Not Controlled When Printed
FAPAS® Report 19194
Pesticide Residues in Tomato
June-July 2015
PRINTED
WHEN
CONTROLLED
NOT
Page 1 of 52 FAPAS Report 19194
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. PRINTED QUALITY SYSTEMS
FAPAS® is accredited by UKAS as complying with WHENthe 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,CONTROLLED 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 corruptionNOT 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.
Page 2 of 52 FAPAS Report 19194
SUMMARY
1. The test material for FAPAS® proficiency test 19194 was dispatched in June 2015. Each participant received a tomato test material
2. From a list of 213 pesticide residues, participants had to identify and quantify those present. The test material contained bifenthrin, dimethoate, flucythrinate, metalaxyl (sum), methiocarb sulfone, phenthoate, profenofos, propoxur, pyriproxyfen and tetradifon.
3. 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. Results for this proficiency test are summarised as follows:
analyte assigned value, xa number of scores, total number % |z| ≤2 µg/kg |z| ≤2 of scores PRINTED bifenthrin 77.0 84 96 88 dimethoate 183 79 94 84 flucythrinate 145 WHEN52 67 78 metalaxyl (sum) 163 74 88 84 methiocarb sulfone 174 25 39 64 phenthoate 27.2 64 74 86 profenofos 107 70 88 80 propoxur 36.1 69 80 86 pyriproxyfen 30.7 64 76 84 tetradifon CONTROLLED91.9 69 84 82
NOT
Page 3 of 52 FAPAS Report 19194
CONTENTS
1. INTRODUCTION 5 1.1. Proficiency Testing 5 2. TEST MATERIAL 5 2.1. Preparation and Screening 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 7 4.3. Individual z-Scores 7 5. INTERPRETATION OF SCORES 7 6. REFERENCES 8 TABLES Table 1: Results and z-Scores for Bifenthrin, Dimethoate, Flucythrinate and Metalaxyl (sum) PRINTED 9 Table 2: Results and z-Scores for Methiocarb sulfone, Phenthoate, Profenofos and Propoxur 17 Table 3: Results and z-Scores for Pyriproxyfen andWHEN Tetradifon 25 Table 4: Additional Pesticide Residues Reported 29 Table 5: Participants’ Comments 29 Table 6: Assigned Values and Standard Deviations for Proficiency 30 Table 7: Number and Percentage of z-Scores where |z| ≤2 30 FIGURES Figure 1: z-Scores for BifenthrinCONTROLLED 31 Figure 2: z-Scores for Dimethoate 32 Figure 3: z-ScoresNOT for Flucythrinate 33 Figure 4: z-Scores for Metalaxyl (sum) 34 Figure 5: z-Scores for Methiocarb sulfone 35 Figure 6: z-Scores for Phenthoate 36 Figure 7: z-Scores for Profenofos 37 Figure 8: z-Scores for Propoxur 38 Figure 9: z-Scores for Pyriproxyfen 39 Figure 10: z-Scores for Tetradifon 40 APPENDICES APPENDIX I: Analytical Methods Used by Participants 41 APPENDIX II: FAPAS SecureWeb, Protocol and Contact Details 52
Page 4 of 52 FAPAS Report 19194
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 and Screening
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 prepared from tomatoes, which were frozen whole and cryogenically milled. The bulk sample was split into two batches: one for spiking and one for the blank test material. PRINTED Sub-samples were taken to screen for the possible presence of incurred residues and the remainder was stored at -20°C. No incurred residues were detected at, or above, 30 μg/kg. Bifenthrin, dimethoate, flucythrinate, metalaxyl (parentWHEN compound only), methiocarb sulfone, phenthoate, profenofos, propoxur, pyriproxyfen and tetradifon were spiked into the test material. 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]. CONTROLLED These data showed sufficient homogeneity and were not included in the subsequent calculation of the assigned values. NOT 2.3. Dispatch
The start date was 15 June 2015. Test materials were sent to 112 participants.
3. RESULTS
The instructions for reporting results were as follows: 1) Determine the concentration of pesticide residues present in the test material, in µg/kg, as received, uncorrected for recovery, together with the percentage recovery and limit of quantification (LoQ). • All pesticide residues are to be reported as the parent compound only, unless specified otherwise on the results form. This included metalaxyl, which was to be reported as the sum of metalaxyl and metalaxyl-M.
Page 5 of 52 FAPAS Report 19194
• If any residues are reported not in the form specified, please note this in the comments box. • For residues tested for but not detected, please enter an LOQ via the ‘review/resubmit your results’ link on your list of tests. This has to be done after you have submitted results for all pesticide residues detected. • This is an identification and quantification test; therefore if you analyse for a pesticide that is in the test material, and do not identify it, and your limit of quantification is below the level needed for a satisfactory z-score or you do not submit an LoQ, you will be assessed as if your result was zero. Results were submitted by 107 participants (96%) before the closing date for this test, 28 July 2015. Each participant was given a laboratory number, assigned in order of receipt of results. The reported analyte concentrations are given in Table 1 for bifenthrin, dimethoate, flucythrinate and metalaxyl (sum); Table 2 for methiocarb sulfone, phenthoate, profenofos and propoxur and in Table 3 for pyriproxyfen and tetradifon. If a participant analysed for a pesticide residue that was in the test material, but did not identify it, and their LoQ (limit of quantification) was below the level needed for a z-score of -3.0 or an LoQ was not reported, they were assessed as if their result was zero. If a participant analysed for a pesticide residue that was in the test material, but did not identify it and their LoQ was above the level needed for a z-scorePRINTED of -3.0, then the result was recorded as 4. STATISTICAL EVALUATION OF RESULTS The results submitted by participants were statistically analysed in order to provide an assigned value for each analyte.CONTROLLED 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 TestingNOT 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) 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), ii) results where no percentage recovery was reported, iii) results whose recovery was outside the range 60-140% [6], iv) results where no limit of quantification was reported, Page 6 of 52 FAPAS Report 19194 v) results lower than the reported LoQ. For all analytes, this procedure was straightforward and the robust mean was chosen as the assigned value. The assigned values for all analytes 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 [7]. The values for σp used to calculate z-scores from the reported results of this test are given in Table 6. 4.3. Individual z-Scores Participants’ z-scores were calculated as: − xx )( z = a σ p where x = the participant’s reported result, PRINTED xa = the assigned value and σp = the standard deviation for proficiency. Participants’ z-scores for all analytes are given in Table 1 to Table 3 and shown as histograms in Figures 1–10. It is possible for the WHENz-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 all analytes are given in Table 7. 5. INTERPRETATION OF SCORES CONTROLLED 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 areNOT 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]. Page 7 of 52 FAPAS Report 19194 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 Analytical Quality Control and Validation Procedures for Pesticide Residues Analysis in Food and Feed, Document No. SANCO/12571/2013. 7 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. PRINTED WHEN CONTROLLED NOT Page 8 of 52 FAPAS Report 19194 Table 1: Results and z-Scores for Bifenthrin, Dimethoate, Flucythrinate and Metalaxyl (sum) laboratory analyte number bifenthrin dimethoate flucythrinate metalaxyl (sum) assigned value 77.0 μg/kg assigned value 183 μg/kg assigned value 145 μg/kg assigned value 163 μg/kg result recovery LoQ z-score result recovery LoQ z-score result recovery LoQ z-score result recovery LoQ z-score μg/kg % μg/kg μg/kg % μg/kg μg/kg % μg/kg μg/kg % μg/kg 001 76 92 10 -0.1 170 84 10 -0.3 147 84 10 0.1 200 89 10 1.1 002 55.69 103 50 -1.3 168.38 117 50 -0.4 # PRINTED 125.99 101 50 -1.1 003 75.6 109 10 -0.1 160.0 93 10 -0.6 162.9 127 10 0.6 158.7 101 10 -0.1 004 67.93 87.1 10 -0.5 177.20 104.6 10 -0.1 # 155.90 80.1 10 -0.2 005 93.11 86 10 0.9 221.25 83 10 1.0 WHEN 117.50 84 10 -0.9 154.15 10 -0.3 006 141.35 112.00 10 3.8 282.14 74.54 10 2.6 273.78 89.00 10 4.2 0 -4.8 007 79.30 91 10 0.1 179.17 90 10 -0.1 155.12 102 10 0.3 173.60 99 10 0.3 008 71.41 86 10 -0.3 0 -4.8 # 100.34 96 10 -1.8 009 78 87 10 0.1 150 97 10 -0.9 # 150 84 10 -0.4 010 70.00 -0.4 147.00 -0.9 134.00 -0.3 204.00 1.2 011 62 100 15 -0.9 163 100 15 -0.5 # 128 100 10 -1.0 012 55 81 10 -1.3 160 CONTROLLED93 10 -0.6 # 125 94 10 -1.1 013 74 100 2 -0.2 200 91 2 0.5 155 95 20 0.3 210 100 2 1.4 014 75.4 88.6 0.01 -0.1 NOT231.2 99.1 0.01 1.3 149.9 93.5 0.01 0.2 197.4 98.1 0.01 1.0 015 # # # # # = not analysed z-scores outside |z| >2 are shown in bold, see Section 5 Page 9 of 52 FAPAS Report 19194 Table 1 (continued): Results and z-Scores for Bifenthrin, Dimethoate, Flucythrinate and Metalaxyl (sum) laboratory analyte number bifenthrin dimethoate flucythrinate metalaxyl (sum) assigned value 77.0 μg/kg assigned value 183 μg/kg assigned value 145 μg/kg assigned value 163 μg/kg result recovery LoQ z-score result recovery LoQ z-score result recovery LoQ z-score result recovery LoQ z-score μg/kg % μg/kg μg/kg % μg/kg μg/kg % μg/kg μg/kg % μg/kg 016 86.1 108 0.03 0.5 169 102.8 .017 -0.4 # 190 106 .04 0.8 017 62 93 -0.9 173 105 -0.3 116 PRINTED99 -0.9 165 97 0.1 018 83 80 10 0.4 170 80 10 -0.3 84 80 10 -2.0 152 80 10 -0.3 019 75.3 -0.1 212 0.8 103 -1.3 195 0.9 020 85.4 113 50 0.5 255 110 20 1.9 WHEN # 165 109 20 0.1 021 78.10 77.6 10 0.1 196.30 109.4 10 0.4 134.35 72.2 10 -0.3 # 022 75.82 85.60 3 -0.1 190.00 96.60 3 0.2 293.35 100.20 3 4.8 165.86 86.30 3 0.1 023 75.00 110.31 0.004 -0.1 169.09 105.73 0.009 -0.4 154.28 105.85 0.04 0.3 152.49 109.67 0.002 -0.3 024 75.562 111.6 10 -0.1 194.907 112.2 10 0.3 121.246 91.3 10 -0.8 # 025 78 82 10 0.1 175 95 10 -0.2 # 176 101 10 0.4 026 66.79 91.49 10 -0.6 184.00 92.81 10 0.0 117.12 90.67 10 -0.9 158.50 84.75 10 -0.1 027 84 102 10 0.4 193 CONTROLLED103 10 0.3 175 100 10 1.0 161 95 10 -0.1 028 88 104 10 0.6 229 94 10 1.2 228 100 10 2.7 210 101 10 1.4 029 85.3 92.4 5 0.5 NOT168.3 106.2 5 -0.4 145.1 91.7 5 0.0 195.7 124.0 5 1.0 030 # # # 90 62 50 -2.1 # = not analysed z-scores outside |z| >2 are shown in bold, see Section 5 Page 10 of 52 FAPAS Report 19194 Table 1 (continued): Results and z-Scores for Bifenthrin, Dimethoate, Flucythrinate and Metalaxyl (sum) laboratory analyte number bifenthrin dimethoate flucythrinate metalaxyl (sum) assigned value 77.0 μg/kg assigned value 183 μg/kg assigned value 145 μg/kg assigned value 163 μg/kg result recovery LoQ z-score result recovery LoQ z-score result recovery LoQ z-score result recovery LoQ z-score μg/kg % μg/kg μg/kg % μg/kg μg/kg % μg/kg μg/kg % μg/kg 031 # # # 77.4 80 20 -2.5 032 # # # PRINTED # 033 82 107 20 0.3 169 101 20 -0.4 209 132 20 2.1 # 034 72 88 5 -0.3 189 105 2 0.2 135 78 3 -0.3 156 103 1 -0.2 035 78 100 10 0.1 195 100 10 0.3 WHEN 145 100 10 0.0 170 100 10 0.2 036 76 100 10 -0.1 185 100 10 0.1 143 100 10 0.0 180 100 10 0.5 037 86.69 5 0.6 137.61 10 -1.2 # 190.97 5 0.8 038 63 100 20 -0.8 427 100 20 6.5 111 100 20 -1.1 283 100 20 3.5 039 74 96 10 -0.2 196 83 10 0.4 144 84 10 0.0 177 56 10 0.4 040 78.4 103 50 0.1 156 97 10 -0.7 150 85 50 0.2 159 96 10 -0.1 041 69 10 -0.5 1000 10 21.7 298 10 5.0 970 10 23.6 042 71 75.2 10 -0.4 182 CONTROLLED118.6 10 0.0 121 75.3 10 -0.8 153 98.4 10 -0.3 043 0.077 98.6 0.01 -4.5 0.206 119.2 0.01 -4.8 0.137 110.0 0.01 -4.7 0.164 79.5 0.01 -4.8 044 # NOT# # # 045 82 84.5 10 0.3 150 80.3 10 -0.9 142 87.1 10 -0.1 160 89.3 10 -0.1 # = not analysed z-scores outside |z| >2 are shown in bold, see Section 5 Page 11 of 52 FAPAS Report 19194 Table 1 (continued): Results and z-Scores for Bifenthrin, Dimethoate, Flucythrinate and Metalaxyl (sum) laboratory analyte number bifenthrin dimethoate flucythrinate metalaxyl (sum) assigned value 77.0 μg/kg assigned value 183 μg/kg assigned value 145 μg/kg assigned value 163 μg/kg result recovery LoQ z-score result recovery LoQ z-score result recovery LoQ z-score result recovery LoQ z-score μg/kg % μg/kg μg/kg % μg/kg μg/kg % μg/kg μg/kg % μg/kg 046 68.19 99.39 10 -0.5 200.05 106.22 10 0.5 130.60 99.17 10 -0.5 144.23 89.92 10 -0.5 047 83 91 10 0.4 194 86 10 0.3 # PRINTED 179 91 10 0.5 048 82.12 96.32 10 0.3 194.74 85.10 10 0.3 # 169.44 99.98 10 0.2 049 80 79 10 0.2 210 107 10 0.7 185 97 10 1.3 95 107 10 -2.0 050 50.9 95.7 0.01 -1.5 190.6 111.9 0.01 0.2 WHEN 144.9 80.5 0.01 0.0 162.1 106.2 0.01 0.0 051 84 0.4 205 0.6 181 1.2 150 -0.4 052 84.7 100 10 0.5 206.4 100 10 0.6 219.0 100 50 2.4 190.4 100 50 0.8 053 # # # 99.6 80 10 -1.8 054 84 6 0.4 208 7 0.7 180 6 1.1 150 6 -0.4 055 48 90 30 -1.7 170 88 30 -0.3 78.5 85 30 -2.1 165 101 10 0.1 056 # 186.42 82 10 0.1 # # 057 162.1 85 10 5.0 167 CONTROLLED92 10 -0.4 # 143.6 89 10 -0.6 058 71.6435 -0.3 161.9465 -0.5 # 142.2521 -0.6 059 86.02 106 10 0.5 NOT160.19 84 10 -0.6 91.67 95 10 -1.7 160.64 96 10 -0.1 060 94 100 10 1.0 174 100 5 -0.2 # 203 100 10 1.2 # = not analysed z-scores outside |z| >2 are shown in bold, see Section 5 Page 12 of 52 FAPAS Report 19194 Table 1 (continued): Results and z-Scores for Bifenthrin, Dimethoate, Flucythrinate and Metalaxyl (sum) laboratory analyte number bifenthrin dimethoate flucythrinate metalaxyl (sum) assigned value 77.0 μg/kg assigned value 183 μg/kg assigned value 145 μg/kg assigned value 163 μg/kg result recovery LoQ z-score result recovery LoQ z-score result recovery LoQ z-score result recovery LoQ z-score μg/kg % μg/kg μg/kg % μg/kg μg/kg % μg/kg μg/kg % μg/kg 061 84.3 91 10 0.4 207.5 98 10 0.7 # 166.1 95 10 0.1 062 84 92 10 0.4 167 119 10 -0.4 161 PRINTED104 10 0.5 174 108 10 0.3 063 89.0 111.7 7.8 0.7 106.0 116.6 1.9 -2.0 # # 064 78.2 0.1 196.13 0.4 130.18 -0.5 # 065 74 -0.2 162 -0.5 WHEN 149 0.1 # 066 # # # # 067 81 95 1 0.2 100.6 93 1 -2.2 # 163.2 94 1 0.0 068 78 101 10 0.1 186 88 10 0.1 134 103 10 -0.3 176 89 10 0.4 069 73.5 101 10 -0.2 111 92.7 10 -1.9 0 -4.7 163.5 92.4 10 0.0 070 83 0.4 100.7 -2.2 # 160 -0.1 071 71.0 110 30 -0.4 97.7 85 20 -2.3 # 162.9 74 20 0.0 072 71 75 3.9 -0.4 99 CONTROLLED85 3.9 -2.2 146 76 3.9 0.0 # 073 95 96 10 1.1 211 116 10 0.8 150 102 10 0.2 0 -4.8 074 # NOT# # # 075 80 0.2 250 1.8 200 1.8 200 1.1 # = not analysed z-scores outside |z| >2 are shown in bold, see Section 5 Page 13 of 52 FAPAS Report 19194 Table 1 (continued): Results and z-Scores for Bifenthrin, Dimethoate, Flucythrinate and Metalaxyl (sum) laboratory analyte number bifenthrin dimethoate flucythrinate metalaxyl (sum) assigned value 77.0 μg/kg assigned value 183 μg/kg assigned value 145 μg/kg assigned value 163 μg/kg result recovery LoQ z-score result recovery LoQ z-score result recovery LoQ z-score result recovery LoQ z-score μg/kg % μg/kg μg/kg % μg/kg μg/kg % μg/kg μg/kg % μg/kg 076 63.9 10 -0.8 207 10 0.6 113.6 10 -1.0 184 10 0.6 077 70.2 94 10 -0.4 218.1 100 10 0.9 171.9 PRINTED96 10 0.9 162.1 94 10 0.0 078 629.35 94.64 10 32.6 # # # 079 76 98.4 5 -0.1 180 101.4 5 -0.1 0 -4.7 145 96.9 5 -0.5 080 73 84 10 -0.2 220 114 10 1.0 WHEN 125 90 10 -0.6 168 105 10 0.2 081 10.00 79.66 0.01 -4.0 # # # 082 72 98.30 8 -0.3 175 95.59 4 -0.2 0 -4.7 143 98.10 8 -0.6 083 # # # # 084 86.36 100 0.05 0.6 180.26 100 0.05 -0.1 # # 085 84.6 - 10.0 0.4 186.2 - 10.0 0.1 # 182.1 - 10.0 0.6 086 85 98 10 0.5 150 97 10 -0.9 160 102 10 0.5 180 100 10 0.5 087 73 93 0.01 -0.2 # CONTROLLED 137 82 0.01 -0.2 # 088 72 110 10 -0.3 180 91 10 -0.1 130 100 10 -0.5 190 87 10 0.8 089 0 10 -4.5 NOT201 104 10 0.5 155 103 50 0.3 211 106 10 1.4 090 86 97 10 0.5 175 107 10 -0.2 102 90 10 -1.4 210 135 10 1.4 # = not analysed z-scores outside |z| >2 are shown in bold, see Section 5 Page 14 of 52 FAPAS Report 19194 Table 1 (continued): Results and z-Scores for Bifenthrin, Dimethoate, Flucythrinate and Metalaxyl (sum) laboratory analyte number bifenthrin dimethoate flucythrinate metalaxyl (sum) assigned value 77.0 μg/kg assigned value 183 μg/kg assigned value 145 μg/kg assigned value 163 μg/kg result recovery LoQ z-score result recovery LoQ z-score result recovery LoQ z-score result recovery LoQ z-score μg/kg % μg/kg μg/kg % μg/kg μg/kg % μg/kg μg/kg % μg/kg 091 92 no 10 0.9 147 no 10 -0.9 382 no 10 7.7 75 no 10 -2.6 092 165.65 98 10 5.2 330.00 100 10 3.9 276.26 PRINTED100 10 4.3 172.00 84 10 0.3 093 66.89 84.9 10.00 -0.6 196.80 118.6 10.00 0.4 116.46 95.4 10.00 -0.9 91.53 86.4 10.00 -2.1 094 73 90 10 -0.2 218 91 10 0.9 159 89 10 0.5 177 104 10 0.4 095 68.3 86 10 -0.5 193 88 10 0.3 WHEN 130 84 10 -0.5 173 98 10 0.3 096 148 78.3 10 4.2 # # # 097 7.4 96.8 3.11 -4.1 170.74 72.0 8.03 -0.3 # 57.92 79.9 5.58 -3.1 098 72.8 95 10 -0.2 112.7 93 10 -1.9 139.4 94 10 -0.2 147.6 95 10 -0.4 099 0.072 -4.5 0.26 -4.8 0.084 -4.7 0.18 -4.8 100 0.0844 -4.5 0.2217 -4.8 0.1417 -4.7 0.182 -4.8 101 0 60.6 20 -4.5 0 106.3 20 -4.8 # 0 100.6 20 -4.8 102 60.1 70 10 -1.0 169.9 CONTROLLED82 10 -0.3 # 135 94 10 -0.8 103 56 95 10 -1.2 136 98 10 -1.2 108 94 10 -1.2 135 90 10 -0.8 104 # NOT0 -4.8 # 0 -4.8 105 68.36 109.59 10 -0.5 0 -4.8 # 168.67 72.48 10 0.2 # = not analysed z-scores outside |z| >2 are shown in bold, see Section 5 Page 15 of 52 FAPAS Report 19194 Table 1 (continued): Results and z-Scores for Bifenthrin, Dimethoate, Flucythrinate and Metalaxyl (sum) laboratory analyte number bifenthrin dimethoate flucythrinate metalaxyl (sum) assigned value 77.0 μg/kg assigned value 183 μg/kg assigned value 145 μg/kg assigned value 163 μg/kg result recovery LoQ z-score result recovery LoQ z-score result recovery LoQ z-score result recovery LoQ z-score μg/kg % μg/kg μg/kg % μg/kg μg/kg % μg/kg μg/kg % μg/kg 106 73 100 10 -0.2 200 120 10 0.5 142 110 10 -0.1 186 100 10 0.7 107 80 - 10 0.2 135 - 10 -1.3 100 PRINTED- 10 -1.4 150 - 10 -0.4 # = not analysed z-scores outside |z| >2 are shown in bold, see Section 5 WHEN CONTROLLED NOT Page 16 of 52 FAPAS Report 19194 Table 2: Results and z-Scores for Methiocarb Sulfone, Phenthoate, Profenofos and Propoxur laboratory analyte number methiocarb sulfone phenthoate profenofos propoxur assigned value 174 μg/kg assigned value 27.2 μg/kg assigned value 107 μg/kg assigned value 36.1 μg/kg result recovery LoQ z-score result recovery LoQ z-score result recovery LoQ z-score result recovery LoQ z-score μg/kg % μg/kg μg/kg % μg/kg μg/kg % μg/kg μg/kg % μg/kg 001 294 84 10 3.3 # 121 88 10 0.6 44 76 10 1.0 002 # # # PRINTED # = not analysed z-scores outside |z| >2 are shown in bold, see Section 5 Page 17 of 52 FAPAS Report 19194 Table 2 (continued): Results and z-Scores for Methiocarb Sulfone, Phenthoate, Profenofos and Propoxur laboratory analyte number methiocarb sulfone phenthoate profenofos propoxur assigned value 174 μg/kg assigned value 27.2 μg/kg assigned value 107 μg/kg assigned value 36.1 μg/kg result recovery LoQ z-score result recovery LoQ z-score result recovery LoQ z-score result recovery LoQ z-score μg/kg % μg/kg μg/kg % μg/kg μg/kg % μg/kg μg/kg % μg/kg 016 # 36.0 103.5 .01 1.5 116.3 105.6 .06 0.4 35.5 98.4 .04 -0.1 017 # 20 91 -1.2 89 PRINTED102 -0.8 31 100 -0.6 018 106 80 10 -1.9 24 80 10 -0.5 99 80 10 -0.3 41 80 10 0.6 019 183 0.2 21.5 -1.0 0 -4.5 35.7 0.0 020 # 28.2 78 20 0.2 WHEN 144 103 20 1.6 44.8 105 20 1.1 021 # 20.54 76.4 10 -1.1 89.80 91.2 10 -0.7 38.80 90.6 10 0.3 022 # 26.94 100.80 3 0.0 93.46 120.00 3 -0.6 28.67 65.60 3 -0.9 023 # 30.48 104.44 0.02 0.5 100.86 108.52 0.005 -0.2 # 024 # 20.445 85.3 10 -1.1 81.438 99.2 10 -1.1 33.432 104.6 10 -0.3 025 # 37 73 10 1.6 257 91 10 6.4 29 96 10 -0.9 026 # 19.47 92.57 10 -1.3 84.20 75.35 10 -1.0 37.30 98.37 10 0.2 027 # 27 CONTROLLED104 10 0.0 100 84 10 -0.3 28 96 10 -1.0 028 # 33 100 10 1.0 161 82 10 2.3 # 029 # NOT# 103.9 102.3 5 -0.1 40.5 106.0 5 0.6 030 # # = not analysed z-scores outside |z| >2 are shown in bold, see Section 5 Page 18 of 52 FAPAS Report 19194 Table 2 (continued): Results and z-Scores for Methiocarb Sulfone, Phenthoate, Profenofos and Propoxur laboratory analyte number methiocarb sulfone phenthoate profenofos propoxur assigned value 174 μg/kg assigned value 27.2 μg/kg assigned value 107 μg/kg assigned value 36.1 μg/kg result recovery LoQ z-score result recovery LoQ z-score result recovery LoQ z-score result recovery LoQ z-score μg/kg % μg/kg μg/kg % μg/kg μg/kg % μg/kg μg/kg % μg/kg 031 # 20.33 80 20 -1.2 72.48 80 20 -1.5 # 032 # # # PRINTED # 033 # 27 123 20 0.0 114 110 20 0.3 # 034 195 98 10 0.6 27 97 5 0.0 112 104 5 0.2 39 83 1 0.4 035 185 100 10 0.3 29 100 10 0.3 WHEN 110 100 10 0.1 42 100 10 0.7 036 183 100 10 0.2 29 100 10 0.3 106 100 10 0.0 41 100 10 0.6 037 # 24.56 5 -0.4 88.24 10 -0.8 31.87 10 -0.5 038 # # 280 100 20 7.4 118 100 20 10.3 039 156 85 10 -0.5 33 99 10 1.0 118 95 10 0.5 33 91 10 -0.4 040 # 25.1 90 20 -0.4 131 92 20 1.0 # 041 600 10 11.7 75 10 8.0 620 10 21.9 170 10 16.9 042 # 24 CONTROLLED81.6 10 -0.5 92 105.8 10 -0.6 33 77.8 10 -0.4 043 # 0.022 100.0 0.01 -4.5 0.106 103.7 0.01 -4.5 0.042 109.3 0.01 -4.5 044 # NOT# # # 045 # # 103 89.8 10 -0.2 78 88.2 10 5.3 # = not analysed z-scores outside |z| >2 are shown in bold, see Section 5 Page 19 of 52 FAPAS Report 19194 Table 2 (continued): Results and z-Scores for Methiocarb Sulfone, Phenthoate, Profenofos and Propoxur laboratory analyte number methiocarb sulfone phenthoate profenofos propoxur assigned value 174 μg/kg assigned value 27.2 μg/kg assigned value 107 μg/kg assigned value 36.1 μg/kg result recovery LoQ z-score result recovery LoQ z-score result recovery LoQ z-score result recovery LoQ z-score μg/kg % μg/kg μg/kg % μg/kg μg/kg % μg/kg μg/kg % μg/kg 046 # 24.24 97.77 10 -0.5 78.28 84.81 10 -1.2 28.95 83.78 10 -0.9 047 0 10 -4.8 34 90 10 1.1 100 PRINTED77 10 -0.3 34 90 10 -0.3 048 # 34.70 102.67 10 1.2 116.04 98.17 10 0.4 35.73 98.50 10 0.0 049 160 89 20 -0.4 22 99 10 -0.9 97 103 10 -0.4 32 99.8 10 -0.5 050 # 28.0 110.7 0.01 0.1 WHEN 125.1 113.1 0.01 0.8 # 051 # 21 -1.0 96 -0.5 32 -0.5 052 # # 134.4 100 10 1.2 # 053 # # # # 054 # 20 7 -1.2 90 6 -0.7 30 9 -0.8 055 # # 66 88 30 -1.7 40 108 30 0.5 056 # # # # 057 # 28.1 CONTROLLED81 10 0.1 0 -4.5 34.1 95 10 -0.3 058 # 19.3534 -1.3 76.7019 -1.3 # 059 405.50 78 10 6.4 NOT29.02 98 10 0.3 148.14 92 10 1.8 36.64 96 10 0.1 060 219 100 5 1.2 29 100 10 0.3 0 -4.5 43 100 10 0.9 # = not analysed z-scores outside |z| >2 are shown in bold, see Section 5 Page 20 of 52 FAPAS Report 19194 Table 2 (continued): Results and z-Scores for Methiocarb Sulfone, Phenthoate, Profenofos and Propoxur laboratory analyte number methiocarb sulfone phenthoate profenofos propoxur assigned value 174 μg/kg assigned value 27.2 μg/kg assigned value 107 μg/kg assigned value 36.1 μg/kg result recovery LoQ z-score result recovery LoQ z-score result recovery LoQ z-score result recovery LoQ z-score μg/kg % μg/kg μg/kg % μg/kg μg/kg % μg/kg μg/kg % μg/kg 061 172.3 85 10 -0.1 22.4 88 10 -0.8 96.8 90 10 -0.4 # 062 177 102 10 0.1 30 101 10 0.5 182 PRINTED102 10 3.2 37 117 10 0.1 063 # 23.0 109.5 1.9 -0.7 # 32.0 106.0 1.9 -0.5 064 # 25.41 -0.3 85.31 -0.9 30.1 -0.8 065 0 -4.8 30 0.5 WHEN 101 -0.2 34 -0.3 066 # # # # 067 # # # 28.8 95 1 -0.9 068 149 90 10 -0.7 28 118 10 0.1 111 118 10 0.2 34 91 10 -0.3 069 0 -4.8 0 -4.5 0 -4.5 24 102 10 -1.5 070 # # # 29 -0.9 071 # # # 26.3 82 10 -1.2 072 # # CONTROLLED 104 82 3.9 -0.1 # 073 # 36 99 10 1.5 92 100 10 -0.6 32 90 10 -0.5 074 # NOT# # # 075 220 1.3 41 2.3 150 1.8 40 0.5 # = not analysed z-scores outside |z| >2 are shown in bold, see Section 5 Page 21 of 52 FAPAS Report 19194 Table 2 (continued): Results and z-Scores for Methiocarb Sulfone, Phenthoate, Profenofos and Propoxur laboratory analyte number methiocarb sulfone phenthoate profenofos propoxur assigned value 174 μg/kg assigned value 27.2 μg/kg assigned value 107 μg/kg assigned value 36.1 μg/kg result recovery LoQ z-score result recovery LoQ z-score result recovery LoQ z-score result recovery LoQ z-score μg/kg % μg/kg μg/kg % μg/kg μg/kg % μg/kg μg/kg % μg/kg 076 153 10 -0.6 0 -4.5 108 10 0.1 0 -4.5 077 # 24.2 83 10 -0.5 96.9 PRINTED89 10 -0.4 41.3 100 10 0.7 078 # # # # 079 0 -4.8 21 98 5 -1.0 83 99.7 5 -1.0 33 99 10 -0.4 080 152 104 10 -0.6 23.9 98 10 -0.6 WHEN 100 105 10 -0.3 37 112 10 0.1 081 # # # # 082 0 -4.8 20 97.69 6 -1.2 81 98.56 4 -1.1 30 100.24 10 -0.8 083 # 24.7 95.0 10.0 -0.4 90.7 90.0 10.0 -0.7 # 084 # 24.94 100 0.05 -0.4 80.88 100 0.05 -1.1 # 085 112.9 - 10.0 -1.7 25.2 - 10.0 -0.3 100.3 - 10.0 -0.3 33.1 - 10.0 -0.4 086 130 91 10 -1.2 33 103 10 1.0 130 97 10 1.0 36 99 10 0.0 087 # # CONTROLLED # # 088 140 100 10 -0.9 32 103 10 0.8 120 109 10 0.6 42 83 10 0.7 089 187 111 10 0.3 NOT28 117 10 0.1 155 110 10 2.1 40 108 10 0.5 090 135 108 10 -1.1 34 94 10 1.1 123 112 10 0.7 41 127 10 0.6 # = not analysed z-scores outside |z| >2 are shown in bold, see Section 5 Page 22 of 52 FAPAS Report 19194 Table 2 (continued): Results and z-Scores for Methiocarb Sulfone, Phenthoate, Profenofos and Propoxur laboratory analyte number methiocarb sulfone phenthoate profenofos propoxur assigned value 174 μg/kg assigned value 27.2 μg/kg assigned value 107 μg/kg assigned value 36.1 μg/kg result recovery LoQ z-score result recovery LoQ z-score result recovery LoQ z-score result recovery LoQ z-score μg/kg % μg/kg μg/kg % μg/kg μg/kg % μg/kg μg/kg % μg/kg 091 # 22 no 10 -0.9 100 no 10 -0.3 38 no 10 0.2 092 # 25.60 96 10 -0.3 59.70 PRINTED70 10 -2.0 # 093 0 -4.8 22.30 90.9 10.00 -0.8 90.81 95.2 10.00 -0.7 40.60 135.7 10.00 0.6 094 # 20 98 10 -1.2 72 98 10 -1.5 38 95 10 0.2 095 158 107 10 -0.5 20.0 87 10 -1.2 WHEN 82.7 96 10 -1.0 33.8 95 10 -0.3 096 # # # # 097 # 9.24 93.23 3.21 -3.0 36.22 90.63 6.59 -3.0 28.33 82.09 2.46 -1.0 098 101.1 98 10 -2.0 28.9 94 10 0.3 100.7 96 10 -0.3 33.1 93 10 -0.4 099 0.14 -4.8 0.038 -4.5 0.12 -4.5 0.039 -4.5 100 0.1406 -4.8 0.0303 -4.5 0.1186 -4.5 0.0363 -4.5 101 # # # # 102 137.1 82 10 -1.0 0 CONTROLLED -4.5 90.4 76 10 -0.7 34.8 82 10 -0.2 103 # # # 36 115 10 0.0 104 # NOT # = not analysed z-scores outside |z| >2 are shown in bold, see Section 5 Page 23 of 52 FAPAS Report 19194 Table 2 (continued): Results and z-Scores for Methiocarb Sulfone, Phenthoate, Profenofos and Propoxur laboratory analyte number methiocarb sulfone phenthoate profenofos propoxur assigned value 174 μg/kg assigned value 27.2 μg/kg assigned value 107 μg/kg assigned value 36.1 μg/kg result recovery LoQ z-score result recovery LoQ z-score result recovery LoQ z-score result recovery LoQ z-score μg/kg % μg/kg μg/kg % μg/kg μg/kg % μg/kg μg/kg % μg/kg 106 # # = not analysed z-scores outside |z| >2 are shown in bold, see Section 5 WHEN CONTROLLED NOT Page 24 of 52 FAPAS Report 19194 Table 3: Results and z-Scores for Pyriproxyfen and Tetradifon laboratory analyte number pyriproxyfen tetradifon assigned value 30.7 μg/kg assigned value 91.9 μg/kg result recovery LoQ z-score result recovery LoQ z-score μg/kg % μg/kg μg/kg % μg/kg 001 30 113 10 -0.1 86 70 10 -0.3 002 21.55 101 50 -1.4 0 10 -4.5 003 32.8 96 10 0.3 128.9 104 10 1.8 004 30.76 94.8 10 0.0 98.14 90.4 10 0.3 005 32.37 61 10 0.3 86.04 60 10 -0.3 006 68.28 84.12 10 5.6 161.05 92.30 10 3.4 007 33.00 121 10 0.3 104.70 96 10 0.6 008 38.95 108 10 1.2 73.03 74 10 -0.9 009 26 91 10 -0.7 83 86 10 -0.4 010 # 79.00 PRINTED -0.6 011 # 83 100 15 -0.4 012 35 120 10 0.6 135 95 10 2.1 013 43 105 2 1.8 WHEN 109 90 5 0.8 014 26.9 82.4 0.01 -0.6 80.5 90.2 0.01 -0.6 015 # # 016 # 72.7 104 .034 -1.0 017 # 65 74 -1.3 018 27 80 10 -0.5 68 80 10 -1.2 019 43.5 1.9 0 -4.5 CONTROLLED 020 # # 021 22.48 79.2 10 -1.2 72.98 76.9 10 -0.9 022 NOT 27.32 79.50 3 -0.5 83.94 75.60 3 -0.4 023 # # 024 23.976 107.3 10 -1.0 70.207 101.8 10 -1.1 025 # 117 91 10 1.2 026 27.36 95.68 10 -0.5 71.08 82.02 10 -1.0 027 28 106 10 -0.4 81 98 10 -0.5 028 33 88 10 0.3 173 99 50 4.0 # = not analysed z-scores outside |z| >2 are shown in bold, see Section 5 Page 25 of 52 FAPAS Report 19194 Table 3 (continued): Results and z-Scores for Pyriproxyfen and Tetradifon laboratory analyte number pyriproxyfen tetradifon assigned value 30.7 μg/kg assigned value 91.9 μg/kg result recovery LoQ z-score result recovery LoQ z-score μg/kg % μg/kg μg/kg % μg/kg 029 26.7 89.4 5 -0.6 88.1 84.8 5 -0.2 030 # 30 112 50 -3.1 031 # # 032 # # 033 232 123 20 29.8 85 95 20 -0.3 034 30 100 2 -0.1 84 99 1 -0.4 035 48 100 10 2.6 100 100 10 0.4 036 48 100 10 2.6 118 100 10 1.3 037 26.13 5 -0.7 79.16 PRINTED 5 -0.6 038 45 100 20 2.1 60 100 20 -1.6 039 35 92 10 0.6 112 103 10 1.0 040 29.2 116 10 -0.2 WHEN 100 91 20 0.4 041 162 10 19.5 0 -4.5 042 19 64.7 10 -1.7 81 90.1 10 -0.5 043 0.027 95.3 0.01 -4.5 0.075 98.8 0.01 -4.5 044 # # 045 # # 046 28.77 105.07 10 -0.3 83.31 105.72 10 -0.4 047 36 CONTROLLED88 10 0.8 109 76 10 0.8 048 30.24 89.99 10 -0.1 104.03 91.23 10 0.6 049 NOT 32 99 10 0.2 84 104 10 -0.4 050 # 101.9 99.2 0.01 0.5 051 33 0.3 95 0.2 052 36.2 100 20 0.8 108.2 100 50 0.8 053 # # 054 35 6 0.6 95 7 0.2 055 31.5 110 30 0.1 60 89 30 -1.6 056 24.63 80 10 -0.9 # # = not analysed z-scores outside |z| >2 are shown in bold, see Section 5 Page 26 of 52 FAPAS Report 19194 Table 3 (continued): Results and z-Scores for Pyriproxyfen and Tetradifon laboratory analyte number pyriproxyfen tetradifon assigned value 30.7 μg/kg assigned value 91.9 μg/kg result recovery LoQ z-score result recovery LoQ z-score μg/kg % μg/kg μg/kg % μg/kg 057 25.9 85 10 -0.7 0 -4.5 058 15.6717 -2.2 23.75 -3.4 059 34.44 102 10 0.6 104.92 95 5 0.6 060 38 100 10 1.1 119 100 10 1.3 061 28.6 96 10 -0.3 86.1 91 10 -0.3 062 35 97 10 0.6 95 98 10 0.2 063 # # 064 24.86 -0.9 77.93 -0.7 065 27 -0.5 84 PRINTED -0.4 066 # # 067 # # 068 31 92 10 0.0 WHEN 95 105 10 0.2 069 0 -4.5 0 -4.5 070 # # 071 # # 072 # # 073 40 97 10 1.4 104 86 10 0.6 074 # 90 -0.1 075 40 CONTROLLED 1.4 90 -0.1 076 # 59.8 10 -1.6 077 NOT 30.8 100 10 0.0 93.8 94 10 0.1 078 # 83.00 91.35 10 -0.4 079 27 102.2 5 -0.5 101 100.5 6 0.4 080 25 101 10 -0.8 82 95 10 -0.5 081 # # 082 26 99.40 6 -0.7 90 100.31 8 -0.1 083 27.8 92.8 10.0 -0.4 # 084 # # # = not analysed z-scores outside |z| >2 are shown in bold, see Section 5 Page 27 of 52 FAPAS Report 19194 Table 3 (continued): Results and z-Scores for Pyriproxyfen and Tetradifon laboratory analyte number pyriproxyfen tetradifon assigned value 30.7 μg/kg assigned value 91.9 μg/kg result recovery LoQ z-score result recovery LoQ z-score μg/kg % μg/kg μg/kg % μg/kg 085 28.6 - 10.0 -0.3 # 086 30 99 10 -0.1 119 100 10 1.3 087 28 85 0.01 -0.4 # 088 31 91 10 0.0 82 101 10 -0.5 089 35 110 10 0.6 85 108 20 -0.3 090 34 88 10 0.5 110 99 10 0.9 091 33 no 10 0.3 99 no 10 0.3 092 0 -4.5 160.84 79 10 3.4 093 26.18 94.0 10.00 -0.7 84.76 PRINTED89.7 10.00 -0.4 094 25 97 10 -0.8 51 119 10 -2.0 095 29.5 110 10 -0.2 74.2 90 10 -0.9 096 # WHEN 186 80.4 10 4.7 097 # 57.12 90.3 7.00 -1.7 098 29.2 94 10 -0.2 87.4 95 10 -0.2 099 0.040 -4.5 0.11 -4.5 100 0.03324 -4.5 0.1324 -4.5 101 # # 102 21.1 80 10 -1.4 81.8 85 10 -0.5 103 23 CONTROLLED82 10 -1.1 65 91 10 -1.3 104 # # 105 NOT # # 106 23 100 10 -1.1 77 100 10 -0.7 107 30 - 10 -0.1 85 - 10 -0.3 # = not analysed z-scores outside |z| >2 are shown in bold, see Section 5 Page 28 of 52 FAPAS Report 19194 Table 4: Additional Pesticide Residues Reported laboratory number pesticide residue >30 μg/kg result recovery LoQ μg/kg % μg/kg 002 cypermethrin 111.26 119 50 093 cypermethrin 75.39 94.1 10.00 104 chlorpyrifos (-ethyl) 748.6 90 30 Table 5: Participants’ Comments participant number comments 002 The result of Metalaxyl is only Metalaxyl, not sum 018 Trace of Methiocarb and Metiocarb sulfoxide 020 We have not reference standard: Metalaxyl - M, so result is Metalaxyl only. 023 metalaxyl only metalaxyl not conclude metalaxylPRINTED-M 030 Laboratory test for Metalaxyl and not Metalaxyl-M. Results are for the Metalaxyl not sum. 047 The pesticides that are not detected shows bad recovery , not in range (70- 120)% WHEN 052 In Blank 19194b sample we detected traces (6 ug/kg) of Spinosad. This value is under ower LOQ (10ug/kg) 057 The test material was not delivered in proper temperature conditions.We mean it was not cold. So the pesticides such as Bifenthrine might have decomposed. 063 Analysis method : QuEChERS method(EN) 073 Mirex: 183 µg/kg 089 We alsoCONTROLLED found bifenazaat with a concentration of 79 µg/kg comments are as submitted by participants NOT Page 29 of 52 FAPAS Report 19194 Table 6: Assigned Values and Standard Deviations for Proficiency analyte data points, assigned value, uncertainty, standard deviation for n xa, μg/kg u proficiency, σp, μg/kg bifenthrin 74 77.0 1.22 Horwitz [7] 16.9 dimethoate 71 183 3.28 Horwitz [7] 37.7 flucythrinate 49 145 4.08 Horwitz [7] 30.9 metalaxyl (sum) 65 163 3.48 Horwitz [7] 34.2 methiocarb sulfone 23 174 10.0 Horwitz [7] 36.3 phenthoate 54 27.2 0.801 Horwitz [7] 5.99 profenofos 66 107 3.16 Horwitz [7] 23.5 propoxur 57 36.1 0.776 Horwitz [7] 7.94 pyriproxyfen 58 30.7 0.773 Horwitz [7] 6.75 tetradifon 62 91.9 2.62 Horwitz [7] 20.2 PRINTED Table 7: Number and Percentage of z-Scores where |z| ≤2 WHEN analyte number of scores where total number % |z| ≤2 |z| ≤2 of scores bifenthrin 84 96 88 dimethoate 79 94 84 flucythrinate 52 67 78 metalaxyl (sum) CONTROLLED74 88 84 methiocarb sulfone 25 39 64 phenthoate 64 74 86 profenofos NOT 70 88 80 propoxur 69 80 86 pyriproxyfen 64 76 84 tetradifon 69 84 82 Page 30 of 52 FAPAS Report 19194 8.0 7.0 6.0 5.0 4.0 3.0 z - score PRINTED 2.0 110.9 µg/kg 1.0 WHEN 0.0 77.0 µg/kg -1.0 -2.0 43.1 µg/kg -3.0 -4.0 CONTROLLED -5.0 2 4 8 3 1 9 7 5 6 89 99 43 97 81 55 50 12 11 17 38 76 26 93 46 95 41 10 77 42 71 72 58 34 82 88 98 80 87 94 69 13 39 65 23 19 14 24 22 36 79 25 35 68 21 64 40 49 75 67 33 45 48 18 47 70 27 51 54 62 61 85 52 86 29 20 90 59 16 84 37 28 63 91 60 73 96 57 92 78 101 100 103 102 105 106 107 NOT Laboratory Number Figure 1: z-Scores for Bifenthrin Page 31 of 52 FAPAS Report 19194 8.0 7.0 6.0 5.0 4.0 3.0 z - score PRINTED 2.0 258 µg/kg 1.0 WHEN 0.0 183 µg/kg -1.0 -2.0 107 µg/kg -3.0 -4.0 CONTROLLED -5.0 8 9 3 2 1 4 7 5 6 43 99 71 72 67 70 63 69 98 37 10 91 45 86 40 12 59 58 65 11 57 62 29 16 33 23 18 55 97 17 60 25 82 90 79 88 84 42 26 36 68 85 56 34 22 50 27 95 47 48 24 35 39 64 21 93 13 46 89 51 52 76 61 54 49 73 19 94 77 80 28 14 75 20 92 38 41 101 104 105 100 107 103 102 106 NOT Laboratory Number Figure 2: z-Scores for Dimethoate Page 32 of 52 FAPAS Report 19194 8.0 7.0 6.0 5.0 4.0 3.0 z - score PRINTED 2.0 206 µg/kg 1.0 WHEN 0.0 145 µg/kg -1.0 -2.0 83 µg/kg -3.0 -4.0 CONTROLLED -5.0 100 107 103 106 69 79 82 99 43 55 18 59 90 19 38 76 17 93 26 42 24 80 88 95 64 46 10 68 21 34 87 98 45 36 39 50 35 29 72 65 14 40 73 23 13 89 94 86 62 77 27 54 51 49 75 33 52 28 92 22 41 91 5 1 7 3 6 NOT Laboratory Number Figure 3: z-Scores for Flucythrinate Page 33 of 52 FAPAS Report 19194 8.0 7.0 6.0 5.0 4.0 3.0 z - score PRINTED 2.0 231 µg/kg 1.0 WHEN 0.0 163 µg/kg -1.0 -2.0 94 µg/kg -3.0 -4.0 CONTROLLED -5.0 6 8 2 9 5 4 3 7 1 73 43 99 97 91 31 30 93 49 53 12 11 58 82 57 46 79 98 51 54 18 23 42 34 26 40 45 70 59 27 50 77 71 67 69 17 20 55 22 61 80 48 35 92 95 62 25 68 39 94 47 36 86 85 76 16 88 52 37 19 29 14 75 60 10 13 28 90 89 38 41 101 104 100 102 103 107 105 106 NOT Laboratory Number Figure 4: z-Scores for Metalaxyl (sum) Page 34 of 52 FAPAS Report 19194 8.0 7.0 6.0 5.0 4.0 3.0 z - score PRINTED 2.0 247 µg/kg 1.0 WHEN 0.0 174 µg/kg -1.0 -2.0 102 µg/kg -3.0 -4.0 CONTROLLED -5.0 100 102 12 47 65 69 79 82 93 99 98 18 85 86 10 90 88 68 80 76 39 95 49 61 62 19 36 35 89 34 60 75 59 41 6 3 5 7 1 NOT Laboratory Number Figure 5: z-Scores for Methiocarb Sulfone Page 35 of 52 FAPAS Report 19194 8.0 7.0 6.0 5.0 4.0 3.0 z - score PRINTED 2.0 39.2 µg/kg 1.0 WHEN 0.0 27.2 µg/kg -1.0 -2.0 15.2 µg/kg -3.0 -4.0 CONTROLLED -5.0 5 4 7 3 6 69 76 43 99 97 58 26 17 54 82 94 95 31 24 21 14 51 79 19 49 91 93 61 10 63 80 18 42 77 46 37 83 84 40 85 64 92 22 27 33 34 50 68 89 57 20 98 35 36 60 59 62 65 23 88 28 39 86 47 90 48 13 16 73 25 75 41 102 100 NOT Laboratory Number Figure 6: z-Scores for Phenthoate Page 36 of 52 FAPAS Report 19194 8.0 7.0 6.0 5.0 4.0 3.0 z - score PRINTED 2.0 154 µg/kg 1.0 WHEN 0.0 107 µg/kg -1.0 -2.0 60 µg/kg -3.0 -4.0 CONTROLLED -5.0 5 4 8 3 1 7 6 19 57 60 69 43 99 97 92 55 94 31 58 11 46 84 82 24 95 79 26 64 37 17 21 54 83 93 42 73 22 51 61 77 49 18 12 27 47 80 91 85 98 23 65 45 29 72 10 36 76 35 68 34 33 48 16 39 88 90 50 86 14 40 52 20 59 75 89 28 30 62 25 38 13 41 100 105 102 106 107 104 NOT Laboratory Number Figure 7: z-Scores for Profenofos Page 37 of 52 FAPAS Report 19194 8.0 7.0 6.0 5.0 4.0 3.0 z - score PRINTED 2.0 52.0 µg/kg 1.0 WHEN 0.0 36.1 µg/kg -1.0 -2.0 20.2 µg/kg -3.0 -4.0 CONTROLLED -5.0 7 3 4 1 8 6 5 12 76 99 43 69 71 27 97 22 67 46 25 70 11 54 82 64 17 37 49 51 63 73 39 42 79 85 98 24 95 13 47 65 68 57 15 16 19 48 86 59 62 80 26 91 94 21 34 55 75 89 29 93 18 36 90 77 14 35 88 60 20 10 45 38 41 104 105 100 106 102 107 103 NOT Laboratory Number Figure 8: z-Scores for Propoxur Page 38 of 52 FAPAS Report 19194 8.0 7.0 6.0 5.0 4.0 3.0 z - score PRINTED 2.0 44.2 µg/kg 1.0 WHEN 0.0 30.7 µg/kg -1.0 -2.0 17.2 µg/kg -3.0 -4.0 CONTROLLED -5.0 2 9 1 4 5 3 7 8 6 69 92 43 99 58 42 21 24 56 64 80 94 57 82 37 93 29 14 18 65 79 22 26 83 27 87 61 85 46 40 98 95 34 86 48 77 68 88 55 49 28 51 91 90 59 12 39 54 62 89 47 52 60 73 75 13 19 38 35 36 41 33 100 102 103 106 107 NOT Laboratory Number Figure 9: z-Scores for Pyriproxyfen Page 39 of 52 FAPAS Report 19194 5.0 4.0 3.0 2.0 132.4 µg/kg z 1.0 - score PRINTED 0.0 91.9 µg/kg -1.0 WHEN -2.0 51.5 µg/kg -3.0 -4.0 CONTROLLED -5.0 2 8 9 1 5 4 7 3 6 19 41 57 69 43 99 58 30 94 97 76 38 55 17 18 24 26 16 21 95 64 10 37 14 27 42 80 88 11 78 46 22 34 49 65 93 33 89 61 98 29 74 75 82 77 51 54 62 68 91 35 40 79 50 73 48 59 52 13 47 90 39 25 36 60 86 12 92 28 96 100 103 106 102 107 NOT Laboratory Number Figure 10: z-Scores for Tetradifon Page 40 of 52 FAPAS Report 19194 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. Accredited Method Used laboratory number yes 001 002 003 004 005 007 009 011 014 017 021 023 024 025 026 027 029 030 034 037 040 042 043 044 045 046 047 048 049 050 051 052 056 057 059 061 062 063 064 066 067 068 070 071 072 073 077 080 081 082 086 087 089 090 093 094 095 098 101 102 103 no 006 008 013 022 028 033 038 058 069 084 085 096 104 105 106 Method Based On laboratory number International Standard 003 005 008 013 014 021 022 029 033 037 047 049 051 052 061 062 068 077 080 081 082 085 086 090 094 096 101 102 106 National Standard 006 023 024 026 027 042 043 044 045 046 048 050 059 063 067 069 070 071 072 073 Paper Published in an International Journal 009 017 025 030 057PRINTED 095 103 104 105 Manufacturer/Kit Instructions/Technical Note 064 In house method 001 002 004 007 011 028 034 040 056 066 084 087 089 098 WHEN Quoted Percentage Recovery Measured in laboratory number Same Analytical Batch as Test Material yes 001 002 004 006 007 008 009 013 017 021 022 023 024 025 026 027 028 033 034 040 042 043 044 045 046 047 048 049 050 051 056 057 059 061 063 064 066 067 068 071 072 073 080 081 082 084 085 089 090 093 094 095 098 101 102 103 104 105 106 no CONTROLLED003 005 011 029 030 037 052 062 069 070 077 086 087 096 NOT If Measured in This Batch, Stage at Which laboratory number the Spike Was Added prior to extraction 001 002 004 006 007 008 009 013 014 017 021 022 023 024 025 026 027 028 033 034 037 040 042 043 044 045 046 047 048 049 051 052 056 057 059 061 063 064 066 067 068 069 071 072 073 080 081 082 084 085 090 093 094 095 098 101 102 103 104 105 106 prior to instrument measurement 089 Page 41 of 52 FAPAS Report 19194 Concentration of Spike (µg/kg) laboratory number ≥5 - <10 022 037 051 056 082 ≥10 - <25 004 025 034 043 067 077 093 095 098 103 105 106 ≥25 - <50 006 009 017 057 064 066 068 080 084 101 104 ≥50 - <100 001 007 013 014 021 024 026 027 028 030 033 042 044 046 048 049 050 052 059 061 063 069 071 073 085 090 102 ≥100 002 008 023 040 045 047 062 072 081 086 089 094 Composition of Blank Commodity used laboratory number for Spiking tomato blank provided 002 004 007 008 013 021 024 026 027 030 033 034 037 040 044 045 046 047 048 049 051 056 061 063 064 066 067 068 072 073 077 080 081 082 084 087 089 090 094 098 101 103 106 tomato test material provided 006 014 023 028 042 043 050 059 069 085 095 102 tomato 052 062 105 cucumber 104 PRINTED pear 071 Calibration laboratoryWHEN number standard addition 034 056 067 070 080 085 093 102 matrix-matched 002 004 005 006 013 014 021 022 023 024 025 026 027 029 030 034 040 042 043 044 045 046 047 048 049 050 051 052 056 057 061 063 064 066 068 073 077 081 082 086 087 094 095 098 101 102 105 solvent 003 033 034 multi-level 001 004 007 008 009 011 013 017 023 025 028 030 033 037 043 045 056 062 069 071 CONTROLLED072 084 089 090 095 098 103 106 single-level 034 059 104 NOT Internal Standard Added laboratory number yes 002 004 005 007 008 009 014 021 022 024 025 026 027 028 030 033 034 037 042 043 044 046 047 048 052 059 061 062 063 064 067 068 073 080 086 089 093 094 096 098 101 105 106 no 001 003 006 011 013 017 023 029 038 040 045 049 050 051 056 057 066 069 070 071 072 077 081 082 084 085 087 090 095 102 103 104 Page 42 of 52 FAPAS Report 19194 Internal Standard Used laboratory number alodan 034 anilofos 059 anthracene 089 anthracene D10 033 carbendazim D4 062 DEE 061 diuron D6 034 fenchlorfos 094 heptachlor-epoxide 044 isoproturon 059 linuron D6 005 mirex 034 080 nicarbazin 080 PCB 209 062 PCB187 059 PCB20 059 PCB31 062 086 sulfotep 086 sulprofos 106 trichloronat 034 triphenylphosphate (TPP) 002 005 007 014 025 026 030 033 042 043 062 068 080 089 094 101 TTP 106 PRINTED GC Method: Sample Weight (g) laboratory number ≥1 - <5 029 034 038WHEN 072 094 ≥5 - <10 003 008 009 017 022 028 037 043 045 046 052 056 063 067 077 098 ≥10 - <20 001 002 004 005 006 007 011 013 014 021 023 024 025 026 027 030 033 042 044 047 048 049 050 051 057 059 061 062 064 066 068 069 070 073 080 081 082 084 085 086 087 089 090 093 095 096 102 103 105 106 ≥20 - <50 040 071 104 CONTROLLED GC Method: Extraction Solvent laboratory number Components acetone 007 021 034 037 045 056 067 070 104 acetonitrile NOT 003 005 006 008 009 013 014 022 023 024 026 027 028 029 030 033 038 042 043 044 046 047 048 049 050 051 052 057 059 061 062 063 064 066 068 069 071 072 073 080 081 082 084 085 086 090 093 094 095 102 105 106 dichloromethane 007 087 ethyl acetate 001 002 004 011 017 037 040 045 077 098 103 hexane 021 petroleum ether 025 089 Page 43 of 52 FAPAS Report 19194 GC Method: Extraction pH Adjusted laboratory number yes 006 008 022 029 030 033 034 042 048 059 061 062 064 080 087 094 101 no 001 002 003 004 005 007 009 011 013 014 017 021 023 024 025 026 027 028 037 038 040 043 044 045 046 047 049 050 051 052 056 057 063 066 067 068 069 070 071 072 073 077 081 082 084 085 086 089 093 095 098 102 103 104 105 106 GC Method: Extraction Techniques Used laboratory number macerate at room temperature 007 017 025 034 040 045 069 077 089 098 103 macerate at elevated temperature 067 QuEChERS 001 003 005 006 008 009 013 014 021 022 023 024 026 027 028 030 033 037 038 042 043 046 047 049 051 052 056 057 059 061 062 063 064 066 068 072 073 080 081 082 085 086 087 090 093 094 095 096 102 105 106 liquid-liquid partition 002 004 029 034 044 045 048 050 070 071 084 104 extraction at elevated pressure 011 084 PRINTED GC Method: Sample Clean-up Technique laboratory number GPC/HPGPC 011 034 WHEN liquid-liquid partition 034 104 solid phase extraction (SPE) 028 029 040 044 045 048 050 057 067 069 (column/cartridge) 070 071 077 084 098 105 solid phase extraction (SPE) (dispersive) 003 005 006 008 009 013 014 022 023 024 026 027 030 033 037 038 042 043 047 052 059 061 062 068 073 080 081 087 094 095 103 106 clean-up with PSA packed in glass Pasteur 066 pipettes PSA, magnesium sulfate CONTROLLED021 none 001 002 004 007 017 025 046 049 051 056 063 064 072 082 085 086 089 093 102 NOT GC Method: SPE Sorbent Type laboratory number Envicarb/GCB 029 040 047 077 098 PSA 006 008 009 022 027 028 030 037 046 049 051 052 057 059 061 062 066 068 080 081 082 086 087 095 102 103 105 NH2 045 048 Mixed Mode 005 014 021 023 024 026 033 038 042 073 Activated magnesium silicate, Florisil 072 Florisil 050 070 084 PSA + Magnesium sulphate 013 043 106 Page 44 of 52 FAPAS Report 19194 GC Method: GC Column Packing laboratory number 50% methyl 50% phenyl polysiloxane 028 051 65% methyl 35% phenyl polysiloxane 008 011 034 95% methyl 5% phenyl polysiloxane 001 002 003 004 005 007 009 013 017 021 022 023 024 025 029 030 033 037 038 040 042 043 044 045 050 052 056 057 059 061 062 063 066 068 069 070 071 072 073 077 080 081 082 085 086 087 089 094 095 098 102 103 104 105 106 Phenyl Arylene polymer virtually equivalent to 046 a (5%-Phenyl)-methylpolysiloxane(Agilent DB- 5MS) GC Method: GC Detector Type laboratory number ECD 011 034 040 045 050 067 069 070 071 081 084 MS 003 006 017 028 029 030 033 034 040 044 051 057 059 061 077 080 082 087 MS-MS 001 002 004 005 007 008 009 013 014 021 022 023 024 025 026 027 034 037 042 043 046 047 048 049 052 056 062 063 064 067 068 072 073 085 086 089 090 093 094 095 096 098 103 105 106PRINTED FPD 034 038 066 NPD 038 071 084 104 PFD 045 WHEN LC Method: Sample Weight (g) laboratory number ≥1 - <5 029 034 038 072 ≥5 - <10 003 008 009 017 022 028 037 043 045 046 052 056 063 067 077 084 098 101 ≥10 - <20 001 004 005 006 007 011 013 014 021 023 024 025 026 027 040 042 044 047 049 051 057 059 061 062 064 068 069 070 073 080 082 085 086 087 089 090 093 095 102 103 CONTROLLED105 106 ≥20 - <50 050 071 104 NOT LC Method: Extraction Solvent laboratory number Components acetic acid 017 acetone 007 104 acetonitrile 003 004 005 006 008 009 013 014 017 022 023 024 025 026 027 028 029 034 037 038 040 042 043 044 045 046 047 049 050 051 052 056 057 059 061 062 063 064 067 068 069 070 071 072 073 080 082 084 085 086 087 090 093 094 095 101 102 105 106 dichloromethane 007 ethyl acetate 001 011 077 098 methanol 021 methylbenzene (toluene) 045 Page 45 of 52 FAPAS Report 19194 LC Method: Extraction pH Adjusted laboratory number yes 006 008 009 022 029 034 040 042 047 059 061 062 064 080 087 094 095 101 no 001 003 004 005 007 011 013 014 017 021 023 024 025 026 027 028 037 038 043 044 045 046 049 050 051 052 056 057 063 066 067 068 069 070 071 072 073 077 082 084 085 086 089 093 098 102 103 104 105 106 LC Method: Extraction Techniques Used laboratory number macerate at room temperature 007 045 069 077 089 098 macerate at elevated temperature 067 QuEChERS 001 003 004 005 006 008 009 013 014 017 021 022 023 024 025 026 027 028 034 037 038 040 042 043 046 047 049 051 052 056 057 059 061 062 063 064 068 072 073 080 082 084 085 086 087 090 093 094 095 101 102 103 105 106 liquid-liquid partition 029 044 045 050 070 071 104 extraction at elevated pressure 011 LC Method: Sample Clean-up Technique laboratory number PRINTED GPC/HPGPC 011 liquid-liquid partition 034 045 082 104 solid phase extraction (SPE) 004 006 028 029 044 045 050 057 067 069 (column/cartridge) 070 071 098 105 106 solid phase extraction (SPE) (dispersive) 003 008 009WHEN 013 014 022 023 024 025 026 027 037 038 042 043 047 052 061 062 068 073 080 084 087 094 095 101 103 QuEChERS clean up 040 none 001 005 007 017 046 049 051 056 059 063 064 072 077 085 086 089 093 102 LC Method: SPE Sorbent Type laboratory number Envicarb/GCB 029 098 PSA CONTROLLED004 006 008 009 021 022 025 027 028 034 037 040 046 047 049 051 052 057 061 062 068 080 082 084 086 087 095 102 103 105 NH2 NOT 044 045 050 067 069 070 071 072 Mixed Mode 014 023 024 026 038 042 073 101 MgSO4+PSA 013 043 106 LC Method: HPLC Column Packing laboratory number C18 001 003 004 005 006 007 008 009 011 014 017 022 023 024 025 026 027 028 029 034 037 038 040 042 043 044 045 047 049 050 051 052 056 059 061 067 068 069 070 071 072 073 077 080 082 084 085 086 087 089 090 093 094 095 098 101 102 103 105 106 C8 063 104 Acquity UPLC ® HSS 046 UPLC HSS 062 Page 46 of 52 FAPAS Report 19194 LC method: Mobile Phase Components laboratory number acetonitrile 007 008 011 045 050 062 067 069 070 071 080 084 093 098 ammonium acetate 006 021 024 026 027 043 046 049 061 063 064 072 073 077 095 098 ammonium formate 005 008 013 017 025 052 080 084 101 102 105 106 formic acid 001 008 011 013 025 029 040 045 093 102 106 methanol 008 009 013 017 023 024 025 026 034 037 040 043 044 049 051 056 061 062 077 082 086 087 093 095 101 102 104 water 003 004 007 011 017 023 024 025 026 034 038 040 042 044 047 049 056 057 059 061 062 067 068 071 084 085 089 090 093 094 095 101 102 103 104 106 LC Method: Detector Type laboratory number fluorescence 044 070 104 HR-MS 013 MS-MS 001 003 004 005 006 007 008 009 011 014 017 021 022 023 024 025 026 027 028 029 034 037 038 040 042PRINTED 043 045 046 047 049 051 052 056 057 059 061 062 063 064 068 069 072 073 077 080 082 084 085 086 087 089 090 093 094 095 098 101 102 103 105 106 WHEN UV/Vis 050 067 FLD 071 Bifenthrin Method Principle laboratory number GC 001 002 003 004 005 006 007 008 009 011 013 014 017 021 022 023 024 025 026 027 CONTROLLED029 033 034 037 038 040 042 043 045 046 047 048 050 059 062 063 064 067 068 069 070 071 072 073 077 080 081 085 086 093 NOT 094 095 096 098 103 105 106 107 LC 028 049 051 052 058 061 079 082 084 087 102 Identification by Mass Spectrometry laboratory number yes 001 002 003 004 005 006 007 008 009 013 014 017 021 022 023 024 025 026 027 028 029 033 034 037 038 040 042 043 045 046 047 048 049 050 051 052 058 059 061 062 063 064 067 068 069 070 071 072 073 077 079 080 082 084 085 086 087 093 094 095 096 098 102 103 105 106 107 no 011 081 Page 47 of 52 FAPAS Report 19194 Dimethoate Method Principle laboratory number GC 002 004 006 011 017 023 033 034 038 045 047 048 050 067 069 070 071 103 LC 001 003 005 007 009 013 014 021 022 024 025 026 027 028 029 037 040 042 043 046 049 051 052 056 058 059 061 062 063 064 068 072 073 077 079 080 082 084 085 086 089 093 094 095 098 102 106 Identification by Mass Spectrometry laboratory number yes 001 002 003 004 005 006 007 009 013 014 017 021 022 023 024 025 026 027 028 029 033 034 037 038 040 042 043 045 046 047 048 049 050 051 052 056 058 059 061 062 063 064 067 068 069 070 071 072 073 077 079 080 082 084 085 086 089 093 094 095 098 102 103 106 no 011 PRINTED Flucythrinate Method Principle laboratory number GC 001 003 005WHEN 006 007 013 014 017 021 022 023 024 026 027 029 033 034 038 040 042 043 045 046 049 050 052 059 062 063 064 068 072 073 077 080 086 089 093 094 095 098 103 106 LC 028 051 087 Identification by Mass Spectrometry laboratory number yes 001 003 005 006 007 013 014 017 021 022 CONTROLLED023 024 026 027 028 029 033 034 038 040 042 043 045 046 049 050 051 052 059 062 063 064 068 072 073 077 080 086 087 089 NOT 093 094 095 098 106 no 103 Metalaxyl & Metalaxyl-M (Sum) Method Principle laboratory number GC 001 002 004 005 008 009 017 022 023 034 037 038 048 050 062 067 069 070 071 077 080 086 094 098 103 105 106 LC 003 007 011 013 014 021 025 026 027 028 029 040 042 043 045 046 047 049 051 052 058 059 061 063 068 079 082 085 089 095 102 Page 48 of 52 FAPAS Report 19194 Identification by Mass Spectrometry laboratory number yes 001 002 003 004 005 007 008 009 011 013 014 017 021 022 023 025 026 027 028 029 034 037 038 040 042 043 045 046 047 048 049 050 051 052 058 059 061 062 063 067 068 069 070 071 077 079 080 082 085 086 089 094 095 098 102 103 105 106 Methiocarb Sulfone Method Principle laboratory number LC 001 003 005 007 034 049 059 061 062 068 080 085 086 089 095 098 102 Identification by Mass Spectrometry laboratory number yes 001 003 005 007 034 049 059 061 062 068 080 085 086 089 095 098 102 Phenthoate PRINTED Method Principle laboratory number GC 003 004 005 006 013 014 017 022 023 024 025 026 027 033 034 037 040 042 043 046 048 050 059WHEN 062 064 068 073 077 080 086 089 093 094 095 098 LC 007 021 028 047 049 051 058 061 063 079 082 084 085 Identification by Mass Spectrometry laboratory number yes 003 004 005 006 007 013 014 017 021 022 023 024 025 026 027 028 033 034 037 040 042 043 046 047 048 049 050 051 058 059 CONTROLLED061 062 063 064 068 077 079 080 082 084 085 086 089 093 094 095 098 NOT Profenofos Method Principle laboratory number GC 001 005 006 007 011 013 017 022 023 025 033 034 038 040 045 048 050 062 068 073 077 080 086 093 094 095 098 104 105 106 LC 003 004 008 014 021 024 026 027 028 029 037 042 043 046 047 049 051 052 058 059 061 063 064 072 079 082 084 089 102 Page 49 of 52 FAPAS Report 19194 Identification by Mass Spectrometry laboratory number yes 001 003 004 005 006 007 008 013 014 017 021 022 023 024 025 026 027 028 029 033 034 037 038 040 042 043 045 046 047 048 049 050 051 052 058 059 061 062 063 064 068 072 073 077 079 080 082 084 086 089 093 094 095 098 102 105 no 011 104 Propoxur Method Principle laboratory number GC 007 022 034 038 048 062 086 094 095 098 LC 001 003 004 005 006 008 011 013 014 017 021 024 025 026 027 029 037 042 043 045 046 047 049 051 059 063 064 067 068 069 070 071 073 077 079 080 082 085 089 093 102 103 106 Identification by Mass Spectrometry laboratory number yes 001 003 004 005 006PRINTED 007 008 011 013 014 017 021 022 024 025 026 027 029 034 037 038 042 043 045 046 047 048 049 051 059 062 063 064 067 068 069 070 071 077 079 080 082 085 086 089 093 094 095 098 102 106 WHEN no 103 Pyriproxyfen Method Principle laboratory number GC 001 002 004 005 006 007 014 021 022 024 026 027 029 033 034 037 038 042 043 046 CONTROLLED047 048 052 064 073 080 093 094 098 103 106 LC 003 008 009 013 028 040 049 051 056 058 NOT 059 061 062 063 068 077 079 082 085 086 087 089 095 102 Identification by Mass Spectrometry laboratory number yes 001 002 003 004 005 006 007 008 009 013 014 021 022 024 026 027 028 029 033 034 037 038 040 042 043 046 047 048 049 051 052 056 058 059 061 062 063 064 068 077 079 080 082 085 086 087 089 093 094 095 098 102 103 106 Page 50 of 52 FAPAS Report 19194 Tetradifon Method Principle laboratory number GC 001 003 004 005 006 007 008 009 011 013 014 017 021 022 024 025 026 027 028 029 033 034 037 038 040 042 043 046 047 048 049 050 051 052 058 059 061 062 063 064 068 073 077 079 080 082 086 089 093 094 095 096 098 102 103 106 Identification by Mass Spectrometry laboratory number yes 001 003 004 005 006 007 008 009 013 014 017 021 022 024 025 026 027 028 029 033 034 037 038 040 042 043 046 047 048 049 050 051 052 058 059 061 062 063 064 068 077 079 080 082 086 089 093 094 095 096 098 102 103 106 no 011 PRINTED WHEN CONTROLLED NOT Page 51 of 52 FAPAS Report 19194 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 PRINTED The Protocols [3, 4] set out how FAPAS® is organised. Copies can be downloaded from our website. WHEN 3. CONTACT DETAILS This report was prepared and authorised on behalf of FAPAS by Michael Knaggs (Round Coordinator). Participants with any comments or concerns about this proficiency test should contact: FAPAS CONTROLLEDFera Science Ltd (Fera) Sand Hutton York NOT YO41 1LZ UK Tel: +44 (0)1904 462100 Fax: +44 (0)1904 500440 [email protected] www.fapas.com Page 52 of 52