonisin B1, gliotoxin, ochratoxin A, and zear-alenone in corn silage. Mass spectrometry was performed on aquadrupole analyzer equipped with an electron-spray ionization(ESI) source and operating in positive and negative modes. Thedetection and quantification limits for aflatoxin B1, citrinin, fu-monisin B1, and ochratoxin A were 1.5 and 5 ppb, and 6.5 and20 ppb for DON, gliotoxin and zearalenone, respectively(Richard and others 2007).

Sulyok and others (2006) improved the LC–MS/MS method forthe determination of 39 mycotoxins to allow the unambiguousdetection and quantification of about 90 mycotoxins and someof their naturally occurring metabolites. MS conditions for allanalyzed substances were optimized to gain multiple reactionmonitoring (MRM) transitions. One MRM transition per analyte



was used for quantification, while another one was used as aqualifier (Sulyok and others 2006). Berthiller and others (2007)mentioned several of the published LC–MS/MS multi-mycotoxinmethods and also introduced a new method, which allowed theconcurrent detection and quantification of major mycotoxins andother secondary fungal metabolites in cereals.

The liquid chromatography/tandem mass spectrometry (LC–MS/MS) method includes relatively few and nonlaborious sampletreatment steps, and it allows for a high throughput of samples(Delmulle and others 2006). Furthermore, according to Silva andothers (2009), LC–MS/MS is the most precise, accurate, and sen-sitive method in comparison with LC-FL and LC–MS, at least forfumonisin determination. They reported that liquid chromatogra-phy coupled to tandem mass spectrometry provides higher sen-sitivity (12 μg/kg for fumonisins B1 and B2) when compared tomass spectrometry (40 μg/kg for both fumonisins) and fluores-cence detection (20 μg/kg for fumonisin B1 and 15 μg/kg for B2)(Silva and others 2009).

Recently, an HPLC-ESI-MS/MS method was developed for si-multaneous determination of 33 mycotoxins in various productssuch as peanuts, pistachios, wheat, maize, cornflakes, raisins,and figs. The mycotoxins were extracted with acetonitrile/waterand then directly injected into a LC–MS/MS system without anycleanup. The limit of quantification for the aflatoxins and ochra-toxin A was 1 mg/kg and for the other mycotoxins were in therange of 10 to 200 mg/ kg (Spanjer and others 2008).

An ion trap can be considered as a “3-dimensionalquadrupole” in which the ions of all masses are trapped in achamber. At first, targeted ions are selected (mass-to-charge ra-tio) by expelling all the others from the ion trap. Then, fragmenta-tion of the selected ions will be done. At the end, the fragmentedions are analyzed by expelling those of a selected mass-to-chargeratio.

An HPLC–MS analysis method for determining mycotoxinswas established, which included extraction, sample pretreatment,and reversed-phase HPLC separation with MS identification andquantification using electrospray ionization on a quadrupole iontrap mass analyzer (ESI–MS–MS) (Razzazi-Fazeli and others 2002;Klotzel and others 2005; Kokkonen and others 2005). Mass spec-tral analysis was performed on a Finnigan LCQ fitted with an elec-trospray ionization (ESI) probe in the positive ion mode. Aqueousmethanol was used in the initial extraction, solvent partition, andsolid phase extraction in the purification of samples. The HPLCseparation was run online with the ESI-MS-MS detection. Recov-eries of the sample pretreatment varied from 28% to 99%. Theaverage accuracy and precision (RSD) were 21% and 113%, re-spectively. In addition, a standardized LC–UV–MS micro-scalemethod for the screening of fungal metabolites and mycotoxinsin culture extracts was presented; the database of 474 mycotox-ins including citrinin was established (Nielsen and Smedsgaard2003).

In time-of-flight mass analyzer, the same electromagnetic forcewill be applied to push the ions accelerate down a flight tube.Lighter ions will flight faster and will be received faster by thedetector. Their mass-to-charge ratio will be determined accord-ing to their receiving time. Tanaka and others (2006) developeda LC-TOF-MS method for the simultaneous determination oftrichothecenes, zearalenone, and aflatoxins in foodstuffs. Also,Elosta and others (2007) reported the same method for the si-multaneous determination of trichothecene mycotoxins in barleyand malt extracts.

Although analytical methods might consist of different extrac-tion, cleanup, and quantification steps, the results of the analysesby such methods should be similar. The confirmation techniquesused can be either chemical derivatization or mass spectrometry(MS).

GC–MS technique. In history, gas chromatography (GC) wasintroduced in the field of mycotoxins in the early 1970s. Ifmycotoxins are sufficiently volatile at the column temperature,or can be converted into volatile derivatives, GC can be ap-plied for their determination. Trichothecenes were extracted di-rectly from sorghum by Clin Elut columns, and cleaned up onFlorisil Sep-Pak cartridges. Simultaneous determination of tri-chothecenes and macrocyclics and neosolaniol were done afterhydrolysis to verrucarol and T-2 tetraol, respectively, and determi-nation by gas chromatography-mass spectrometry with selectedion monitoring, or gas chromatography with electron-capture de-tection. In one study, use of a magnetic sector instrument withelectron-impact ionization gave comparable sensitivity for mosttrichothecenes, but was less useful for the simultaneous detectionof verrucarol in the presence of other trichothecenes (Black andothers 1987).

Aflatoxin B could be detected by fused silica capillary GC–MSwith on-column injection. Aflatoxins B1, B2, G1, and G2 couldbe separated, and the limit of quantification was 1 ng for B1and B2 and 2 ng for G1 and G2, when a flame ionization de-tector was used; however, the limit of detection by GC–MS wassomewhat lower (Scott 1993). Ochratoxin A was converted to itsO-methyl ochratoxin A, a methyl ester derivative that was iden-tified by capillary GC–MS (Scott 1993). Also, Soleas and others(2001) utilized gas chromatography with mass-selective detec-tion, monitoring 8 specific ions for ochratoxin A in wines andbeers. Limits of detection (LOD) and quantification (LOQ) were0.1 and 2 μg/L, respectively, whereas the recovery and impre-cision were 69 to 75 and 9% to 11.1%, respectively. The GCmethod is not suitable for routine quantification but is potentiallyuseful as a confirmatory tool for samples with OTA up to 0.1 μg/L(Soleas and others 2001). In another study, SPE cleanup withFlorisil cartridge columns was used followed by a derivatizingprocedure to prepare trimethylsilyl derivatives of 7 trichothecenemycotoxins (DON, 3-acetyldeoxynivalenol, diacetoxyscirpenol,fusarenon-X, nivalenol, neosolaniol, T-2 toxin) and zearalenonein cereals (Tanaka and others 2000). The possibility of using fun-gal volatile metabolites as indicators of ochratoxin A (OTA) andDON mycotoxins to determine grain quality has been investi-gated by Olsson and others (2002) using both electronic noseand gas chromatographic–mass spectrometric detection.

For a study on Fusarium, extracts were micro-scale ex-tracted from crude Fusarium culture extracts and deriva-tized: acetyl T-2 toxin, T-2 toxin, HT-2 toxin, T-2 triol,T-2 tetraol, neosolaniol, iso-neosolaniol, scirpentriol, 4,15-diacetoxyscirpenol, 15-acetoxyscirpenol, 4-acetoxyscirpentriol,NIV, fusarenon-X, DON, 15-acetyl-DON and 3-acetyl-DON. Forderivatization, pentafluoropropionic anhydride was used beforedetermination by GC-tandem mass spectrometric detection. Neg-ative ion chemical ionization (NICI) GC–MS was used for molec-ular mass determination verification (Nielsen and Thrane 2001).In the development of a multi-mycotoxin detection method byGC–MS, A and B type trichothecenes, namely 4,15-diacetoxy-scirpenol, T2-toxin, DON, and nivalenol (NIV) of semolina andcorn grits were derivatized by cleanup cartridge consisting ofammonium sulfate, celite, alumina, charcoal, and C18 with N,N-dimethyl-trimethylsilyl-carbamate, then they were determined bygas chromatography with flame ionization detector (GC-FID) ormass selective detector (GC–MSD). Limit of detection of themethod was from 0.30 to 0.47 mg/kg for GC-FID and from0.05 to 0.35 mg/kg for GC–MSD. Using this cartridge, no fur-ther sample cleanup steps are required thus making the devel-oped method time- and cost-effective (Eke and others 2004).Recently, 13 trichothecenes were determined in whole beans,roasted soy, nuts, flour and flakes, textured soy protein, tofu,infant formulas, and fermented products (soy sauce) by gas



chromatography/mass spectrometry, and HPLC with fluorescenceand UV-detection (Schollenberger and others 2007). Careri andothers (2002) presented the applications of mass spectrometry(MS)-based techniques for the analysis of compounds in foodsand discussed differences between LC–MS and GC–MS tech-niques.

Bioassay techniqueIn general, the previously mentioned physicochemical de-

tection methods required tedious sample extract and cleanup.Besides, there is loss of mycotoxins during sample treatment, un-stable chromatographic behavior of mycotoxins, or relative lowsensitivity and recovery. Therefore, bioassays have become in-creasingly useful for mycotoxin detection as a precursor of chem-ical analysis (Yates 1986).

Bioassay by biosensor is designed as an inhibition assay. Inthese methods a fixed concentration of mycotoxin-specific anti-body is mixed with a sample containing an unknown amount ofmycotoxin. The antibody and mycotoxin form a complex. Thenthe sample is passed over a sensor surface to which mycotoxin hasbeen immobilized. Noncomplexed antibodies are measured asthey bind to the mycotoxin on the sensor surface. The responsesgenerated over a range of standard mycotoxin concentrations areused to create a calibration curve and table. Finally, unknownsamples are determined by referring to the calibration curve.

Advances in biotechnology have made it possible to develophighly specific antibody-based tests. Commercially available testkits can identify and measure aflatoxins in food in less than10 minutes. For illustration, ochratoxin A, aflatoxin B1, and T-2toxin in cereal grains can be determined by monoclonal anti-bodies specific for detection limits of 1 ng/mL ochratoxin A, 0.1ng/mL aflatoxin B1, and 10 ng/mL T-2 toxin after simple liquid–liquid cleanup procedure. These tests are based on the affinitiesof the monoclonal or polyclonal antibodies for aflatoxins. The 3types of immunochemical methods are radioimmunoassay (RIA),ELISA, and immuno-affinity column assay (ICA).

T-2 toxin determination in cereals has been done bymembrane-based flow-through enzyme immunoassay. Immun-odyne ABC and membrane was coated with 2 microliter of goatanti-horseradish peroxidase (HRP) and rabbit anti-mouse (testspot) (undiluted) immunoglobulins, and the free binding siteswere blocked. In one study recovery was between 16% and 82%(Sibanda and others 2000). After that, Charoenpornsook and Kav-isarasai (2006) developed another method for T-2 toxin and DONdetermination, using ELISA on animal feeds.

Although enzyme immunoassay (EIA) methods for major my-cotoxins have been known for many years, only recently, EIAsfor mycotoxin determination have been developed (Vrabchevaand others 2000). The antibodies developed for EIA were alsoused for immunoaffinity columns for HPLC extract cleanup. Fordetection of ochratoxin A and citrinin, cereal samples includ-ing foods (wheat, corn) and feeds (barley, oats, and wheat bran)were mixed with HCl and dichloromethane. After centrifuging,the lower organic layer was extracted by magnetic stirring withaqueous NaHCO3 solution, centrifuged again, and the upperlayer was used for EIA analysis. Detection limits were 0.5 and5 ng/g, for ochratoxin A and citrinin, respectively (Vrabchevaand others 2000).

A radio immunochemical method was used for aflatoxin B1and ochratoxin in wheat and barely. Detection limit of the RIAmethod was 0.3 μg/kg (Sedmikova and others 2001). Further,Korde and others (2003) determined aflatoxin B1 in agriculturalcommodities rice, wheat, and soy beans by radio-immunoassay(RIA) using AfB1-bovine serum albumin conjugate as immuno-gen. The recovery values obtained ranged between 92% and107%. The assay system was optimized in the range of 0.2 to

5 ng/mL. On the other hand, using the electrochemical immuno-sensor ELISA, a calibration plot for AFB1of grains was obtainedover the concentration range 0.15 to 2.5 ng/mL, which gave adetection limit of around 0.15 ng/mL in buffer solution (Pem-berton and others 2006). ELISA, flow-through membrane-basedimmunoasays, chromatographic techniques, nucleic acid ampli-fication on assays, biosensors, and microarrays were studied forthe detection of mold and mycotoxins by Foong-Cunninghamand others (2006) and Gutleb and others (2002) have written areview on bioassay methods for fumonisins in fungal cultures andcereals.

Many experiments have been conducted on immunoassaymethods for mycotoxins; for example a study on fumonisin B1and B2 in maize (Paepens and others 2004) and aflatoxin M1 inmilk and aflatoxin B1 in feed (Decastelli and others 2007) andalso for multi-mycotoxin detection. Among different mycotoxinsCurtui and others 1998 selected deoxynivalenon, 3-acetylDON,15- acetyl DON, fusarenone X (FX), T-2 toxin (T-2), diacetoxyscir-penol (DAS), ZEA, FB1, AFB1, OTA, and citrinin (CIT) in wheat,maize as feed for their study.

Developing rapid and innovative methods offer the microtiter-plate immunoassay (ELISA format) has made them the most fre-quently used rapid tests for mycotoxins. ELISAs are commerciallyavailable for important mycotoxins like aflatoxins, fumonisins,trichothecenes, ZEA, OTA, citrinin (Sangare-Tigori and others2006). They are useful tools for screening and quantification andoffer benefits with respect to speed and sensitivity.

These days ELISA is well known as a useful semiquantita-tive method for mycotoxins and commercial enzyme-linked im-munosorbent assays (ELISAs) are widely used (Ruprich and Ostry1995; Papadopoulou-Bouraoui and others 2004). For example,aflatoxins like aflatoxin B1 in groundnut, corn, wheat, cheese,and chili have been determined after dilution of the aqueousmethanol extracts without sample cleanup. In this study, recov-eries from different food samples were between 91% and 104%and detection limit were 0.25 pg/spot, 0.01 ng/mL (Pal and oth-ers 2004). In addition, the results of aflatoxin determination inred-scaled, red and black pepper determined by ELISA showed agood correlation with HPLC, since ELISA (in terms of simplicity,rapidity, reliability, cost-effectiveness) can be used in the routinescreening of aflatoxin contamination in spices (Colak and oth-ers 2006). Aflatoxin M1 in milk has been determined by ELISAby some researchers (Thirumala-Devi and others 2002; Magliuloand others 2005; Decastelli and others 2007).

In a competitive ELISA with monoclonal antibody,dichloromethane/citric acid mixture was used for extraction ofcereal ochratoxin A. This cleanup procedure proved to be as ef-fective for OTA extraction as protocols using strong acids. Recov-ery from cereals infected with 5 to 100 ng/mL ochratoxin A variedbetween 90% and 130% in different cereals, and the results wereconfimed by HPLC fluorescence detector (Barna-Vetro and others1996). Later, Thirumala and others (2002) extracted ochratoxinA (OTA) from chilies with methanol-water and KCl. This step isfollowed by dilution to 1:4 with PBS-T-BSA for processing byELISA. The mean recoveries from OA-free chilies spiked with 1 to100 μg of OA per kilogram of chili sample were 90% and 110%(Thirumala-Devi and others 2002).

In another experiment, chratoxin A (OTA) in soybean sampleswas extracted using extract solvent and loaded onto a C18 Sep-Pak cartridge, then determined by competitive direct enzyme-linked immuno-sorbent assay (cdELISA), and a competitiveindirect ELISA (ciELISA) was used. Efficacy of cdELISA was con-firmed by the HPLC method. Recovery rate of OTA was found tobe 85.9% in the cdELISA (Yu and others 2005).

Simultaneous estimation of aflatoxin B1 and ochratoxin A havebeen done using membrane-based immunoassay consisting of a



membrane with immobilized anti-AFB1 and anti-OA antibodiesand a filter paper attached to a polyethylene card below the mem-brane. In an experiment on chili samples the limit of quantifica-tion obtained was 2 and 10 μg/kg for AFB1 and OA, respectively(Saha and others 2007). At the same time, aflatoxin and ochra-toxin were determined in barley and wheat flour by Adanyi andothers (2007). After immobilizing the antibody or antigen con-jugate for the direct and indirect measurement, respectively, asensor chip was used in the flow-injection analyzer (FIA) system.The regression coefficient between the 2 methods for ochratoxinand aflatoxin was determined to be 0.96 and 0.89, respectively.Sensitivity detection range of the competitive detection methodwas between 0.5 and 10 ng/mL in both cases (Adanyi and others2007). In the case of spices, ginger, pepper, and chili, simulta-neous detection of aflatoxin B1 and ochratoxin has been doneby tandem immunoassay after one cleanup. Cutoff levels were5 and 10 μg/kg. Results were confirmed by LC–MS/MS with im-munoaffinity column cleanup (Goryacheva and others 2007a).

Recently, Iacumin and others (2009) used an ELISA kit for OTAdetermination in Italian sausages after digesting with hydrochlo-ric acid and extracting with dichloroethane; the method was thesame as reported by Matrella and others (2006). Also, Wang andGan (2009) developed a flow-through quartz crystal microbal-ance (QCM) immunoassay method based on aflatoxin B1 anti-body. The proposed immunoassay system was simple and rapidwithout multiple labeling and separation steps.

Bioassay methods provided a rapid means for screening sam-ples and allowed the analyst to make an informed decision.Immunochemical methods provided a convenient and sensitivealternative for detecting many mycotoxins (Chu 1991). Ease ofoperation and high throughput, associated with their use, arethe best advantages of ELISA method. Like other methods, thesemethods have some weakness, which includes cross-reactivityand matrix dependence, often resulting in overestimation (Schuh-macher and Magnuson 1997; Josephs and others 2001; Krska andMolinelli 2007). Besides the common ELISA procedures, thereis an increasing demand for immunoassay techniques for fielduse, offering protocols for quick and reliable results. Multiana-lyte dipstick immunoassays for various mycotoxins have been de-veloped, however, with limited sensitivity (Schneider and others1995).

One of the recently developed methods for mycotoxin de-tection is polymerase chain reaction (PCR) method. The mainprinciples of PCR are as follows: first, denaturing (separating theindividual strands) DNA by heat. Second, a small segment ofDNA will be taken as a probe that will target to anneal withthe piece of DNA of interest (the target). Then, it will be ampli-fied and yield doubled DNA. After that, the process will cycledaround 40 times to give the desired quantity of DNA product. Fi-nally, the negatively charged DNA will be separated through thegel based on size (Jurado and others 2006). Small pieces of DNAcan be amplified and detected routinely. It is rapid, and does notneed to culture organisms prior to their identification. They arespecific, since identification of species is made on the basis ofgenotypic differences, and are highly sensitive, detecting targetDNA molecules in complex mixtures even when the mycelia areno longer viable (Russell and Paterson 2006).

ConclusionsThe aim of this review was to discuss the various ana-

lytical techniques involved in mycotoxin detection and esti-mation. Mycotoxins to be analyzed are originally present incontaminated samples. Hence, mycotoxins must be extractedwith different extraction methods and cleaned-up prior to de-tection techniques, if reliable results are to be obtained. Ex-

traction procedures include extraction of mycotoxins from feedsand foodstuffs. SPE and IAC-cleanup will become of increas-ing importance as sample preparation techniques prior to in-strumental analysis. Immunoaffinity cleanup techniques withhigh-resolution chromatography showed the most selectivity formycotoxin analysis. Recently, advances using tandem or mixedselectivity immunoaffinity cartridges have demonstrated the fea-sibility of multitarget mycotoxin assays. In the early 1980s, TLCwas the most widely used chromatographic technique appliedto mycotoxins because of its relatively simple, fast, and inex-pensive properties; however, it has some disadvantages, such aslow sensitivity, high detection limit, and lack of potential for au-tomation. Consequently, it is now almost replaced by the HPLCtechniques. Among the available detectors, the most frequentlyused are PDA, UV, and Fl, which have a particular applicationin the field of mycotoxins. HPLC–MS has all the HPLC advan-tages for trace level detection and confirmation, especially forcomplex matrices and it can obtain qualitative data concerningthe identity of mycotoxins. The great potential of LC–MS/MS forscreening large amounts of samples for the presence of a numberof mycotoxins has recently been demonstrated. Immunoassaysthat deliver quantitative or semiquantitative results, still representthe most frequently used rapid methods. There is an ongoing de-velopment toward quick and reliable methods providing rapidyes/no decisions or semiquantitative results. Also, many projectsare in progress aiming to avoid purification step, for example, tomeasure the analytes directly after extraction. Easy-to-use meth-ods are often either too expensive or show a lack of sensitivity. Ina nutshell, the previously mentioned methods have their advan-tages and disadvantages, and the desired method selection shouldbe done according to the analytical objective, sample properties,and environmental conditions. Although there are some reportsfor qualitative and quantitative analysis of mycotoxins, rapid andsensitive quantitative methods are still high on the wish list.

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Qualitative and Quantitative Analysis of Mycotoxins

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