OMB First to Final Action Recommendation Checklist 11-12-18

3/9/2017

SINGLE LABORATORY VALIDATION 4. In your experience with the method, do you have data demonstrating linearity, accuracy, repeatability, LOD/LOQ? Lab Organization Question 4 Lab-1 Asia pacific technicalcenter, the coca-cola company N Lab-2 Inspection & QuarantineTechnique Centre of Fujian Entry-exit Inspection and Quarantine Bureau Y Lab-3 HuangshanTea QualityAnd Safety Research Center of Huangshan Entry-Exit Inspection & QuarantineBureau Y Lab-4 Food inspection central of CIQ ShenZhen Y Lab-5 QinhuangdaoEntry-exit Inspection and QuarantineBureau Y Lab-6 Japan grain inspection association central research laboratory N Lab-8 Tea research institute ChineseAcademy of agricultural sciences Y Lab-9 EURL-FV, University of Almería N Lab-10 Dalianentry-exit inspection and quarantine bureau Y Lab-11 ICAS Testing Center (Shanghai) Y Lab-12 BENGBUCenter for Disease Control and prevention N Lab-13 Shanghai BinoTesting Service Co., Ltd Y Lab-14 DENO TESTING Service (Shanghai) Y Lab-15 Tea Research Institute, Chinese Academy of Agricultural Sciences Y  Yes: 10 Labs No: 4 Labs  Lab -2: The data obtained using AOAC Official Method 2014.09 to demonstrate the linearity, accuracy and repeatability attached in Appendix (see Table below).  Lab-13: Recoveries for 41 pesticides in green tea and black tea determined by GC-MS (see Table below).

Lab-2:

Determination results of multi-residues in tea by GC-MS

Green tea

Retention time/min

Spike levels (μg/kg)

Calibration curve

Recovery/%

Pesticides

No.

RSD/ %

R 2

Slope Intercept

No.1 No.2 No.3 No.4 No.5 AVE

IS heptachlor 1 trifluralin 2 tefluthrin 3 pyrimethanil 4 propyzamide 5 pirimicarb 6 dimethenamid 7 tolclofos-methyl 8 fenchlorphos 9 pirimiphos-methyl 13 procymidone 14 picoxystrobin 15 chlorfenapyr 16 quinoxyfen 17 benalaxyl 18 bifenthrin 19 diflufenican 20 bromopropylate 10 2,4-DDE 11 bromophos-ethyl 12 4,4-DDE

18.787

9.940

0.9997 0.9982 0.9977 0.9984 0.9981 0.9963 0.9971 0.9965 0.9977 0.9977 0.9973 0.9978 0.9975 0.9979 0.9976 0.9980 0.9976 0.9978 0.9982 0.9978

1.0858 1.8509 2.6666 0.9642 1.5951 0.4662 1.3229 1.2458 0.5001 4.0213 0.3133 3.1875 0.3892 0.7657 0.4209 1.1099 1.5987 3.0963 2.0066 1.8023

-0.0155 0.3906 0.5547 0.2457 0.4131 0.1679 0.3183 0.3545 0.1095 0.7936 0.0691 0.6239 0.0890 0.1335 0.0998 0.2239 0.3213 0.8757 0.3759 0.3328

200 100 100 100 100 100 200 100 400 100 400 100 200 800 100 100 100 100 200 40

82.2 88.1 81.3 83.8 91.6 86.7 88.3 95.1 90.1 90.5 83.9 87.7 88.1 97.2 81.3 85.9 85.0 86.3 87.0

85.5 89.7 83.3 85.5 94.2 95.2 90.9 99.2 92.0 92.3 86.1 92.6 91.4 99.1 84.3 90.7 88.4 89.8 91.5

83.7 87.6 80.9 80.3 83.1 90.8 88.5 95.4 89.7 86.4 89.6 83.9 90.8 87.6 95.9 82.1 87.0 85.7 86.5 88.5

84.7 87.3 80.8 81.5 91.0 89.8 87.9 96.7 89.1 84.7 89.4 83.8 87.6 87.7 95.4 81.7 86.2 84.2 85.2 87.3

94.2 97.3 94.5 87.2

86.1 90.0 84.2 83.7 92.7 93.0 90.6 98.0 91.8 96.0 92.2 86.1 91.3 90.0 98.0 84.2 88.7 87.2 88.4 90.0

5.47 4.66 6.96 3.37 7.99 6.52 4.40 3.62 4.01 4.36 4.56 4.68 3.68 3.01 5.27 3.91 3.97 4.20 3.99

12.609 14.156 13.246 15.174 15.305 16.264 16.017 16.337 20.000 19.611 21.820 19.907 21.198 23.250 27.183 26.357 28.293 27.751 29.781

103.7 102.3

97.4

103.6 98.1 94.6 99.1 92.9 98.0 95.2 91.9 93.9 92.7 94.3 95.5 102.6

113.4

101.0

12.18

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