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The Effect of Ascorbic Acid, Citric Acid and Salt on theQuality of Spiny Dogfish (Squalus acanthias) FilletGülgün F. Şengör a , Sühendan Mol a & Didem Üçok a

a Istanbul University, Faculty of Fisheries, Department of Seafood Science and Technology ,Laleli, Istanbul, TurkeyPublished online: 22 Sep 2008.

To cite this article: Gülgün F. Şengör , Sühendan Mol & Didem Üçok (2007) The Effect of Ascorbic Acid, Citric Acid and Salton the Quality of Spiny Dogfish (Squalus acanthias) Fillet, Journal of Aquatic Food Product Technology, 16:1, 103-113, DOI:10.1300/J030v16n01_08

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The Effect of Ascorbic Acid, Citric Acidand Salt on the Quality of Spiny Dogfish

(Squalus acanthias) Fillet

Gülgün F. �engörSühendan MolDidem Üçok

ABSTRACT. In this study, spiny dogfish fillets were soaked in 10%brine (1:2 w fillet/v solution) for 30 min. Then they were dipped in a so-lution containing 0.1% ascorbic acid and 1.0% citric acid (1:2 w/v) for5 min. All samples were covered with ice and stored at 3 ± 1�C for 12 days.Sensory, chemical, and bacteriological analyses were done in every 3 days.Sensory values were 3 and 5; pH values were 7.03 and 6.87; mesophilicaerobic bacteria counts were 5.77 and 5.56 for the control and treated sam-ples, respectively, at the 12th day and these values were significantly (p <0.05) different. Control samples were marketable on the 9th day and spoiledon the 12th day of storage while the treated samples were still marketable.It was seen that treatment of the spiny dogfish fillet with salt, ascorbicacid, citric acid increased the shelf life. doi:10.1300/J030v16n01_08 [Arti-cle copies available for a fee from The Haworth Document Delivery Service:1-800-HAWORTH. E-mail address: <docdelivery@haworthpress.com> Website:<http://www.HaworthPress. com> © 2007 by The Haworth Press, Inc. All rightsreserved.]

Gülgün F. �engör, Sühendan Mol, and Didem Üçok are affiliated with Istanbul Uni-versity, Faculty of Fisheries, Department of Seafood Science and Technology, Laleli,Istanbul, Turkey.

Address correspondence to: Gülgün F. �engör at the above address (E-mail: sengor@istanbul.edu.tr).

The authors thank Mr. Haluk �engor, MBA, BSc EE, for his invaluable assistancein the manuscript preparation.

This work was supported by the Research Foundation of Istanbul University. Pro-ject Number: BYP-561/21122004.

Journal of Aquatic Food Product Technology, Vol. 16(1) 2007Available online at http://jafpt.haworthpress.com

© 2007 by The Haworth Press, Inc. All rights reserved.doi:10.1300/J030v16n01_08 103

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KEYWORDS. Shark, spiny dogfish, total volatile base, trimethylaminenitrogen, shelf-life, chemical treatment, bacteriological analyses

INTRODUCTION

Shark meat is consumed in many countries, although its quality variesfrom species to species. The most valuable product is shark fin, which isone of the most expensive fish products in the world. Asia (such asHong Kong, Singapore, Macao, Taiwan, and China) holds the mainmarket for shark fins. Shark fins are traditionally consumed in thesecountries (Fong and Anderson, 2000). The spiny dogfish is a commonshark species in Turkish waters. It is also prevalent in the Atlantic andPacific coasts of the United States (Yang et al., 1981). But its consump-tion is not popular in Turkey and the majority of the catch is exported toEC countries (Kutaygil and Bilecik, 1998).

Sharks differ from bony fish since they maintain a high concentrationof urea, a metabolic waste product, in their bodies. After the shark dies,urea can quickly degrade to ammonia, causing shark meat to developoff-odors and flavors (Anonymous, 2004). There are many factors(handling, storage and processing operations) that can influence the fi-nal quality. In studies conducted on the storage of spiny dogfish, it wasfound that formation of ammonia is strongly inhibited by icing (Stansbyet al., 1968; Bilinski et al., 1983; Kutaygil and Bilecik, 1998; Selviet al., 1999). Preservatives like ascorbic acid and citric acid are also be-ing used to extend its shelf life (Yang et al., 1981). Preservatives keepproduct on the shelf longer, minimize economic losses, decrease wast-ing of foods, and minimize health hazards. Therefore preservatives of-fer benefits to the producer, consumer and society (Robach, 1980).Chub mackerels were treated with lactic acid by Metin et al. (2001).Lactic acid extended the shelf life of chub mackerels by 3 days. Thecontrol samples spoiled on the 9th day while treated ones spoiled on the12th day of storage.

High level of ammonia is a problem since it is the reason for the hightrimethylamine nitrogen (TMA-N) and total volatile bases nitrogen(TVB-N) values of fish flesh. Therefore, decreasing their levels is im-portant to extend shelf life. The estimation of volatile nitrogen has beenwidely used as an index of the freshness of fish (Schormüller, 1968).The European Commission (Council Regulation no. 95/149/EEC ofMarch 1995) specified TVB-N to be used if sensory evaluation indi-cates doubt about freshness of different fish species (Dalgaard, 2000).

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Most often a TVB-N content of 30-35 mg TVB-N/100 g is regarded asthe acceptability limit for different groups of fish species. However, thislimit is 50 mg/100 g for sharks and rays, which are heavily laden withurea (Dalgaard, 2000; Sikorski et al., 1990; Schormuller, 1968; Ludorffand Meyer, 1973; Varl�k et al., 1993).

The aim of this study was to extend shelf life of spiny dogfish bytreating its flesh with ascorbic acid, citric acid and salt. Similar to ourstudy, Yang et al. (1981) used this treatment to extend shelf life of spinydogfish at 20�C; Jhaveri and Constantinides (1981) treated Squalusacanthias with ascorbate solution and sodium tripolyphosphate. Theyreported that treatment increased shelf life of the samples.

Changes in seafood during storage due to microbial activity, auto-lytic enzymes or chemical reactions can be useful indices of quality orspoilage. The implementation of seafood quality control and assuranceshould consider not only their microbial, chemical compositions, toxi-cological safety and nutritional characteristic but also their sensoryquality. In this study, spiny dogfish fillets were treated with ascorbicacid, citric acid and salt; and their shelf life was studied using sensory,chemical and microbiological analyses in order to extend the shelf life.

MATERIALS AND METHODS

Eight fresh spiny dogfish (Squalus acanthias) were purchased fromthe seafood wholesale market in Kumkap�, Istanbul. The fish werecaught from Black Sea in April 2005. Within 6-8 hr of the catch, the fishwere transported on ice to the laboratory where they were headed, gut-ted, bled, washed in cold water and iced (ice was made from potable wa-ter). The fish had an average live weight of 7.52 � 1.47 kg and 130.2 �7.25 cm length. The fish were skinned and filleted. Fillets were sepa-rated in two groups. One group was control and the other was soaked in10% brine (refined table salt) for 30 min (1:2 w fillet/v solution). Thisstep was essential in removing traces of blood and nonprotein nitroge-nous substances. After, excess water was drained off and the fillets weredipped in a solution containing 0.1% ascorbic acid (Merck 501461)and 1.0% citric acid (Merck 100241) for 5 min (1:2 w/v), in order to ex-tending shelf-life and reduce pH. Control and treated samples were wellcovered with crushed ice. Samples were placed in straphore boxes, andkept in cold storage (3 ± 1�C) with controlled temperature (Ebsero ther-mometer, Hanna Instruments, Padova, Italy �40/�120�C ± 0.2�C).

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The liquid from melting ice was drained from a hole at the bottom of thestorage boxes. The ice was replenished when necessary maintaining theratio ice:fish (2:1) used. The fish remained iced for 12 d, and 2 sampleswere taken on days 1, 3, 6, 9, 12 for sensory, chemical, and bacteriologi-cal analyses. This experiment was repeated triplicate.

Sensory Evaluation

At each sampling time observations on the quality of the raw filletswere recorded by four experienced judges. Judges were trained by sem-inars on sensory analyses, had contributed the sensory tests of seafoodsfor many other studies, and improved their experience. Their ages werebetween 25 and 40; two of them were male. Sensory analyses were car-ried out under daylight in a well-ventilated laboratory. Samples werepresented to the judges on white plates, and judges evaluated the sam-ples in separated places. Appearance, color, texture, and smell of thefillets were evaluated by the judges using a ballot: ten was the highestpoint and four was the limit of acceptability (Amerina et al., 1965).

Chemical Analysis

Samples were diluted with distilled water (1:1) and pH measure-ments were made with a WTW InoLab-pH meter. For TVB-N measure-ment, vapor distillation method was used. The sample (10 g) was mixedwith catalyst (1 g MgO) and 200 ml distilled water, and boiled for 20min. The vapor components captured with 0.1 N HCl. Hydrochloricacid was titrated with 0.1 N NaOH and the TVB-N was expressed asmg/100 g fish (Schormüller, 1968). Trimethylamine nitrogen (TMA-N)content was measured according to the method of Schormüller (1968).

Bacteriological Analyses

Three fillets of each group were analyzed to estimate aerobic platecounts and psychrotrophic flora. Samples were diluted (101-106) inpeptone water and mixed (fish:buffer = 25:225) in a stomacher for90 seconds (IUL Instruments Barcelona, Spain). Mesophilic aerobicbacteria were determined by plating on plate count agar (PCA) and in-cubated for 24 h at 37�C. Following the incubation, colonies werecounted and data reported as log colony forming units (log CFU/g).

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Plates were incubated for 7 h at 10�C for the estimation of psychrophilicaerobic bacteria (Baumgard, 1986).

Statistical Analysis

The comparison of the data means obtained during shark storage un-der the different treatment was conducted by analysis of variance andthe Student’s t-test procedure of Microsoft Excel 2000 (Redmond,WA). Differences were studied at p < 0.05 level (Renner, 1970).

RESULTS AND DISCUSSION

At the beginning of storage all the samples were in good quality. Sen-sory score of the control samples were lower than the treated ones dur-ing the storage period. Control samples were marketable since thesensory score was between 4 and 5 on the 9th day; and spoiled on the12th day of storage while the treated samples were still marketable.Sensory score of treated samples were significantly higher (p < 0.05)than control group at the 12th day of storage (Figure 1).

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FIGURE 1. Sensory value of the fillets from dogfish stored in crushed ice at3 ± 1�C.

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pH value should be between 6.00-6.50 for fresh fish and the limit ofacceptability is 6.80-7.00 (Ludorff and Meyer, 1973). However, sharksand rays contain high urea in their body and pH could be higher than 7for them (Schormuller, 1968). In this study pH value increased due tothe decomposition of nitrogenous compounds, and control samples hada higher value than treated ones on the 9th day of storage (p < 0.05) ac-cording to t test (Renner, 1970). pH value was reduced through ascorbicacid and citric acid since they are acidity regulators (Anonymous,1988). pH value exceeded 7 in control samples on the 12th day of stor-age. In a similar study chub mackerels were dipped in 0%, 2% and 4%potassium sorbate and pH values reached to 6.88, 6.30 and 6.68, respec-tively, on the 12th day of cold storage (Erkan et al., 2001). pH value ofspiny dogfish was higher than chub mackerels since it contains ammo-nia in its flesh. pH was 7.03 for control group and 6.87 for treated sam-ples on the 12th day in present study. pH value of the control sampleswas significantly higher (p < 0.05) than the others according to t-test(Figure 2) (Renner, 1970).

The initial TVB-N for control group was 39.28 mg/100 g and for thetreatment group it was 37.18 mg/100 g. After 6 days TVB-N contentwas over 50 mg/100 g which is the limit for sharks (Dalgaard, 2000;Sikorski et al., 1990; Schormüller, 1968; Ludorff and Meyer, 1973;Varl�k et al., 1993). This value increased to 76.59 mg/100 g and it was

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FIGURE 2. pH value of the fillets from dogfish stored in crushed ice at 3 ± 1�C.

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significantly higher (p < 0.05) than treated samples on the 9th day ofstorage (Figure 3).

Metin et al. (2002) treated chub mackerels with potassium lactate andcompared their quality with the control group which was not treatedwith potassium lactate. The TVB-N values of chub mackerel werelower than the TVB-N results of our study since sharks contain highamounts of ammonia in their flesh. However TVB-N value of controlsamples was significantly higher than the treated chub mackerels on the9th day of storage, similar to the present study. Chub mackerels weredipped in 2% and 4% lactic acid solutions and stored at �4 � 1�C (Metinet al., 2001). Both of these groups had significantly lower TVB-N valuethan control samples on the last day of storage.

Trimethylamine content of fish increased during the storage periodand it was correlated with the bacterial counts and the sensory scores. Itis a useful method to determine quality level of various marine species(Botta, 1994). Trimethylamine values between 5 to 10 mg/100 g wereproposed as a rejection limit by Sikorski et al. (1990). However, thislimit is between 10-15 mg/100 g in Connel (1980) and 8 mg/100 gin Varl�k et al. (1993). In this study, TMA-N content of the fresh sam-ples was over 5 mg/100 g at the beginning of storage since dogfish con-tain high amounts of ammonia in their flesh. Therefore, regardless the

�engör, Mol, and Üçok 109

FIGURE 3. TVB-N value of the fillets from dogfish stored in crushed ice at3 ± 1�C.

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treatment TMA-N content of the samples increased significanlty (p <0.05) according to t-test (Renner, 1970) and it was over 10 mg/100 g af-ter 9 days (Figure 4).

Total mesophilic aerobic bacteria count is an important quality indi-cator of foods (Do�gan and Tükel, 2000). It must be lower than 5 � 105

cfu/g in fish (ICMSF, 1986). Total mesophilic aerobic bacteria countsover 6-7 log cfu/g are regarded as the acceptability limit for seafoods(Anonymous, 1991). The bacterial load of the treated samples did notexceed these limits during the cold storage. However, total mesophilicaerobic bacteria counts of control samples were significantly higher(p < 0.05) than the treated ones on the 9th and 12th days of storage ac-cording to Renner (1970) (Figure 5). Similarly, microbial load of chubmackerel was studied and control samples had significantly higher val-ues than the samples dipped in potassium lactate (Metin et al., 2002).

There is not a clear limit of acceptance for psychrohilic aerobic bac-teria. However, estimation of the psychrophilic microorganisms is im-portant in cold stored seafoods since these microorganisms grow inchilled temperatures (Do�gan and Tükel, 2000). On the 6th day of stor-age psychrophilic aerobic bacteria counts of the control samples wassignificantly higher (p < 0.05) than treated samples according to Renner(1970) (Figure 5). Yang et al. (1981) treated Squalus acanthias filletswith salt, ascorbic acid and citrate. They reported that ascorbic acid hadan antioxidative effect for 2 weeks of storage at 20�C. They mentioned

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FIGURE 4. TMA-N value of the fillets from dogfish stored in crushed ice at3 � 1�C

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that this technique would be of great use especially in developing coun-tries. Jhaveri and Constantinides (1981) treated Squalus acanthias withascorbate solution and sodium tripolyphosphate; and reported the shelflife on ice as 6-8 days.

In this study, mesophilic bacteria counts of control samples were sig-nificantly higher (p < 0.05) than the others during the storage period,and pH of the control group was over the limits on the 12th day whiletreated ones still acceptable. Control samples were marketable on the9th day and spoiled on the 12th day of storage while the treated sampleswere still marketable according to the results of pH, sensory, mesophilicbacteria analyses. At the end of this study it was found that, treatment ofthe spiny dogfish with salt, ascorbic acid, citric acid increased the shelflife. However, it is advantageous to consume treated spiny dogfish before12 days of storage.

CONCLUSION

Landed shark must be handled carefully and quickly in order to pre-serve product quality. Immediately after capture, the shark must be bledby cutting off the head and tail portion, then must be gutted, washed and

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FIGURE 5. Total mesophilic bacteria and psychrophilic bacteria of the filletsfrom dogfish stored in crushed ice at 3 ± 1�C.

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soaked with preserving chemicals such as citric acid, ascorbic acidbefore packing in ice. When properly handled and iced, shark will re-main fresh for 12 days.

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