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3/9/2017

11

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).

No.

Pesticides

Retention

time/min

Green tea

Calibration curve

Spike

levels

(μg/kg)

Recovery/%

RSD/

%

R

2

Slope Intercept

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

IS heptachlor

18.787

1 trifluralin

9.940

0.9997

1.0858

-0.0155

200

82.2

85.5

83.7

84.7

94.2

86.1

5.47

2 tefluthrin

12.609

0.9982

1.8509

0.3906

100

88.1

89.7

87.6

87.3

97.3

90.0

4.66

3 pyrimethanil

14.156

0.9977

2.6666

0.5547

100

81.3

83.3

80.9

80.8

94.5

84.2

6.96

4 propyzamide

13.246

0.9984

0.9642

0.2457

100

83.8

85.5

80.3

81.5

87.2

83.7

3.37

5 pirimicarb

15.174

0.9981

1.5951

0.4131

100

91.6

94.2

83.1

91.0

103.7

92.7

7.99

6 dimethenamid

15.305

0.9963

0.4662

0.1679

40

86.7

95.2

90.8

89.8

102.3

93.0

6.52

7 tolclofos-methyl

16.264

0.9971

1.3229

0.3183

100

88.3

90.9

88.5

87.9

97.4

90.6

4.40

8 fenchlorphos

16.017

0.9965

1.2458

0.3545

200

95.1

99.2

95.4

96.7

103.6

98.0

3.62

9 pirimiphos-methyl

16.337

0.9977

0.5001

0.1095

100

90.1

92.0

89.7

89.1

98.1

91.8

4.01

10 2,4-DDE

20.000

0.9977

4.0213

0.7936

400

113.4

101.0

86.4

84.7

94.6

96.0

12.18

11 bromophos-ethyl

19.611

0.9973

0.3133

0.0691

100

90.5

92.3

89.6

89.4

99.1

92.2

4.36

12 4,4-DDE

21.820

0.9978

3.1875

0.6239

400

83.9

86.1

83.9

83.8

92.9

86.1

4.56

13 procymidone

19.907

0.9975

0.3892

0.0890

100

87.7

92.6

90.8

87.6

98.0

91.3

4.68

14 picoxystrobin

21.198

0.9979

0.7657

0.1335

200

88.1

91.4

87.6

87.7

95.2

90.0

3.68

15 chlorfenapyr

23.250

0.9976

0.4209

0.0998

800

97.2

99.1

95.9

95.4

102.6

98.0

3.01

16 quinoxyfen

27.183

0.9980

1.1099

0.2239

100

81.3

84.3

82.1

81.7

91.9

84.2

5.27

17 benalaxyl

26.357

0.9976

1.5987

0.3213

100

85.9

90.7

87.0

86.2

93.9

88.7

3.91

18 bifenthrin

28.293

0.9978

3.0963

0.8757

100

85.0

88.4

85.7

84.2

92.7

87.2

3.97

19 diflufenican

27.751

0.9982

2.0066

0.3759

100

86.3

89.8

86.5

85.2

94.3

88.4

4.20

20 bromopropylate

29.781

0.9978

1.8023

0.3328

200

87.0

91.5

88.5

87.3

95.5

90.0

3.99

Lab-2:

Determination results of multi-residues in tea by

GC-MS