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FAPAS® Report 04261

Aflatoxins B & G &/or total in Maize

May-June 2015

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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. All rights reserved.

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SUMMARY

1. The test material for FAPAS® proficiency test 04261 was dispatched in May 2015. Each

participant received a maize test material to be analysed for aflatoxins B1, B2, G1, G2

and/or total aflatoxin (AFB1, AFB2, AFG1, AFG2, total AF).

2. 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.

3. 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

AFB1 3.80 48 55 87

AFB2 1.89 45 50 90

AFG1 1.07 45 51 88

AFG2 1.00 45 50 90

AF (total) 7.67 57 61 93

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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 6

5. INTERPRETATION OF SCORES 7

6. REFERENCES 7

TABLES

Table 1: Results and z-Scores 8

Table 2: Participants’ Comments 13

Table 3: Assigned Values and Standard Deviations for Proficiency 13

Table 4: Number and Percentage of z-Scores where |z| ≤2 13

FIGURES

Figure 1: z-Scores for AFB1 14

Figure 2: z-Scores for AFB2 15

Figure 3: z-Scores for AFG1 16

Figure 4: z-Scores for AFG2 17

Figure 5: z-Scores for AF (total) 18

APPENDICES

APPENDIX I: Analytical Methods Used by Participants 19

APPENDIX II: FAPAS SecureWeb, Protocol and Contact Details 25

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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 test material was procured from a retail source and was found to contain no detectable AFB1, AFB2, AFG1 or AFG2. The test material was spiked with a solution of AFB1, AFB2, AFG1 and AFG2 and further mixed

Samples were stored at -20°C 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 1 May 2015. Test materials were sent to 67 participants.

3. RESULTS

The instructions for reporting results were as follows:

• Determine the level of aflatoxins B1, B2, G1, G2 and/or total aflatoxin, present in the test material, in μg/kg, as received, corrected for recovery.

Results were submitted by 66 participants (99%) before the closing date for this test, 11 June 2015.

Each participant was given a laboratory number, assigned in order of receipt of results. The reported analyte concentrations are given in Table 1.

Participants’ comments are given in Table 2.

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

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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),

iii) results from participants not quoting a percentage recovery, EXCEPT for total AF, where participants submitted results that were the sum of their recovery corrected individual aflatoxins.

For AFB1, AFB2, AFG1, AFG2 and AF (total), this procedure was straightforward and the robust mean was chosen as the assigned value.

The assigned values for all analytes are shown in Table 3.

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 AFB1, AFB2, AFG1, AFG2 and AF (total), 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 3.

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 all analytes are given in Table 1 and are shown as histograms in Figures 1–5. 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 3.

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The number and percentage of z-scores in the range -2 ≤ z ≤ 2 for all analytes are given in Table 4.

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.

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 10/05/2015.

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: Results and z-Scores

laboratory number

analyte

AFB1 AFB2 AFG1 AFG2 AF (total) assigned value

3.80 µg/kg assigned value

1.89 µg/kg assigned value

1.07 µg/kg assigned value

1.00 µg/kg assigned value

7.67 µg/kg

result recovery, %

z-score result recovery, %

z-score result recovery, %

z-score result recovery, %

z-score result recovery, %

z-score

µg/kg µg/kg µg/kg µg/kg µg/kg

001 3.02 93.53 -0.9 1.14 96.71 -1.8 3.55 97.79 10.5 1.12 97.58 0.6 8.83 96.40 0.7

002 3.6 83.9 -0.2 1.90 84.0 0.0 0.91 83.0 -0.7 1.11 65.7 0.5 7.5 -0.1

003 3.70 91 -0.1 1.63 96 -0.6 0.68 97 -1.7 0.71 82 -1.3 6.72 -0.6

004 3.8 113 0.0 2.1 102 0.5 1.0 107 -0.3 1.0 102 0.0 7.9 0.1

005 3.32 79.3 -0.6 1.67 86.9 -0.5 0.97 85.5 -0.4 0.97 89.6 -0.1 6.94 85.3 -0.4

006 3.1 95 -0.8 1.9 97 0.0 0.9 93 -0.7 0.9 93 -0.4 6.8 95 -0.5

007 3.83 96 0.0 1.85 96 -0.1 0.93 96 -0.6 0.91 96 -0.4 7.52 96 -0.1

008 3.23 96 -0.7 2.00 89 0.3 0.76 95 -1.3 0.81 81 -0.9 6.80 -0.5

009 4.04 83 0.3 2.04 89 0.4 1.24 71 0.7 1.17 76 0.8 8.49 0.5

010 3.90 87.3 0.1 1.98 91.5 0.2 1.03 88.4 -0.2 1.02 91.4 0.1 7.93 0.2

011 3.7 76 -0.1 1.8 69 -0.2 1.1 68 0.1 1.0 88 0.0 7.6 0.0

012 5.5 -1.3

013 3.18 79 -0.7 1.89 102 0.0 1.12 79 0.2 1.20 80 0.9 7.39 - -0.2

014 4.2 100 0.5 2 100 0.3 1.07 88.3 0.0 0.95 100 -0.2 8.2 100 0.3

015 7.3 -0.2

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

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Table 1: Results and z-Scores

laboratory number

analyte

AFB1 AFB2 AFG1 AFG2 AF (total) assigned value

3.80 µg/kg assigned value

1.89 µg/kg assigned value

1.07 µg/kg assigned value

1.00 µg/kg assigned value

7.67 µg/kg

result recovery, %

z-score result recovery, %

z-score result recovery, %

z-score result recovery, %

z-score result recovery, %

z-score

µg/kg µg/kg µg/kg µg/kg µg/kg

016 6.48 -0.7

017 3.6 109.7 -0.2 2.0 87.7 0.3 1.2 117.2 0.5 0.9 109.3 -0.4 7.7 106 0.0

018 12.35 73 10.2 16.00 75 4.9

019 3.82 99 0.0 1.81 97 -0.2 0.85 89 -0.9 0.90 96 -0.4 7.38 95 -0.2

020 4.74 91 1.1 2.63 93 1.8 1.25 96 0.8 1.27 96 1.2 9.89 94 1.3

021 3.25 83 -0.7 1.43 84 -1.1 0.72 95 -1.5 0.64 86 -1.6 6.04 -1.0

022 4.718 115.46 1.1 3.449 80.62 3.8 1.099 70.27 0.1 0.786 70.69 -1.0 10.052 84.26 1.4

023 4.07 100 0.3 1.91 100 0.0 1.17 100 0.4 1.14 100 0.6 8.29 100 0.4

024 3.5 110 -0.4 1.72 100 -0.4 1.26 100 0.8 1.03 100 0.1 7.51 100 -0.1

025 5 90.8 1.4 3 91.8 2.7 1 88.4 -0.3 1 82.8 0.0

026 5.83 2.4 8.18 0.3

027 3.03 100.0 -0.9

028 1.07 69.36 -3.3 1.15 83.88 -1.8 2.15 94.14 4.6 3.78 98.66 12.7 8.15 0.3

029 0.85 90.84% -3.5 0.93 84.51% -2.3 1.50 92.83% 1.8 3.50 76.11% 11.4 6.78 86.07% -0.5

030 5.6 80 - 120 -1.2

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

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Table 1: Results and z-Scores

laboratory number

analyte

AFB1 AFB2 AFG1 AFG2 AF (total) assigned value

3.80 µg/kg assigned value

1.89 µg/kg assigned value

1.07 µg/kg assigned value

1.00 µg/kg assigned value

7.67 µg/kg

result recovery, %

z-score result recovery, %

z-score result recovery, %

z-score result recovery, %

z-score result recovery, %

z-score

µg/kg µg/kg µg/kg µg/kg µg/kg

031 3.34 103.1 -0.6 1.55 100.3 -0.8 0.93 100.9 -0.6 0.92 97.9 -0.4 6.74 100.5 -0.6

032 3.38 94.82 -0.5 1.66 94.90 -0.6 0.86 97.29 -0.9 0.89 98.36 -0.5 6.79 96.34 -0.5

033 4.55 100 0.9 2.40 95 1.2 1.30 95 1.0 1.30 105 1.4 9.55 1.1

034 4.20 86 0.5 1.87 96 0.0 1.23 80 0.7 0.79 90 -0.9 8.09 0.2

035 3.34 90.83 -0.6 1.51 98.01 -0.9 0.83 100.46 -1.0 0.84 95.62 -0.7 6.52 96.23 -0.7

036 2.7 82.3% -2.9

037 4.0 89.7 0.2 1.9 94.4 0.0 1.1 90.1 0.1 1.0 87.1 0.0 8.0 0.2

038 3.23 97.20 -0.7 1.82 92.40 -0.2 1.03 93.30 -0.2 0.99 97.20 0.0 7.08 95.10 -0.4

039 3.696 99 -0.1 1.81 100 -0.2 0.836 100 -1.0 0.941 100 -0.3 7.283 100 -0.2

040 4.556 89.2 0.9 2.345 81.2 1.1 1.148 101.5 0.3 1.313 87.7 1.4

041 3.98 96 0.2 2.00 95 0.3 1.24 95 0.7 1.05 96 0.2 8.27 96 0.4

042 3.87 Standard Addition 0.1 1.84 Standard Addition -0.1 0.95 Standard Addition -0.5 0.96 Standard Addition -0.2 7.62 Standard Addition 0.0

043 3.62 -0.2 1.87 0.0 1.08 0.0 0.92 -0.4 7.49 -0.1

044 4 88.3 0.2 1.727 88.5 -0.4 0.8 110.5 -1.1 0.938 118.8 -0.3 7.465 -0.1

045 8 0.2

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

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Table 1: Results and z-Scores

laboratory number

analyte

AFB1 AFB2 AFG1 AFG2 AF (total) assigned value

3.80 µg/kg assigned value

1.89 µg/kg assigned value

1.07 µg/kg assigned value

1.00 µg/kg assigned value

7.67 µg/kg

result recovery, %

z-score result recovery, %

z-score result recovery, %

z-score result recovery, %

z-score result recovery, %

z-score

µg/kg µg/kg µg/kg µg/kg µg/kg

046 7.5 -0.1

047 4.02 0.3 2.06 0.4 0.81 -1.1 1.06 0.3 7.95 0.2

048 2.84 110.08 -1.1 1.35 107.30 -1.3 0.82 105.51 -1.1 0.68 102.61 -1.5 5.69 107.56 -1.2

049 2.65 -1.4 2.35 5.4

050 3.52 96.3 -0.3 2.13 82.6 0.6 1.06 102.9 0 1.18 51.2 0.8 7.89 92.1 0.1

051 3.50 120 -0.4 1.74 114 -0.4 1.01 102 -0.3 0.93 103 -0.3 7.18 110 -0.3

052 4.00 94.8 0.2 1.94 102.6 0.1 1.13 98.4 0.3 1.05 99.8 0.2 8.12 98.9 0.3

053 4.7 86 1.1 2.0 84 0.3 0.9 99 -0.7 1.0 80 0.0 8.6 0.5

054 3.79 101 0.0 2.00 96.5 0.3 1.16 96.7 0.4 1.04 96.6 0.2 7.99 / 0.2

055 3.7 84% -0.1 1.8 98% -0.2 1.1 76% 0.1 0.94 84% -0.3 7.5 -0.1

056 3.15 83 -0.8 2.73 96.3 2.0 1.906 101.9 3.5 1.212 86.5 1.0 8.999 91.925 0.8

057 3.82 95.1 0.0 2.16 98.0 0.7 1.17 94.2 0.4 0.83 96.0 -0.8 7.98 0.2

058 7.69 90 4.6 3.89 90 4.8 1.80 90 3.1 1.78 90 3.6 15.2 90 4.5

059 5.8 89 -1.1

060 6.83 42.1 3.6 30.2 47.5 68.1 3.08 23.0 8.5 28.2 25.8 123.8

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

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Table 1: Results and z-Scores

laboratory number

analyte

AFB1 AFB2 AFG1 AFG2 AF (total) assigned value

3.80 µg/kg assigned value

1.89 µg/kg assigned value

1.07 µg/kg assigned value

1.00 µg/kg assigned value

7.67 µg/kg

result recovery, %

z-score result recovery, %

z-score result recovery, %

z-score result recovery, %

z-score result recovery, %

z-score

µg/kg µg/kg µg/kg µg/kg µg/kg

061 3.796 88.3 0.0 1.507 88.5 -0.9 0.888 110.5 -0.8 0.929 118.8 -0.3 7.120 -0.3

062 5.9 -1.0

063 3.6 -0.2 6.7 -0.6

064 6.76 95.8 3.5 1.85 96.2 -0.1 1.35 92.1 1.2 0.51 89.3 -2.2 10.5 93.4 1.7

065 3.61 -2.4

066 7.3 -0.2

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

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Table 2: Participants’ Comments

participant number comments

024 Results for AFB2 , AFG1 , AFG2 are less than our reporting limits (5, 2.5 and 5 respectively)

035 Results for the test material 'as received' CORRECTED for recovery

047 standard addition

049 Not corrected for recovery

060 matrix-extracted calibration curve

066 Method AOAC 991.31 Fluorimetric, this result is not corrected by % recovery (our recovery is 90%).We do not understand how we fill the space for recovery therefore we decided to leave unfilled space.

comments are as submitted by participants

Table 3: Assigned Values and Standard Deviations for Proficiency

analyte data points, n

assigned value, xa µg/kg

uncertainty, u

standard deviation for proficiency, σp

AFB1 51 3.80 0.0917 Horwitz [6] 0.836

AFB2 48 1.89 0.0459 Horwitz [6] 0.416

AFG1 49 1.07 0.0332 Horwitz [6] 0.236

AFG2 48 1.00 0.0262 Horwitz [6] 0.22

AF (total) 50 7.67 0.149 Horwitz [6] 1.69

Table 4: Number and Percentage of z-Scores where |z| ≤2

analyte number of scores, |z| ≤2

total number of scores

% |z| ≤2

AFB1 48 55 87

AFB2 45 50 90

AFG1 45 51 88

AFG2 45 50 90

AF (total) 57 61 93

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Figure 1: z-Scores for AFB1

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Figure 2: z-Scores for AFB2

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Figure 3: z-Scores for AFG1

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Figure 4: z-Scores for AFG2

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Figure 5: z-Scores for AF (total)

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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.

Method Used Accredited laboratory number

yes 001 002 003 007 008 009 011 012 015 017 020 022 023 024 032 034 035 036 037 038 040 041 042 044 048 050 051 054 057 058 059 061 064

no 005 016 029 030 033 043 049 055 060 063 065 066

Method Based On laboratory number

International Standard 002 003 009 011 012 017 038 044 048 057 058 061 066

National Standard 001 007 015 022 032 035 041 042 051 054 060

Paper Published In An International Journal 005

Manufacturer/Kit Instructions/Technical Note 008 016 030 037 050 059 063 065

In house method 020 023 024 029 033 034 036 040 049 055 064

Sample Weight (g) laboratory number

≥2 - <5 024 029 030 033 063

≥5 - <10 035 036 042 044 049 050 051 055 060 061 064 065

≥10 - <25 007 009 011 012 015 016 020 023 034 041 054 057 058

≥25 - <50 003 017 032 038 040 048 059 066

≥50 001 002 005 008 022 037 043

Extraction Solvent Components laboratory number

acetone 007

acetonitrile 011 023 024 032 033 038 049 051 064

heptane 009

methanol 001 005 009 011 012 015 016 022 029 030 034 035 036 037 042 043 044 049 055 057 058 059 060 061 063 065 066

sodium chloride solution 009 023 042

water 002 003 007 008 009 011 015 016 017 020 024 032 034 036 037 038 040 042 043 048 049 050 054 055 060 063 064

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Extraction Procedure laboratory number

add NaCl 001 022 029 034 043 048 055 060 066

blend / homogenise with solvent 005 008 017 029 030 034 041 042 057 059 060

hot water extraction 065

maceration / homogenisation 020

shake with solvent 007 009 012 015 016 023 024 030 033 036 038 040 042 049 063 064

shaking 032 058

sonicate/ultrasonic bath 064

Ultra Turrax 002 011 034 037 043

ultrasonic extraction 054

vortex mix 035 042 050 060

Extraction Type laboratory number

single 001 002 005 007 008 009 011 016 017 020 023 024 029 030 032 034 036 037 041 042 043 048 049 050 054 055 057 059 060 063 065 066

multiple 003 012 015 022 033 035 038 040 044 051 058 061 064

Sample Work Up laboratory number

centrifuge 012 015 023 024 029 030 032 042 049 050 055 060 064

defatted with hexane 009

dilute 005 030 042 060 065

evaporate 029 033 060

filter 007 008 011 017 020 022 029 034 035 036 037 041 042 043 048 055 057 060 065 066

none 054

pH adjustment 016 038 043

Ultra Turrax 002

inmunoaffinity column 044

mix 065

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Sample Clean-up by Immunoaffinity Column (Brand)

laboratory number

R-Biopharm Rhone 002 008 009 020 037 038 041 042 044 050 057 058 061

VICAM 001 005 007 011 022 029 034 035 043 048 055 066

Micotox 033

AflaTest-P 060

IneratSep VAR-3 032

Sample Clean-up by SPE laboratory number

Romer Labs 033 040 041 051 054 064

Micotox 001 017 038

AflaTest-P 035

IneraSep VAR-3 032

Mycotoxin Determination laboratory number

ELISA 012 015 016 036 059 063 065

fluorometric 058 066

HPLC 001 002 003 005 007 008 009 011 017 020 023 029 032 034 035 037 038 040 041 042 043 044 048 050 054 055 057 060 061 064

ELISA EuroProxima 030

Immunoassay 049

LC-MS/MS 024 033 051

UPLC 022

HPLC Injection Volume (μl) laboratory number

≥5 - <10 017 032 033 044 061

≥10 - <25 001 008 022 035 041 054 055 064

≥25 - <50 009 020 023 024

≥50 - <100 005 007 011 029 034 043 048 051 057 058 060

≥100 - <150 002 003 037 038 040 050

≥150 042

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HPLC Column Packing laboratory number

C18 002 003 005 007 008 009 011 017 020 022 023 024 029 032 033 034 037 041 042 043 044 048 050 051 054 055 057 058 060 061 064

endcapped 001 034 040 043

Inertsil ODS - 3V 038

Waters High Strength Silica (HSS) C18 035

HPLC Column Temperature (°C) laboratory number

ambient 001 002 003 020 038 040 041 042 054 058 064

>ambient - <50 005 007 008 009 011 017 022 023 024 029 032 033 034 035 037 043 044 048 050 051 055 061

≥50 057 060

Mobile Phase Components laboratory number

acetate 023 024 033

acetic acid 064

acetone 023

acetonitrile 007 011 029 032 034 042 043 055 058

formic acid 023 060

HNO3 & KBr (for Kobra Cell) 007 042 043 050

methanol 005 007 009 011 022 024 029 032 034 035 037 038 041 042 043 050 051 055 058 060 064

water 001 002 003 005 007 008 009 011 017 020 023 024 029 032 034 037 038 040 041 043 044 048 054 055 057 058 060 061 064

Mobile Phase Flow Rate (ml/min) laboratory number

<0.25 033 035

≥0.25 - <0.75 007 011 017 022 023 024 044 050 060 061 064

≥0.75 - <1.25 001 002 003 005 008 009 020 029 032 034 037 041 043 048 055 057 058

≥1.25 - <1.75 038 042

≥1.75 - <2.25 040 054

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Post Column Mobile Phase Flow Rate (ml/min)

laboratory number

<0.25 033 041 055

≥0.25 - <0.75 007 017 023 038 058

≥0.75 001 003 043 048 054

HPLC Pre Column Derivatisation laboratory number

fluorescamine 032

none 020 023 033 041 043 044 054 061

KBr Derivetised 038

photochemical reactor 001

HPLC Post Column Derivatisation laboratory number

Kobra cell 002 003 007 008 020 038 040 042 043 048 050

pyridinium bromide perbromide (C5H6Br3N) 009 057 058

saturated iodine 041 055

TFA 032

none 001 023 033 044 061

photochemical 005

photochemical reactor 029

photochemische NSD 034

PHRED Photochemical Reactor for Enhanced Detection

017

Source of Standards laboratory number

Fluka 050

R-Biopharm Rhone 008 012 015 020 058 063 065

Romer Labs 016 023 033 040 054

Sigma/Aldrich 005 009 011 034 037 038 044 048 055 061 064

Supelco 002 003 029 032 035 057 059 060

VICAM 001 066

Micotox 017

biopure 007 043

Coring 007 042

Discovery Fine Chemicals 049

Fermentek 022

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Source of Standards (continued) laboratory number

JRC-IRMM 037

LGC standards 030

pribolab 041

HPLC Detector Type laboratory number

fluorescence 001 002 003 005 007 008 009 011 017 020 022 029 032 034 035 037 038 040 041 042 043 048 050 054 055 057 058

MS-MS 023 033 044 051 060 061 064

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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 Jennifer Leak (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

info@fapas.com

www.fapas.com

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