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GB 23200.85-2016: Food safety national standard -- Determination of various pyrethroid pesticide residues in milk and dairy products -- Gas chromatography-mass spectrometry
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Standard similar to GB 23200.85-2016

GB/T 38211   GB/T 18418   GB/T 18419   GB 23200.78   GB 23200.79   GB 23200.77   

Basic data

Standard ID GB 23200.85-2016 (GB23200.85-2016)
Description (Translated English) Food safety national standard -- Determination of various pyrethroid pesticide residues in milk and dairy products -- Gas chromatography-mass spectrometry
Sector / Industry National Standard
Classification of Chinese Standard G25
Word Count Estimation 18,122
Date of Issue 2016-12-18
Date of Implementation 2017-06-18
Older Standard (superseded by this standard) SN/T 2912-2011
Regulation (derived from) State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16 of 2016
Issuing agency(ies) National Health and Family Planning Commission of the People's Republic of China, State Food and Drug Administration

GB 23200.85-2016: Food safety national standard -- Determination of various pyrethroid pesticide residues in milk and dairy products -- Gas chromatography-mass spectrometry


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Food safety national standard - Determination of various pyrethroid pesticide residues in milk and dairy products - Gas chromatography - mass spectrometry National Standards of People's Republic of China GB Instead of SN/T 2912-2011 National standards for food safety Milk and dairy products in a variety of pyrethroids Determination of pesticide residues Gas chromatography - mass spectrometry National food safety standards- Determination of multiple pyrethroid pesticide residues in dairy products Gas chromatography - mass spectrometry 2016-12-18 Release.2017-06-18 Implementation National Health and Family Planning Commission of the People 's Republic of China Issued by the Ministry of Agriculture of the People 's Republic of China State Administration of Food and Drug Administration

Foreword

This standard replaces SN/T 2912-2011 "Method for the determination of various pyrethroid pesticide residues in imported and exported milk and dairy products - Gas phase Chromatography-mass spectrometry ". Compared with SN/T 2912-2011, the main changes are as follows. - Standard text format is modified to national standard text format for food safety; - "Name and scope of the import and export of milk and dairy products" to "milk and dairy products"; - increase the "other food reference implementation" in the standard range. This standard replaced the previous version of the standard release. -SN/T 2912-2011. National standards for food safety Determination of various pyrethroid pesticide residues in milk and dairy products Gas chromatography - mass spectrometry

1 Scope

This standard specifies the import and export of milk and dairy products in 2,6 - diisopropylnaphthalene, tefluthrin, biological allyl permethrin, Esters, bifenthrin, fenpropathrin, cyhalothrin, fenpropathrin, permethrin, cypermethrin, cypermethrin, fenvalerate, ether Pyrethrins, fenvalerate, deltamethrin, deltamethrin and other 17 multi-component pesticide residues by gas chromatography-mass spectrometry. This standard applies to liquid milk, milk powder, condensed milk, milk fat, cheese, ice cream and whey powder 2,6 - diisopropyl naphthalene, Pyrethroid, fenpropathrin, permethrin, fenpropathrin, fenpropathrin, fenpropathrin, fenpropathrin Cypermethrin, cypermethrin, fenvalerate, permethrin, fenvalerate, fenpropathrin, deltamethrin and other pesticide residues Testing and confirmation, other food can refer to the implementation.

2 normative reference documents

The following documents are indispensable for the application of this document. For dated references, only the dated edition applies to this article Pieces. For undated references, the latest edition (including all modifications) applies to this document. GB 2763 National Standard for Food Safety - Maximum Residue Limit of Pesticides in Foodstuffs GB/T 6682 Analytical laboratory water specifications and test methods

3 principle

The samples were extracted with sodium chloride and acetonitrile to separate the acetonitrile layer. The samples were extracted with C18 solid phase extraction column and florisil silica solid phase extraction Column purification, elution concentration dissolved dissolved volume, the gas chromatography - mass spectrometer detection and confirmation, external standard quantitative.

4 reagents and materials

Unless otherwise specified, all reagents are of analytical grade and water is in accordance with the primary water specified in GB/T 6682. 4.1 Reagents 4.1.1 acetonitrile (C2H3N, CAS No. 75-05-8). residual grade. 4.1.2 n-Hexane (C6H14, CAS No. 110-54-3). Residue level. 4.1.3 Ethyl acetate (C4H8O2, CAS No. 141-78-6). Residue level. 4.1.4 Sodium chloride (NaCl, CAS No. 7647-14-5). 4.2 solution preparation 4.2.1 N-Hexane-Ethyl Acetate (9 2, VV). Take 90 mL of n-hexane and 20 mL of ethyl acetate and mix well. 4.3 standards 4.3.1 2,6-diisopropylnaphthalene and other pesticide standards. purity ≥ 98%, CAS number see Appendix A. 4.4 standard solution preparation 4.4.1 2,6-diisopropylnaphthalene and other 17 kinds of pesticide standard stock solution. accurately weighed an appropriate amount of 2,6 - diisopropyl naphthalene and other 17 kinds of agriculture Drug standard, with n-hexane prepared into a concentration of 100 μg/mL standard stock solution. The solution was stored in a refrigerator at 0 ° C to 4 ° C. 4.4.2 2,6-diisopropyl naphthalene and other 17 kinds of pesticide standard working solution. If necessary, with 2,6 - diisopropyl naphthalene and other 17 kinds of pesticides Blank sample prepared into the standard concentration of the working solution, the solution is now used. 4.5 Materials 4.5.1 C18 solid phase extraction column. C18, 500 mg, 3 mL. 4.5.2 Fluoresa Silica Solid Phase Extraction Column. Florisil, 500 mg, 3 mL.

5 instruments and equipment

5.1 Gas Chromatography-Mass Spectrometer. Equipped with an electron impact source (EI). 5.2 Analysis of the balance. the amount of 0.01 g. 5.3 Analysis of balance. sense of 0.0001 g. 5.4 homogenizer. speed of not less than 10000 r/min. 5.5 Centrifuge. speed of not less than 4000 r/min. 5.6 nitrogen blowing instrument. 5.7 vortex mixer.

6 Preparation and storage of samples

6.1 Preparation of the sample Take the sample about 500 g, the sampling site according to GB 2763 Appendix A implementation, crushed with a grinder, mix, into a clean container, sealed, standard Mark. 6.2 Sample storage The samples were stored at 0 ° C to 4 ° C. During the operation of the sample preparation, the sample should be protected from contamination or changes in the content of the residue.

7 Analysis steps

7.1 Extraction Accurately weigh liquid milk, ice cream sample 2.0 g (accurate to 0.01 g), add 0.5 g sodium chloride, 10.0 mL acetonitrile at 10,000 r/min Homogenate extraction for 60 s, then centrifuged at 4000 r/min for 5 min, accurately remove 5.0 mL of acetonitrile, at 40 ° C nitrogen blowing to about 1 mL, to be purified. Accurately weigh cheese, milk powder, whey powder, condensed milk, milk fat sample 2.0 g (accurate to 0.01 g), add 0.5 g sodium chloride, 5 mL Water, 10.0 mL of acetonitrile, homogenized at 10,000 r/min for 60 s, centrifuged at 4000 r/min for 5 min, accurately removed 5.0 mL of acetonitrile, Boil at about 40 ° C to about 1 mL to be purified. The 7.2 Purification 7.2.1 C18 solid phase extraction purification The sample concentrate obtained in 7.1 was poured into a C18 solid phase extraction column previously eluted with 5 mL of acetonitrile and eluted with 4 mL of acetonitrile to collect the eluate, At 40 ℃ nitrogen blowing to near dry, with 0.5 mL n-hexane vortex mixed dissolved residue, stand-by. 7.2.2 Fluoresa Silica Solid Phase Extraction Purification The eluate obtained in 7.2.1 was poured into a preflora deuterated preflora with 5 mL of n-hexane-ethyl acetate and extracted with 5.0 mL N-hexane-ethyl acetate, the eluate was collected, the mixture was blown to near dry at 40 ° C, and the residue was dissolved in 0.5 mL of n-hexane vortex to dissolve the residue Determination of the instrument. 7.3 Determination 7.3.1 Gas Chromatography - Mass Spectrometry Reference Conditions A) Column. TR-5MS quartz capillary column, 30 m × 0.25 mm (inner diameter) × 0.25 μm, or equivalent performance; B) Column temperature. 50 ° C 20 ° C/min.200 ° C (1 min) 5 ° C/min 280 ° C (10 min); C) Inlet temperature. 250 ° C; D) chromatographic - mass spectrometer interface temperature. 280 ° C; E) ionization mode. EI; F) ion source temperature. 250 ° C; G) Filament current. 25 μA; G) Carrier gas. helium, purity greater than or equal 99.999%, flow rate 1 mL/min; H) Injection method. no shunt, 0.75 min after the opening of the diversion valve; I) Injection volume. 1 μL; J) Measurement method. Select ion monitoring; K) Select the monitoring ion (m/z). Select a quantitative ion for each pesticide, 3 qualitative ions, retention time for each pesticide, Quantitative ions, qualitative ions and quantitative ions and qualitative ion abundance ratio see Appendix B; L) solvent delay. 8.5 min. 7.3.2 Determination and confirmation of chromatography According to the sample content of the sample to be measured, the selected concentration of similar standard working solution, the standard working solution and the sample solution to be 2,6- Diisopropylnaphthalene and other 17 kinds of pesticide response value should be within the linear range of instrument detection. Standard working solution and sample solution volume into the sample set. Standard solution and sample solution are determined according to the conditions specified in 7.3.1, if the sample solution with the standard solution of the same retention time there are peaks, It is confirmed. It was confirmed that the retention time of the chromatographic peak of the tested substance was consistent with that of the reference substance, and in the sample spectrum after subtracting the background, The selected ions are present, and the abundance of the selected ions is consistent with the relative abundance of the reference substance associated with the reference substance, or the similarity is Poor (see Table 1), confirmed the sample can be judged as positive detection. 2,6-diisopropylnaphthalene and other 17 kinds of pesticide reference material gas chromatography-mass spectrometry total ion flow diagram see Appendix C in Figure C.1. Table 1 Maximum allowable error for relative ion abundance using gas chromatography-mass spectrometry 7.4 blank experiment In addition to the sample, according to the above determination steps.

8 results are calculated and expressed

Use the chromatographic data processor or (1) to calculate the amount of 2,6 pesticide residues such as 2,6-diisopropylnaphthalene in the sample.   MA VCA S (1) Where. X - Samples of 2,6 - diisopropylnaphthalene and other 17 pesticide residues in milligrams per kilogram, mg/kg; A - peak area (or peak height) of 17 pesticides such as 2,6 - diisopropylnaphthalene in sample solution; C - standard working solution of 2,6 - diisopropylnaphthalene and other 17 kinds of pesticide concentration, the unit is microgram per milliliter, g/mL; V - the final volume of the sample solution, in milliliters, mL; As - the peak area (or peak height) of 17 pesticides such as 2,6 - diisopropylnaphthalene in standard working solution; M - the final sample of the sample quality, in grams, g. Note. The result of the calculation shall be deducted from the blank value. The result of the measurement shall be expressed as the arithmetic mean of the parallel measurement, and two valid digits shall be retained.

9 precision

9.1 The ratio of the absolute difference between the two independent determinations obtained under reproducibility and its arithmetic mean (percentage) shall be in accordance with Appendix E requirements. 9.2 The ratio of the absolute difference between the two independent determinations obtained under reproducibility and its arithmetic mean (percentage) shall be in accordance with Appendix F requirements. 10% limit and recovery rate 10.1 Quantitation limits The quantitative limits for pyrethroids of this method are given in Appendix D. 10.2 Recovery rate When the levels were 0.005 mg/kg, 0.01 mg/kg, 0.02 mg/kg, 0.2 mg/kg, 17 pesticides were added in different matrices The recoveries are given in Appendix D. Relative abundance (base) 50% 20% to 50% 10% to 20% ≤10% Allowable relative deviation ± 20% ± 25% ± 30% ± 50%

Appendix A

(Informative) 2,6-diisopropylnaphthalene, etc. 17 Pyrethroid pesticide type table Table A.1 Table of 17 kinds of pyrethroid pesticide types such as 2,6-diisopropylnaphthalene No. Name of pesticide English name CAS No. Chemical formula 1 2,6-diisopropylnaphthalene 2,6-diisopropylnaphtalene 24157-81-1 C10H6 (CH (CH3) 2) 2 2 tefluthrin 79538-32-2 C17H14ClF7O2 3 Bioabethrin Bioallethrin 584-79-2 C19H26O3 4 Methoprene 40596-69-8 C19H34O3 5 benzathrin Resmethrin 10453-86-8 C22H26O3 6 Bifenthrin Bifenthrin 82657-04-3 C23H22ClF3O2 7 Fenpropathrin 64257-84-7 C22H23NO3 8 Cyhalothrin 68085-85-8 C23H19ClF3NO3 9 Fenpropathrin Acrinathrin 101007-06-1 C26H21F6NO5 Permethrin (Ⅰ) Permethrin (Ⅰ) 52645-53-1 C21H20Cl2O3 Permethrin (II) Cyfluthrin (Ⅰ) Cyfluthrin (Ⅰ) 68359-37-5 C22H18Cl2FNO3 Cyfluthrin (Ⅱ) Cyfluthrin (Ⅱ) Cyfluthrin (Ⅲ) Cyfluthrin (Ⅲ) Cyfluthrin (Ⅳ) Cyfluthrin (Ⅳ) Cypermethrin (Ⅰ) Cypermethrin (Ⅰ) 52315-07-8 C22H19Cl2NO3 Cypermethrin (Ⅱ) Cypermethrin (Ⅱ) Cypermethrin (Ⅲ) Cypermethrin (Ⅲ) Cypermethrin (Ⅳ) Cypermethrin (Ⅳ) Fenvalerate (Ⅰ) Flucythrinate (I) 70124-77-5 C26H23F2NO4 Fenvalerate (Ⅱ) Flucythrinate (Ⅱ) 14 etheroctate Etofenprox 80844-07-1 C25H28O3 Fenvalerate (Ⅰ) Fenvalerate (Ⅰ) 51630-58-1 C25H22ClNO3 Fenvalerate (Ⅱ) Fenvalerate (Ⅱ) Fenpropathrin (Ⅰ) tau-Fluvalinate (I) 102851-06-9 C26H22ClF3N2O3 (6) tau-Fluvalinate (Ⅱ) 17 Deltamethrin 52918-63-5 C22H19Br2NO3

Appendix B

(Informative) Buprenorphine and other 17 kinds of pyrethroid pesticide quantitative and qualitative selection of ions Table B.1 17 kinds of pyrethroids and other pseudo-pyrethroid pesticide quantitative and qualitative selection of ions Peak Shun Serial number Pesticide name retention time Characteristic fragment ion Quantitative qualitative abundance ratio The first paragraph 8.5-12.0 1 2,6-diisopropylnaphthalene 9.97 197 155,167,212 100. 34. 8. 45 2 Chlortetracycline 10.55 177 142,161,197 100 ︰ 9 ︰ 5.24 The second paragraph 12.0-18.0 3 Bioprostol 14.03 123 107,136,168 100. 19. 28. 6 4 insecticidal ester 14.22 73 111,153,191 100. 32 ︰ 19. 14 The third paragraph 18.0-21.2 5 benzathrin 19.14 171 123,143,338 61. 100. 47. 3 6 Bifenthrin 19.83 181 152,165,166 100 ︰ 2 ︰ 26 ︰ 30 7 fenpropathrin 20.33 265 97,181,349 38. 100. 96. 6 Fourth paragraph 21.2-22.5 8 cyhalothrin 21.74 181 197,208,449 100. 34. 8. 45 9 Fenvalerate 21.90 181 152,247,289 100. 9 ︰ 14.27 Fifth paragraph 22.5-24.0 10 permethrin (Ⅰ) 23.42 183 163,184,255 100. 18. 14. 2 11 permethrin (Ⅱ) 23.67 183 163,184,255 100 ︰ 25 ︰ 16 ︰ 2 Paragraph 6 24.0-26.2 12 cyfluthrin (Ⅰ) 24.43 163.199,206,226 100. 59. 86. 47 13 cyfluthrin (II) 24.63 163.199,206,226 100. 44. 61. 34 14 cyfluthrin (III) 24.74 163.199,206,226 100. 46. 80. 41 15 cyfluthrin (IV) 24.84 163.199,206,226 100. 41. 54. 33 16 cypermethrin (Ⅰ) 25.12 163 91,152,165 100. 30. 16. 67 17 cypermethrin (II) 25.36 163 91,152,165 100. 39. 26. 58 18 cypermethrin (III) 25.46 163 91,152,165 100 ︰ 26. 14. 66 19 cypermethrin (IV) 25.57 163 91,152,165 100. 32. 22. 70 20 Fenvalerate (Ⅰ) 25.42.199 157,225,451 100. 73. 32. 15 21 Fenvalerate (II) 25.87.199 157,225,451 100. 68. 29. 11 22 Etodinate 25.85 163 135,183,376 100 ︰ 14. 4 ︰ 3 Paragraph 7 26.2-28.2 23 fenvalerate (Ⅰ) 27.28 167 181,225,419 100 ︰ 56. 73. 22 24 fenvalerate (Ⅱ) 27.86 167 181,225,419 100. 34. 8. 45 25 Fluorocarbamate (Ⅰ) 27.37 250 181,252,502 100 ︰ 21. 35. 5 26 Fluorocarbamate (Ⅱ) 27.59 250 181,252,502 100 ︰ 21. 34. 6 Paragraph 8 28.2-34.0 27 deltamethrin 29.62 181 172,209,253 100. 38. 19. 68

Appendix C

(Informative) Benzodiazepines and other 17 kinds of pyrethroid pesticide total ion mobility gas chromatography - mass spectrometry Figure C.1 17 kinds of pyrethroids and other pyrethroids pesticide total ion mobility gas chromatography-mass spectrometry 1 - 2, 6 - diisopropylnaphthalene 2 - difenoconazole 3 - bio-allyl ester 4 - insect insect ester 5 - benzathrin 6 - bifenthrin 7 - fenpropathrin 8 - cyhalothrin 9 - Fentanyl ester 10 - permethrin (I) 11 - permethrin (II) 12 - cyfluthrin (I) 13 - cyfluthrin (II) 14 - cyfluthrin (III) 15 - cypermethrin (IV) 16 - cypermethrin (Ⅰ) 17 - cypermethrin (Ⅱ) 18 - cypermethrin (III) 19 - cypermethrin (IV) 20 - fenvalerate (I) 21 - fenvalerate (II) 22 - permethrin 23 - fenvalerate (Ⅰ) 24 - fenvalerate (II) 25 - fenpropathrin (Ⅰ) 26 - fenpropathrin (II) 27 - deltamethrin

Appendix D

(Informative) Quantitative limits and recovery rates of 17 pesticides in different substrates Table D.1 Quantitative limits and recovery rates for 17 pesticides in different matrices Pesticide name Sample type Quantification limit mg/kg Add level mg/kg Average recovery range% 2.6 - diisopropylnaphthalene Milk 0.005 0.005 82.3 ~ 108.1 0.01 84.2 to 110.3 0.2 85.3 ~ 109.4 Ice cream 0.005 0.005 73.5 to 98.2 0.01 91 to 103.3 0.2 84.6 to 112.3 Milk powder 0.005 0.005 78.5 to 106.3 0.01 81.5 to 104.2 0.2 93.2 to 110.0 Cheese 0.005 0.005 80.1 to 101.5 0.01 76.1 to 106.3 0.2 94.5 to 103.2 Heptachlor Milk 0.005 0.005 91.2 ~ 106.7 0.01 84.2 to 113.2 0.2 90.5 to 106.7 Ice cream 0.005 0.005 85.5 to 104.2 0.01 90.5 to 113.4 0.2 75.6 ~ 106.4 Milk powder 0.005 0.005 87.5 to 113.1 0.01 79 to 105.4 0.2 77.8 to 110.1 Cheese 0.005 0.005 84.5 to 105.6 0.01 86.6 ~ 105.4 0.2 82.3 to 106.3 Bio-Almond Butter Milk 0.01 0.01 89.1 to 113.2 0.02 81.3 ~ 113.6 0.2 86.4 to 111.3 Ice cream 0.01 0.01 87.5 to 96.2 0.02 79.3 ~ 106.2 0.2 94.4 to 99.5 Milk powder 0.01 0.01 67.5 to 96.1 0.02 89.3 to 95.6 0.2 76.2 to 106.2 Cheese 0.01 0.01 86.0 to 110.6 0.02 76.0 to 109.1 0.2 85.3 ~ 112.6 0.2 92.2 to 106.4 Asteroid Milk 0.01 0.01 79.6 ~ 106.5 0.02 80.6 ~ 103.2 0.2 89.3 to 100.9 Ice cream 0.01 0.01 66.0 to 91.2 0.02 89.0 to 103.4 0.2 81.2 ~ 97.6 Milk powder 0.01 0.01 72.0 to 108.2 0.02 82.5 to 98.6 0.2 85.3 ~ 99.3 Cheese 0.01 0.01 85.5 to 105.4 0.02 84.2 to 112.3 0.2 83.1 to 102.3 Benzathrin Milk 0.01 0.01 80 to 116.7 0.02 77.5 ~ 104.2 0.2 80.0 to 105.0 Ice cream 0.01 0.01 89.0 to 109.3 0.02 87.0 ~ 98.2 0.2 94.7 to 120.2 Milk powder 0.01 0.01 91.0 to 105.8 0.02 81.7 to 96.8 0.2 78.3 ~ 98.1 Cheese 0.01 0.01 78.5 to 89.5 0.02 90.2 to 103.5 0.2 77.0 to 92.5 Bifenthrin Milk 0.005 0.005 73.5 to 106.2 0.01 85.4 to 112.2 0.2 79.2 to 103.8 Ice cream 0.005 0.005 89.0 to 92.1 0.01 95.5 to 115.2 0.2 82.5 to 105.3 Milk powder 0.005 0.005 85.4 to 105.3 0.01 83.2 to 105.2 0.2 90.2 to 112.1 Cheese 0.005 0.005 87.5 to 105.6 0.01 82.2 to 105.4 0.2 85.4 ~ 98.0 Fenpropathrin Milk 0.01 0.01 86.5 to 98.5 0.02 85.7 ~ 114.8 0.2 85.4 to 100.8 Ice cream 0.01 0.01 85.0 to 104.3 0.02 76.5 to 110.2 0.2 82.1 to 106.4 Milk powder 0.01 0.01 85.0 to 116.2 0.02 88.7 to 100.9 0.2 88.5 to 104.2 Cheese 0.01 0.01 73.0 to 113.5 0.02 87.5 ~ 106.3 0.2 86.0 to 114.3 Cyhalothrin Milk 0.01 0.01 90.5 to 110.4 0.02 81.2 ~ 101.8 0.2 91.0 to 106.7 Ice cream 0.01 0.01 88.5 to 99.1 0.02 85.2 ~ 105.2 0.2 85.1 to 110.6 Milk powder 0.01 0.01 75.0 to 94.1 0.02 85.0 to 106.2 0.2 86.1 to 105.2 Cheese 0.01 0.01 90.0 to 110.8 0.02 89.5 to 109.2 0.2 78.9 to 106.0 Fenpropathrin Milk 0.01 0.01 73.5 to 110.0 0.02 90.5 to 96.2 0.2 84.0 to 89.2 Ice cream 0.01 0.01 68.5 to 90.0 0.02 82.0 to 105.7 0.2 92.5 to 110.8 Milk powder 0.01 0.01 75.5 to 106.1 0.02 82.5 to 105.5 0.2 85.0 to 105.3 Cheese 0.01 0.01 90.8 to 110.1 0.02 91.0 to 103.3 0.2 82.5 to 106.4 Permethrin (I, II) Milk 0.01 0.01 78.5 to 91.2 0.02 92.5 to 105 0.2 84.0 to 97.3 Ice cream 0.01 0.01 73.0 to 93.7 0.02 71.5 to 95.0 0.2 89.5 to 102.3 Milk powder 0.01 0.01 80.5 to 110.8 0.02 85.1 to 112.5 0.2 95.7 to 109.0 Cheese 0.01 0.01 89.5 to 111.5 0.02 85.0 to 106.7 0.2 86.1 to 95.4 Cyfluthrin (I, II, III, IV) Milk 0.02 0.02 84.0 to 95.3 0.04 85.4 to 95.7 0.2 78.4 to 92.2 Ice cream 0.02 0.02 84.8 ~ 115.2 0.04 86.3 to 112.8 0.2 86.1 to 105.3 Milk powder 0.02 0.02 78.6 to 95.0 0.04 88.6 to 114.3 0.2 85.2 ~ 106.3 Cheese 0.02 0.02 87.5 to 112.3 0.04 85.0 ~ 98.5 0.2 83.0 to 92.3 Cypermethrin (I, II, III, IV) Milk 0.02 0.02 76.5 to 94.7 0.04 76.2 to 102.1 0.2 82.5 to 110.3 Ice cream 0.02 0.02 88.5 to 104.7 0.04 89.5 to 108.1 0.2 85.0 to 118.2 Milk powder 0.02 0.02 85.5 to 103.5 0.04 85.2 to 110.4 0.2 85.2 ~ 106.3 Cheese 0.02 0.02 90.5 to 102.3 0.04 82.7 to 110.2 0.2 75.0 to 88.6 Fenvalerate (I, II) Milk 0.01 0.01 90.7 to 112.4 0.02 87.0 ~ 98.1 0.2 80.1 to 94.0 Ice cream 0.01 0.01 83.5 to 110.5 0.02 88.5 to 105.3 0.2 83.7 to 110.8 Milk powder 0.01 0.01 75.5 to 89.4 0.02 82.5 to 98.3 0.2 76.2 to 108.3 Cheese 0.01 0.01 90.5 to 110.6 0.02 85.2 to 102.3 0.2 95.3 to 105.2 Ether pyrethrins Milk 0.01 0.01 63.5 to 90.2 0.02 93.1 to 98.0 0.2 85.4 to 106.3 Ice cream 0.01 0.01 78.5 to 102.0 0.02 71.6 ~ 100.5 0.2 86.0 to 106.2 Milk powder 0.01 0.01 80.5 to 93.2 0.02 96.0 to 118.1 0.2 95.3 to 112.8 Cheese 0.01 0.01 89.5 to 103.5 0.02 91.5 to 94.2 0.2 92.5 to 105.8 Fenvalerate (I, II) Milk 0.01 0.01 84.0 to 96.5 0.02 88.7 to 100.8 0.2 78.6 ~ 101.2 Ice cream 0.01 0.01 76.5 to 105.4 0.02 86.5 to 95.3 0.2 78.4 to 110.5 Milk powder 0.01 0.01 86.0 to 105.4 0.02 82.5 to 103.2 0.2 79.5 to 98.1 Cheese 0.01 0.01 89.0 to 98.4 0.02 88.5 to 110.5 0.2 94.8 to 103.4 Fenpropathrin (I, II) Milk 0.01 0.01 73.0 to 89.4 0.02 79.7 to 105.2 0.2 79.5 to 95.1 Ice cream 0.01 0.01 83.0 to 104.8 0.02 78.5 to 89.6 0.2 80.5 to 95.1 Milk powder 0.01 0.01 85.5 to 97.4 0.02 81.2 ~ 106.8 0.2 95.1 to 110.6 Cheese 0.01 0.01 74.5 to 96.8 0.02 90.2 to 109.3 0.2 84.2 to 89.4 Deltamethrin Milk 0.01 0.01 84.0 to 96.6 0.02 95.0 to 110.3 0.2 78.9 to 100.7 Ice cream 0.01 0.01 78.0 to 92.3 0.02 71.5 to 90.1 0.2 90.3 to 96.4 Milk powder 0.01 0.01 88.5 to 106.4 0.02 90.5 to 106.4 0.2 82.6 to 96.2 Cheese 0.01 0.01 79.5 to 102.4 0.02 90.5 to 120.5 0.2 86.3 to 102.1

Appendix E

(Normative appendix) Laboratory repeatability requirements Table E.1 Laboratory repeatability requirements Measured component content Mg/kg Precision 0.001 36 > 0.01 > 1 14

Appendix F

(Normative appendix) Inter-laboratory reproducibility requirements Table F.1 Inter-laboratory reproducibility requirements Measured component content Mg/kg Precision 0.001 54 > 0.01 > 1 19

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