AOAC-RI ERP Book - FAOM METHOD.pdf

3/9/2017

Lab-2:

Determination results of multi-residues in tea by LC-MS/MS

Greentea

Retention time/min

Spike levels (μg/kg)

Calibration curve

Recovery/%

No.

Pesticides

RSD/ %

R2

Slope Intercept

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

IS chlorpyrifos-methyl

17.618

1 imidacloprid

5.663 8.264 9.409

0.9987 0.9989 0.9980

0.0850 1.8593 0.0116 0.7681 0.3678 0.2186 0.2468 0.4262 2.5914 0.1833 1.4234 1.2458 2.9582 0.2903 0.6027 0.0441 0.0263 0.4936 0.0072

0.0856 31.8969 -0.0314 0.9358 1.0466 -1.0063 -0.3841 -0.8631 18.3183 5.8772 1.7725 5.7368 -2.6557 0.2172 4.4482 -0.3803 -0.0882 -1.0594 -0.0321

45 50 20 20 20 20 40 20 20 20 20 20 60 20 20 20

115.4 108.6

103.8

114.8 114.0

111.4 108.4

105.3 108.1

110.1 106.5

4.87 7.30 3.28 5.00 4.65 4.28 4.14 4.01 4.44 6.21 3.45 5.93 8.30 7.50 6.22 5.84 3.85

2 propoxur

93.3 91.6 94.0 92.7 94.2 94.0 96.1 92.5 96.0 97.5 90.0 95.5 93.3 95.6 99.8 94.3 98.6

3 monolinuron 4 clomazone 5 ethoprophos 6 triadimefon 7 acetochlor

87.3 93.8

93.1

86.3 96.6 97.1 98.2 99.4

91.1

89.9 98.0 99.6

11.107 0.9991 13.899 0.9991 14.096 0.9985 15.138 0.9990 15.671 0.9969 16.571 0.9946 17.119 0.9965 16.453 0.9999 17.405 0.9952 17.491 0.9961 18.016 0.9941 18.262 0.9992 18.311 0.9978 18.884 0.9928 16.24 0.9990 17.09 0.9997

100.2 103.0 102.9 102.2 105.9 102.5

105.5 104.0 104.2 105.2 105.0 104.0 103.7 110.3

101.1 103.6

100.6 100.0 102.8

99.4

8 flutolanil 9 benalaxyl

105.4

101.6

99.9

98.9

99.6

10 kresoxim-methyl 11 picoxystrobin 12 pirimiphos-methyl 13 diazinon 14 bensulide 15 quinoxyfen 16 tebufenpyrad 17 indoxacarb 18 trifloxystrobin 19 chlorpyrifos

200

107.1 133.5

92.0 97.4 94.3 97.4 99.7 89.3 97.9

103.6 102.5

100.5 108.2

13.93

93.1

91.7 97.1

98.5

93.5

105.9 116.7

108.8 106.0

101.0 103.8

103.2

100

81.6

93.8

99.6

92.0

114.5 100.6 101.7 111.4

105.3 104.2 100.2

106.4 104.9 108.9

104.8 102.9 102.2 101.0

110.6 101.7

200

126.6

92.8

87.2

87.1

17.26

20 butralin

19.292 0.9956

0.0022

-0.0035

20

72.1

84.2

82.1

99.2

128.0

93.1

23.37

Lab-13: Recoveries for 41 pesticides in green tea and black tea determined by GC-MS: 70%-94% Pesticides Recovery Pesticides Recovery Pesticides Recovery Phorate 84% Fenthion 82% Cypermethrin 88% Quintozene 81% Malathion 82% Fenvalerate 90% Diazinon 85% Fenitrothion 84% Deltamethrin 87% Fonofos 80% Triadimefon 78% Trifluralin 84% Etrimfos 79% Pendimethalin 81% Sulfotep 81% Dimethoate 70% Quinalphos 88% Α-HCH 84% Aldrin 81% Phenthoate 81% Δ-HCH 88% Vinclozolin 79% Procymidone 92% Β-HCH 83% Buprofezin 82% Dieldrin 80% Dicofol 85% Metalaxyl 81% Methidathion 80% p,p'-DDD 79% Methyl-parathion 85% Fenamiphos 80% o,p'-DDD 80% Chlorpyrifos 90% Terbufos 81% o,p'-DDT 80% Chlorpyrifosmethyl 93% Bifenthrin 94% p,p'-DDE 80% Triazophos 84% Fenpropathrin 89%

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