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FAPAS® Report 20115

Illegal Dyes in Hot Pepper Sauce

March-April 2015

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FAPAS Report 20115

PARTICIPANT LABORATORY NUMBER

Participants can log in to FAPAS SecureWeb at any time to obtain their laboratory number for this proficiency test.

Laboratory numbers are displayed in SecureWeb next to the download link for this report.

REPORT INTEGRITY

FAPAS reports are distributed as Adobe® Certified Document Services (CDS) Adobe® PDF documents [1]. The use of Adobe® CDS allows the PDF files to certify that the author of the report is FAPAS and that the document has not been altered in anyway. A blue ribbon and information bar indicates this validation when the document is opened using Adobe® Reader v7 or later.

Hard copies of FAPAS reports can never incorporate this level of integrity and consequently when a FAPAS report is printed a watermark, stating that printed copies are not controlled, appears on every page.

End users of FAPAS reports should ensure that either the opened PDF file displays a valid FAPAS digital signature or that the content of any hard copy exactly matches the content of a PDF file that displays a valid FAPAS digital signature.

QUALITY SYSTEMS

FAPAS® is accredited by UKAS as complying with the requirements of ISO/IEC 17043:2010 [2].

Fera is an ISO 9001 certified organisation.

0009

Fera hereby excludes all liability for any claim, loss, demands or damages of any kind whatsoever (whether such claims, loss, demands or damages were foreseeable, known or otherwise) arising out of or in connection with the preparation of any technical or scientific report, including without limitation, indirect or consequential loss or damage; loss of actual or anticipated profits (including loss of profits on contracts); loss of revenue; loss of business; loss of opportunity; loss of anticipated savings; loss of goodwill; loss of reputation; loss or damage to or corruption of data; loss of use of money or otherwise, and whether or not advised of the possibility of such claim, loss demand or damages and whether arising in tort (including negligence), contract or otherwise. This statement does not affect your statutory rights.

Nothing in this disclaimer excludes or limits Fera liability for: (a) death or personal injury caused by Fera negligence (or that of its employees, agents or directors); or (b) the tort of deceit; [or (c) any breach of the obligations implied by Sale of Goods Act 1979 or Supply of Goods and Services Act 1982 (including those relating to the title, fitness for purpose and satisfactory quality of goods);] or (d) any liability which may not be limited or excluded by law (e) fraud or fraudulent misrepresentation.

The parties agree that any matters are governed by English law and irrevocably submit to the non-exclusive jurisdiction of the English courts.

© Copyright Fera Science Ltd (Fera) 2015

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SUMMARY

1. The test material for FAPAS® proficiency test 20115 was dispatched in March 2015.

Each participant received a hot pepper sauce test material. From a list of fourteen illegal

dyes participants had to identify and, optionally, quantify those present.

2. The test material contained sudan l, sudan lll, sudan red B, and sudan red G. An

assigned value (xa) was determined for each analyte and in conjunction with the

standard deviation for proficiency (σp) was used to calculate a z-score for each result.

However, those for sudan red B, an assigned value and z-scores have not being set due

to several participants reporting co-elution between sudan red B and sudan lV. See

section 4.1 for additional information.

3. Quantitative results for this proficiency test are summarised as follows:

analyte assigned value, xa µg/kg

number of scores, |z| ≤2

total number of scores

% |z| ≤2

sudan l 449 50 58 86

sudan lll 691 40 54 74

sudan red G 224 24 27 89

4. Qualitative results for this proficiency test are summarised as follows:

analyte number of satisfactory qualitative assessments

total number of qualitative assessments (including <LOD and NS)

satisfactory %

sudan l 14 17 82

sudan lll 16 19 84

sudan red G 9 11 82

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CONTENTS

1. INTRODUCTION 5

1.1. Proficiency Testing 5

2. TEST MATERIAL 5

2.1. Preparation 5 2.2. Homogeneity 5 2.3. Dispatch 5

3. RESULTS 5

4. STATISTICAL EVALUATION OF RESULTS 6

4.1. Calculation of the Assigned Value, xa 6 4.2. Standard Deviation for Proficiency, σp 6 4.3. Individual z-Scores 7 4.4. Assessment of Qualitative Results 7 4.5. Additional Dyes Identified 7

5. INTERPRETATION OF SCORES 7

6. REFERENCES 8

TABLES

Table 1: Quantitative Results and z-Scores for Sudan l, Sudan lll and Sudan Red G 9

Table 2: Quantitative Results for Sudan Red B and Sudan lV 12

Table 3: Qualitative Results and Assessments for Sudan l, Sudan lll and Sudan Red G 15

Table 4: Qualitative Results for Sudan Red B and Sudan lV 17

Table 5: Participants’ Comments 19

Table 6: Assigned Values and Standard Deviations for Proficiency 20

Table 7: Number and Percentage of z-Scores where |z| ≤2 20

Table 8: Summary of Qualitative Assessments 20

Table 9: Additional Dyes Identified 21

FIGURES

Figure 1: z-Scores for Sudan l 22

Figure 2: z-Scores for Sudan lll 23

Figure 3: z-Scores for Sudan Red G 24

APPENDICES

APPENDIX I: Analytical Methods Used by Participants 25

APPENDIX II: FAPAS SecureWeb, Protocol and Contact Details 35

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1. INTRODUCTION

1.1. Proficiency Testing

Proficiency testing aims to provide an independent assessment of the competence of participating laboratories. Together with the use of validated methods, proficiency testing is an essential element of laboratory quality assurance.

Further details of the FAPAS® proficiency testing scheme are available in our protocols [3, 4].

2. TEST MATERIAL

2.1. Preparation

Preparation of the samples for this proficiency test was sub-contracted to a laboratory meeting the quality requirements of the scheme’s accreditation [2].

The hot pepper sauce was purchased from a retail source.

Four illegal dyes were spiked into the test material; sudan l, sudan lll, sudan red B and sudan red G.

Samples were stored at ambient temperature until dispatch.

2.2. Homogeneity

To test for homogeneity, randomly selected test materials were analysed in duplicate. Testing was sub-contracted to a laboratory meeting the quality requirements of the scheme’s accreditation [2].

These data showed sufficient homogeneity and were not included in the subsequent calculation of the assigned values.

2.3. Dispatch

The start date was 5 March 2015. Test materials were sent to 88 participants.

3. RESULTS

The instructions for reporting results were as follows:

• This sample may contain any of the illegal dyes listed.

• You may carry out your analysis as quantitative and/or qualitative for each dye. In the report, laboratories that have not identified or misidentified dyes will be noted and the assessment will take into account the dyes looked for and the limit of detection (LOD).

• If you fail to report your LOD, your result will be assessed as if your LOD were zero.

• Your attention is drawn to Statutory Analysis Government Chemist Programme Ad Hoc Project 1, October 2006, Analysis of Illegal Dyes in Paprika Powder by LC-MS/MS which concerns illegal dye determination and can be obtained in pdf format by using the following web address, www.governmentchemist.org.uk/docGallery/53.PDF.

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Results were submitted by 76 participants (86%) before the closing date for this test, 16 April 2015.

Each participant was given a laboratory number, assigned in order of receipt of results. The reported results for quantitative data for sudan l, sudan lll and sudan red G are given in Table 1. The reported results for quantitative data for sudan red B and sudan lV are given in Table 2. The reported results for qualitative data for sudan l, sudan lll and sudan red G are reported in Table 3. The reported results for qualitative data for sudan red B and sudan lV are reported in Table 4.

Participants’ comments are given in Table 5.

The analytical methods used by each participant are summarised in APPENDIX I.

4. STATISTICAL EVALUATION OF RESULTS

The results submitted by participants were statistically analysed in order to provide an assigned value for each analyte. The assigned values were then used in combination with the standard deviation for proficiency, σp, to calculate a z-score for each result. The procedure follows that recommended in the IUPAC International Harmonised Protocol for the Proficiency Testing of Analytical Chemistry Laboratories [5].

Further details on the procedure followed can be found in the relevant protocols [3, 4].

4.1. Calculation of the Assigned Value, xa

The assigned value, xa, for each analyte was derived from the consensus of the results submitted by participants.

The following results were excluded from the calculation of the assigned value:

i) non numerical results i.e. qualitative or semi-quantitative results,

ii) results reported as approximately 10, 100 or 1000 × greater or smaller than the majority of submitted results (as these were considered to be reporting errors).

For sudan l, sudan lll and sudan red G, this procedure was straightforward and the robust mean was chosen as the assigned value.

For sudan red B, several participants reported an issue of co-elution between sudan red B and sudan lV. For this reason z-scores and qualitative assessments could not be calculated and could not be assessed but the reported data is given for information in Table 2 and Table 4.

The assigned values for sudan l, sudan lll and sudan red G are shown in Table 6.

4.2. Standard Deviation for Proficiency, σp

The standard deviation for proficiency, σp, was set at a value that reflects best practice for the analyses in question.

For all analytes, σp was derived from the appropriate form of the Horwitz equation [6].

The values for σp used to calculate z-scores from the reported results of this test are given in Table 6.

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4.3. Individual z-Scores

Participants’ z-scores were calculated as:

p

axxzσ

)( −=

where x = the participant’s reported result,

xa = the assigned value and σp = the standard deviation for proficiency.

Participants’ z-scores for sudan l, sudan lll and sudan red G are given in Table 1 and shown as histograms in Figures 1–3. It is possible for the z-scores published in this report to differ slightly from the z-score that can be calculated using the formula given above. These differences arise from the necessary rounding of the actual assigned values and standard deviations for proficiency prior to their publication in Table 6.

The number and percentage of z-scores in the range -2 ≤ z ≤ 2 for sudan l, sudan lll and sudan red G are given in Table 7.

4.4. Assessment of Qualitative Results

For sudan l, sudan lll and sudan red G participants who had reported their results qualitatively were assessed as follows:

• For each of the four dyes reported as ‘detected’, participants were assessed as satisfactory.

• Where participants had reported one of these four dyes as ‘not detected’ they were assessed against their limit of detection (LOD). If their LOD was lower than the value required to receive a z-score of -3 they were assessed as ‘NS’ (not satisfactory). If their LOD was equal to or greater than the value required to receive a z-score of -3 then they are marked in Table 3 as ‘<LOD’. If no LOD was given, the participant’s result was assessed as if their LOD was zero.

Qualitative assessment of participants’ results is given in Table 3 and a summary of qualitative assessments is given in Table 8.

4.5. Additional Dyes Identified

Any participants identifying dyes other than sudan l, sudan lll, sudan red B, sudan red G and sudan lV are listed in Table 9 together with the dyes reported, the level determined if applicable, and the LOD.

5. INTERPRETATION OF SCORES

In normal circumstances, over time, about 95% of z-scores will lie in the range -2 ≤ z ≤ 2. Occasional scores in the range 2 <|z| <3 are to be expected, at a rate of 1 in 20. Whether or not such scores are of importance can only be decided by considering them in the context of the other scores obtained by that laboratory.

Scores where |z| >3 are to be expected at a rate of about 1 in 300. Given this rarity, such z-scores very strongly indicate that the result is not fit-for-purpose and almost certainly requires investigation.

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The consideration of a set or sequence of z-scores over time provides more useful information than a single z-score. Examples of suitable methods of comparison are provided in the IUPAC International Harmonised Protocol for the Proficiency Testing of Analytical Chemistry Laboratories [5].

6. REFERENCES

1 Adobe Certified Document Services, http://www.adobe.com/misc/pki/cds_cp.html, accessed 14/05/2014.

2 ISO/IEC 17043:2010, Conformity assessment – General requirements for proficiency testing.

3 FAPAS, 2014, Protocol for Proficiency Testing Schemes, Part 1 – Common Principles, Version 4, Issued May 2014.

4 FAPAS, 2014, Protocol for Proficiency Testing Schemes, Part 2 – FAPAS®, Version 3, Issued May 2014.

5 Thompson, M., Ellison, S.L.R. and Wood, R., 2006, The International Harmonised Protocol for the Proficiency Testing of Analytical Chemistry Laboratories, Pure Appl. Chem., 78, No. 1, 145–196.

6 Thompson, M., 2000, Recent trends in inter-laboratory precision at ppb and sub-ppb concentrations in relation to fitness for purpose criteria in proficiency testing, Analyst, 125, 385-386.

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Table 1: Quantitative Results and z-Scores for Sudan l, Sudan lll and Sudan Red G

laboratory number

analyte

sudan l sudan lll sudan red G

assigned value

449 µg/kg assigned value


224 µg/kg

result LOD result LOD result LOD µg/kg µg/kg z-score µg/kg µg/kg z-score µg/kg µg/kg z-score

001 482 5 0.4 735 5 0.4

002 467 <50 0.2 703 <50 0.1 256 <65 0.7

003

004 434.0 10 -0.2 578.0 20 -1.0 229.9 10 0.1

005 401 20 -0.6 2532 20 15.8 232 20 0.2

006

007

008

009 493 10 0.5 819 100 1.1 302 10 1.8

010 392 50 -0.7 681 50 -0.1

011 435 200 -0.2 2135 200 12.4

012 470.00 250.00 0.3 630.00 250.00 -0.5 240.00 250.00 0.4

013 510 10 0.8 260 10 0.8

014 493 250 0.5 863 250 1.5

015

016 468 7 0.2 853 5 1.4 235 44 0.3

017 500 200 0.6 709 200 0.2

018 <600 150 <600 150

019 417 10 -0.4 616 10 -0.6

020 600 20 1.9 700 20 0.1

021 490 0.5 736 0.4 242 0.4

022 1080 1000 3.3

023 686 30 2.9 734 30 0.4

024 468.54 2.00 0.2

025 447 10 0.0 475 10 -1.8 210 10 -0.3

z-scores outside |z| >2 are shown in bold, see Section 5

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Table 1 (continued): Quantitative Results and z-Scores for Sudan l, Sudan lll and Sudan Red G

laboratory number

analyte


assigned value



224 µg/kg


026 454 0.1 727 0.3

027

028

029 346.8 10 -1.3 208.6 10 -4.1 134.7 10 -2.0

030 370.4 90 -1.0 612 90 -0.7

031

032 473.2 100 0.3 616.5 100 -0.6

033 362 20 -1.1 440 200 -2.1

034 557 4 1.3 697 4 0.1

035

036 3249 500 34.6 17544 500 144.2 1684 500 32.6

037 389 100 -0.7

038

039

040 517 500 0.8 766 500 0.6 294 100 1.6

041 580 25 1.6

042 471 10 0.3 841 10 1.3 223 10 0.0

043 374 100 -0.9 647 100 -0.4

044 446 3 0.0 539 3 -1.3 283 3 1.3

045 380 5 -0.9 632 10 -0.5

046 293.00 500 -1.9 598.90 500 -0.8 166.26 500 -1.3

047 148 5 -3.7 196.7 5 -4.2 104 0.5 -2.7

048 165 10 -3.5 52 10 -5.5 82 10 -3.2

049 617.6 500 -0.6

050 465 10 0.2 801 10 0.9


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Table 1 (continued): Quantitative Results and z-Scores for Sudan l, Sudan lll and Sudan Red G

laboratory number

analyte


assigned value



224 µg/kg


051 450 65 0.0 860 135 1.4

052 359.7 4 -1.1 1317.9 4 5.4

053 449 20 0.0 705 20 0.1

054 503 10 0.7 654 10 -0.3 278 10 1.2

055

056 276.9 10 -2.1 454.1 10 -2.0 139.5 10 -1.9

057 383 10 -0.8 420 10 -2.3 173 10 -1.1

058

059 468 10 0.2 1862 10 10.0

060 583.33 7.6 1.7 1116.66 1.4 3.6 287.67 5.4 1.4

061

062 429 5 -0.2 241 5 0.4

063 400 10 -0.6 479 20 -1.8 305 10 1.8

064 391.5 20 -0.7 857.5 20 1.4

065 439 1 -0.1 797 1 0.9

066 427 40 -0.3 647 80 -0.4

067 470 10 0.3 730 10 0.3 250 10 0.6

068 447 420 0.0 696 230 0.0

069 2242 2480 22.1 17463 1800 143.5

070 463.61 100 0.2 768.67 100 0.7

071

072 505 50 0.7 190 50 -0.7

073 700 500 3.1 670 500 -0.2

074 0.35 -5.5 2.40 -5.9

075 402 10 -0.6 698 10 0.1 221 10 -0.1

076 477 25 0.3 689 25 0.0 160 25 -1.4


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Table 2: Quantitative Results for Sudan Red B and Sudan lV

laboratory number

analyte

sudan red B sudan lV

assigned value not set assigned value not set

result LOD result LOD µg/kg µg/kg µg/kg µg/kg

001

002

003

004 641.9 20

005 2179 20

006

007

008

009 1120 25 151 10

010 847 50

011 1000 200

012

013 480 10

014 2669 250

015

016 1037

017 268 200

018 <600 150

019 825 10

020

021 605 590

022 1300 1000

023 902 30

024

025 999 10

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Table 2 (continued): Quantitative Results for Sudan Red B and Sudan lV

laboratory number

analyte




026 913

027

028

029 702.7 10 1027.4 10

030 587.7 90

031

032

033

034

035

036 7090 500

037

038

039

040

041

042

043 1028 100

044 2125 15

045 3600 25

046 381.7 500

047 408 0.5

048 138 10

049 835.5 500

050 1452 10

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Table 2 (continued): Quantitative Results for Sudan Red B and Sudan lV

laboratory number

analyte




051

052

053

054 820 10

055

056 793.9 10

057

058

059 1968 10

060 1543.33 10.4 75.33 0.2

061

062

063 2007 20

064

065

066

067 880 10

068

069 996 1500

070 757.35 100

071

072 612 50 550 50

073

074 0.5

075 399 10 399 10

076 821 25 821 25

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Table 3: Qualitative Results and Assessments for Sudan l, Sudan lll and Sudan Red G

laboratory number

analyte


result LOD assessment result LOD assessment result LOD assessment µg/kg µg/kg µg/kg µg/kg µg/kg µg/kg

001 Detected 2 S

003 detected 10 S detected 10 S detected 10 S

006 Detected S Detected S Detected S

007 not detected

NS detected S Detected S

008 Detected 250 S Detected 250 S

013 detected 10 S

015 detected S detected S

017 not detected

NS

022 not detected

1000 <LoD

024 not detected

2.00 NS


028 Detected S not detected

NS

S = satisfactory NS = not satisfactory

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Table 3 (continued): Qualitative Results and Assessments for Sudan l, Sudan lll and Sudan Red G

laboratory number

analyte


result LOD assessment result LOD assessment result LOD assessment µg/kg µg/kg µg/kg µg/kg µg/kg µg/kg

031 detected 800 S detected 800 S

033 detected 100 S

034 detected 4 S


038 Detected 1000 S Detected 1000 S


049 not detected

500 <LoD



061 Detected S Detected S not detected

NS

062 Detected 5 S

071 detected 8.9 S detected 7.6 S

072 not detected

NS

S = satisfactory NS = not satisfactory

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Table 4: Qualitative Results for Sudan Red B and Sudan lV

laboratory number

analyte



001 Detected 10 (as SIV) not detected

002 not detected

003 not detected detected 10

004 not detected

006 not detected not detected

007 Detected qualitative positive

008 not detected

012 not detected 250.00

013 not detected 10

015 detected

016 not detected

017 not detected

018 <600 150

019 not detected

020 not detected

024 not detected 2.00

025 not detected

027 detected 30

028 not detected

031 detected 800

032 not detected

033 detected 60 not detected 60

034 not detected 4

036 not detected

038 Detected 1000 ug/kg

039 detected 400

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Table 4 (continued): Qualitative Results for Sudan Red B and Sudan lV

laboratory number

analyte




041 not detected 25

042 not detected 10

044 not detected

047 not detected

048 not detected

051 not detected 135

052 not detected

053 not detected

054 not detected

055 not detected detected 40

056 not detected

057 not detected

058 not detected 20


062 Detected 5 not detected 5

063 not detected 10

064 not detected

065 not detected


067 not detected 10

068 not detected 340

071 detected 8.9 not detected

073 not detected

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Table 5: Participants’ Comments

participant number comments

001 1.Orange II and Rhodamine B are not listed in our method. But they were scanned using their appropriate ions, and they were not detected. 2.Sudan Red B is an isomer of Sudan IV, and we have the ability to distinguish them. 3. STD purity of SRG is unknown.

006 tests done as qualitative basis

007 Not quantitativ, only qualitativ detected

009 Cannot enter reporting limits for non-detected dyes. Why? This was possible in earlier tests.

010 Result corrected % Recovery (Sudan I = 84%,Sudan II = 90%, Sudan III = 83%, Sudan VI = 80%)

027 Sudan I (501 µg/kg); Sudan III (898 µg/kg), Sudan IV (214 µg/kg) Sudanred G (254 µg/kg)

028 Qualitative analysis

033 Sudan IV and Sudan Red B cannot be separated by HPLC, identification by HPTLC

041 HPLC-Ref total solution for food safety (sudan red p 14,2005)

044 The result of Sudan IV is the sum of Sudan IV and Sudan Rot B!

053 There is a strong interference around the peak of Sudan IV, exhibiting similar MRM pair ratio but different RT. It is outside our scope so we dont ID it.

057 Results entered are based on the average of the two bottles supplied. Disparity of result (224-617ug/kg) observed in Sudan III between the two bottles.

062 LOD means LOQ

063 Sudan IV is the sum of Sudan IV and Sudan Red B (the isomers cannot separated chromatographically)

067 Results corrected by % purity dyes on COA. For Sudan Red G, we estimated this purity % by LC-PDA injection.

075 Sudan IV and Sudan Red B are reported as the sum, due to co-elution cannot separate

076 Sudan IV and Sudan Red B co-elute with our method of analysis. We cannot discriminate one from they other. Therefore, the same result was reported for both dyes.

comments are as submitted by participants

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Table 6: Assigned Values and Standard Deviations for Proficiency

analyte data points, n

assigned value, xa, µg/kg

uncertainty, u

standard deviation for proficiency, σp, µg/kg

sudan l 56 449 9.68 Horwitz [6] 81.0

sudan lll 48 691 21.7 Horwitz [6] 117

sudan red G 26 224 12.3 Horwitz [6] 44.8

Table 7: Number and Percentage of z-Scores where |z| ≤2

analyte number of scores where |z| ≤2

total number of scores

% |z| ≤2

sudan l 50 58 86

sudan lll 40 54 74

sudan red G 24 27 89

Table 8: Summary of Qualitative Assessments

analyte number of satisfactory qualitative

assessments

number of <LOD

total number of qualitative results (including

<LOD and no LOD results)

satisfactory %

sudan l 14 2 17 82

sudan lll 16 0 19 84

sudan red G 9 0 11 82

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Table 9: Additional Dyes Identified

laboratory number dye identified result, detected/not detected

result, μg/kg

LOD, μg/kg

% rec

024 Sudan II 612.7 2.00 N

029 Orange II 24.9 10 100 & Y

059 Sudan Red 7B 388 10 100%&Y

060 Sudan Red 7B 46.06 0.8 N

061 Sudan Red 7B Detected

061 Toluidine Red Detected

069 Sudan II 1297 2200 77

074 Sudan II 0.013

074 Sudan Black B 0.06

074 Sudan Red 7B 0.42

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Figure 1: z-Scores for Sudan l

74 47 48 56 46 29 52 33 30 43 45 57 37 64 10 63 5 75 19 66 62 4 11 65 44 25 68 53 51 26 70 50 2 16 59 24 12 67 42 32 76 1 21 9 14 17 54 72 13 40 34 41 60 20 23 73 69 36

611 µg/kg

449 µg/kg

287 µg/kg

-6.0

-5.0

-4.0

-3.0

-2.0

-1.0

0.0

1.0

2.0

3.0

4.0

5.0

6.0

7.0

8.0

z-score

Laboratory Number

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Figure 2: z-Scores for Sudan lll

74 48 47 29 57 33 56 25 63 44 4 46 30 19 32 49 12 45 43 66 54 73 10 76 68 34 75 20 2 53 17 26 67 23 1 21 40 70 65 50 9 42 16 64 51 14 22 60 52 59 11 5 69 36

925 µg/kg

691 µg/kg

457 µg/kg

-6.0

-5.0

-4.0

-3.0

-2.0

-1.0

0.0

1.0

2.0

3.0

4.0

5.0

6.0

7.0

8.0

z-score

Laboratory Number

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Figure 3: z-Scores for Sudan Red G

48 47 29 56 76 46 57 72 25 75 42 4 5 16 12 62 21 67 2 13 54 44 60 40 9 63 36

313 µg/kg

224 µg/kg

134 µg/kg

-4.0

-3.0

-2.0

-1.0

0.0

1.0

2.0

3.0

4.0

5.0

6.0

7.0

8.0

z-score

Laboratory Number

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APPENDIX I: Analytical Methods Used by Participants

Methods are tabulated according to the information supplied by participants, but some responses may have been combined or edited for clarity.

Sudan I

Recovery calculated laboratory number

70 041

78 019

82.4 033

84 010 034

84.7 072

85.28 070

90 012 016

92 011

92.3 018

93 051 063

95 001

95.5 057

97 037

98,8 068

99.4 026

100 059

101 066

102 040 045

103 044

112 076

By ISTD 014

No 038

standard addition 042

Result corrected for recovery laboratory number

yes 001 004 009 010 012 014 016 026 034 040 041 044 051 057 059 063 068 070 072 076

no 003 006 008 011 013 017 018 019 024 032 033 035 036 037 038 039 042 045 047 048 050 054 055 056 060 064 065 066 067 071

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Source of Standards laboratory number

Accu Standard 051

Acros 026 033 040 048

Dr Ehrenstorfer 008 009 010 014 018 019 031 034 037 047 050 054 063 066

Fluka 002 033 059 070

Merck 033 056

Sigma/Aldrich 001 003 004 006 011 012 013 016 017 024 033 036 038 039 041 044 055 057 060 067 068 071 072 073 076

Institut of Dyes and Organic Products 035

Institute Of Leather Industry 015

LGC Standards 045

QMX 042

Purity of the dye standard determined

laboratory number

>90 013

1 045

85 016

95 018 050

96 002 060

96.9 057

97 001 006 012 015 036 040 048 059 068

97.8 072

99 010 019 031 034 042 047 063 066

99.5 076

99.7 051

99.9 011

100 067

no 038

Correct for the purity of the dye standard

laboratory number

yes 001 004 006 010 011 013 015 016 018 019 024 032 034 038 039 040 042 045 047 048 051 054 059 060 063 066 067 068 072 076

no 002 003 008 009 012 014 017 026 031 033 035 036 050 055 056 057 065 070 071

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Wavelength (nm) for DAD/UV detectors laboratory number

377 nm, 410 nm, 500 nm 070

400;473;525;625 076

401, 503 and 550 040

476 039

478 010 015 051 057 068

480 031 038

484 012

488 033

500 026

505 018

510 011 065

520 017 035

Ions monitored (MS/MS confirmation) laboratory number

149>93,156 024

156-232 071

249,1-93,0 / 156,1 / 128,1 063

249.0>93.0 : 249.0>156.0 060

249.1/93.0 055

249.1/93.1, 249.1/156.1 036

249.1>156 042

249.1>93 (quantification trace) 249.1>156.2 045

249.1025 047

249.12>153.11 048

249.16 - 77 - 91.9 - 156.1 006

249.2/156.1, 249.2/232.2, 249.2/127.8 034

249.2>156.1 014

249.2>93.0, 249.2>156.0 004

249/ 232, 156 001

249/156 019

249/156 249/128 044

249/93;249/232 003

249->128, 156 009

249>156 057

249>232, 249>156 008 072

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Ions monitored (MS/MS confirmation) (continued)

laboratory number

249-->92,9;155,9 037

249-156 067

92.732,127.813 059

N 051

UPLC/MS/MS 050

yes 016

Sudan III


1.008 049

100 063

101 066

101,9 068

104.8 026

111 044

71 019

74 001

76.9 033

80 012

83 010

88 034

90 016

90 045

90.56 070

91,1 022

92 011

94 051

98 076

no 050


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yes 001 004 009 010 012 016 022 026 034 044 049 051 063 068 070

no 003 006 007 008 011 013 014 017 018 019 032 033 035 036 038 039 042 045 047 048 050 054 055 056 057 060 064 065 066 067 071 076


Acros 026 033

Dr Ehrenstorfer 008 009 010 014 018 019 031 034 047 050 054 063 066

Fluka 002 033 070

Merck 007 033 056

Sigma/Aldrich 001 003 004 006 011 012 013 016 017 033 036 038 039 044 048 049 055 057 060 067 068 071 073 076

Institut of Dyes and Organic Products 035

Institute Of Leather Industry 015 022

LGC Standards 045 051

QMX 042


laboratory number

>85 036

>90 013

1 045

81,1 015 022

85 016

90 006

92.8 057

94.9 051

95 012 050 067 068

96 002 031 034 060

96.1 049

96.5 010 018 019 042 063

97 001

98 047 066

99.9 011

no 038

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laboratory number

yes 001 004 006 010 011 012 013 015 016 018 019 032 034 038 039 042 045 047 049 051 054 060 063 066 067 068 076

no 002 003 007 008 009 014 017 022 026 031 033 035 036 048 050 055 056 057 065 070 071


377 nm, 410 nm, 500 nm 070

400;473;525;625 076

476 039

478 010

480 031

500 022 026 049

505 018

506 012

510 011 033 065

512 057

520 015 017 035 051 068

550 038


156-196 071

353 -> 120, 197 009

353,2-197,2 / 128,1 / 156,1 063

353.0>76.9 (quantification trace) 353.0>156.2 045

353.1/197.1 055

353.1/197.1, 353.1/92.1 036

353.1>196 042

353.1>196.1 ; 353.1>197.1 060

353.1>76.9 014

353.1397 047

353.16 - 77 - 91.1 - 156.1 006

353.19>77.06 048

353.2/120.2, 353.2/156.2, 353.2/196.2 034

353.2>155.8, 353.2>119.7 004

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Ions monitored (MS/MS confirmation) (continued)

laboratory number

353/ 120, 156 001

353/128 019

353/156 353/120 044

353/77;353/196 003

353>156 057

353>77, 353>120 008

353-156 067

N 051

UPLC/MS/MS 050

yes 016 056

Sudan Red B


72 019

82.4 072

90 016

94 001

108 076


yes 001 004 009 016 072

no 007 017 033 036 047 054 056 060 067 071 076


Acros 033

Dr Ehrenstorfer 001 009 019 047 054

Fluka 033 036

Merck 007 033 056

Sigma/Aldrich 004 016 017 033 060 067 071 072 076

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laboratory number

85 016

90 019 047 067

95 001

97.8 072

100 060


laboratory number

yes 001 004 016 019 047 054 067 072

no 007 009 017 033 036 056 071 076


400;473;525;625 076

510 033

520 017


224-209-156-91 071

381 -> 156, 224 009

381.0/91.1, 381.0/65.2 036

381.1/106.1 019

381.1709 047

381.2/134.1>381.2/156.1 060

381.2>90.8, 381.2>105.8 004

381.2-90.9 067

381/ 224, 225 001

381>224, 381>156, 381>91 072

yes 016

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Sudan Red G


90 016

90.7 072

96 063

97 001

99 012

102 044 076



yes 001 004 006 009 012 016 042 044 063 072

no 003 007 013 033 035 036 047 048 054 055 056 057 060 067 076


Acros 033

Dr Ehrenstorfer 009 047 054 063

Fluka 002 033 035 036 048

Merck 007 012 033 056

Sigma/Aldrich 001 003 004 006 013 016 033 044 055 057 060 067 072 076

QMX 042


laboratory number

>90 013

85 006 016

90 067

93.5 042 047 063

96 002 060

98 012

100 057

unknown 001

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laboratory number

yes 001 004 006 012 013 016 042 047 054 063 067 076

no 002 003 007 009 033 035 036 048 055 056 057 072


96.0 036

400;473;525;625 076

495 057

506 012

510 033

520 035


279,0-122,9 / 108,1 / 156,1 063

279.1/108.1>279.1/123.0 060

279.1/123.1 055

279.1>156 042

279.1-108.2 067

279.1135 047

279.16 - 108.09 - 123.08 - 156.07 006

279.2/123.1, 279.2/108.1 036

279.2>156.1, 279.2>123.1 004

279.22>108.09 048

279/ 248, 156 001

279/123;279/108 003

279/156 279/108 044

279-> 156, 247 009

279>108 057

279>123, 279>156, 279>248 072

yes 016

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APPENDIX II: FAPAS SecureWeb, Protocol and Contact Details

1. FAPAS SECUREWEB

Access to the secure area of our website is only available to participants in our proficiency tests. Please contact us if you require a UserID and Password. FAPAS SecureWeb allows participants to:

• Obtain their laboratory numbers for the proficiency tests in which they have participated.

• View the results they submitted in past and current proficiency tests.

• Submit their results and methods for current tests.

• Review future tests they have ordered.

• Order proficiency tests, reference materials and quality control materials.

• Freely download copies of reports (PDF file), of proficiency tests in which they have participated.

• View charts of their z-scores obtained in previous FAPAS® proficiency tests.

2. PROTOCOL

The Protocols [3, 4] set out how FAPAS® is organised. Copies can be downloaded from our website.

3. CONTACT DETAILS

This report was prepared and authorised on behalf of FAPAS by Simon Hunter (Round Coordinator). Participants with any comments or concerns about this proficiency test should contact:

FAPAS

Fera Science Ltd (Fera) Sand Hutton

York YO41 1LZ

UK

Tel: +44 (0)1904 462100 Fax: +44 (0)1904 500440

[email protected]

www.fapas.com

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