Determination of various pesticide residues in traditional Chinese medicine - GC/MS method

There are hundreds of pesticides used in the cultivation of Chinese herbal medicines, including organophosphate, organochlorine and pyrethroid. The pesticide residues of traditional Chinese medicines have become the bottleneck for Chinese medicines to enter the international market, which seriously lags behind the pace of modernization and internationalization of Chinese herbal medicines. The 2015 edition of the Chinese Pharmacopoeia regulates the determination methods and residue limits of pesticide residues, and also indicates that China's research on pesticide residues in Chinese herbal medicines has been further standardized and standardized.

Method advantages:

Dima Technology follows the "Chinese Pharmacopoeia" 2015 edition of the four parts of the 2341 pesticide residue determination method, the fourth method, pesticide multi-residue determination - mass spectrometry, P212, based on the QuEChERS method principle, using acetic acid water soaking, acetonitrile extraction, adding QuEChERS extraction The salt pack separates the water from the acetonitrile extract. The extraction environment is at a mild pH value to ensure the stability of the target compound. The extract is taken out, added to the QuEChERS purification tube for purification, concentrated and analyzed on the machine. Gas chromatography-mass spectrometry for the detection of pesticide residues in medicinal materials and decoction pieces can achieve quasi-deterministic quantification, quantitative limits meet the requirements of pharmacopoeia, with simple pre-treatment, less recovery loss, obvious purification effect, good method reproducibility, etc. Advantages can be widely used by Chinese medicine analysts. Applicable to all provinces and cities for entry and exit, quality inspection, disease control, food and drug inspection, third-party testing institutions, food testing institutions, large pharmaceutical manufacturers, universities and research institutes.

The following is a detailed solution, please refer to!

Determination of various pesticide residues in traditional Chinese medicine——GC/MS method

1. Scope of application

This program is applicable to dichlorvos, chlorpyrifos, trifluralin, phorate, α-hexachlorocyclohexane, dimethoate, β-hexachlorocyclohexane, lindane, pentachloronitrobenzene, acetonitrile, δ in medicinal materials or decoction pieces. - hexachlorocyclohexane, chlorpyrifos, diarrhea, methyl chlorpyrifos, methyl parathion, heptachlor, methyl chlorpyrifos, picophos, chlorpyrifos, methyl pyrimidine, aldrin , malathion, fenthion, dicofol, chlorpyrifos, parathion, pyrimidine, hexachlorocyclohexane, triazolol, procymidone, chlorpyrifos, alpha-endosulfan, chlordane, dieldrin, Profenofos, p,p'-DDE, endrin, beta-endosulfan, p,p'-DDD, o, p-DDT, ethion, triazophos, endosulfan sulfate, p,p Detection of '-DDT, phoxim, sulforaphane, cyfluthrin, cypermethrin, fenvalerate, difenoconazole, deltamethrin.

*According to the "Chinese Pharmacopoeia" 2015 edition of the four parts of the 2341 pesticide residue determination method, the fourth method of pesticide multi-residue determination - mass spectrometry, P212

2, standard preparation

(1) Single standard stock solution: Accurately weigh each standard and prepare a standard stock solution of 10 mg/mL with toluene.

(2) Mixing standard stock solution: separately absorb each standard standard stock solution and make a mixed standard stock solution of 10 μg/mL with toluene.

3, extraction

(1) Weigh 3 g of sample (pulverized into powder, passed through No. 3 sieve), add 15 mL of 1% acetic acid aqueous solution, mix and soak for 30 min;

(2) Accurately add 15 mL of acetonitrile, shake for 5 min, add QuEChERS extract salt*, shake immediately, shake for 3 min, cool in ice bath for 10 min, centrifuge at 4000 rpm for 5 min, take 9 mL of supernatant, to be purified .

*QuEChERS extraction salt: 6 g anhydrous magnesium sulfate and 1.5 g anhydrous sodium acetate.

4, purification - ProElut QuE 15 mL Tube (Cat#: 64565)

Transfer the liquid to be purified to a 15 mL ProElut QuEChERS purification tube, shake for 5 min, centrifuge at 4000 rpm for 5 min, accurately take 5 mL of the supernatant, slowly blow nitrogen into a 0.4 mL water bath at 40 °C, and dilute to acetonitrile to 1 mL for GC/MS analysis.

5, chromatographic conditions

Column: DM-5MS, 30 m × 0.32 mm × 0.25 μm (Cat. #: 8231)

Inlet temperature: 240 °C

Heating program: initial temperature 70 °C, hold for 2 min, heat up to 150 °C at 25 °C / min, then increase to 3 °C / min to 200 °C, then increase the temperature to 280 °C at 8 °C / min for 10 min

Carrier gas: helium, column flow rate: 0.54 mL/min

Injection method: split injection

Injection volume: 1.0 μL

Ion source temperature: 230 °C

Interface temperature: 280 °C

Solvent delay: 4 min

Electron Impact Ionization Source (EI): Select ion monitoring mode (SIM), group monitoring is shown in Table 1.

Table 1 Selected ion monitoring group table

aisle

Start time (min)

End time (min)

Selective ion (m/z)

1

5.30

6.00

109,185,79

2

10.10

10.50

158,97,139

3

10.90

12.54

306,264,75,121,183,219,111,87,125

4

12.55

13.30

219,181,109,237,295

5

13.70

14.90

88,97,125,142,183,109,219,124,231,161,119,91,204,123

6

15.70

16.80

286,125,109,263,100,272,265,285

7

17.10

18.80

277,125,109,290,305,66,263,93,173,278,139,111,250,97,197,314,291

8

19.60

20.10

333,318,168,353,81

9

20.60

22.20

112,128,168,283,96,145,85,375,237,272,241,195,339

10

23.00

23.60

79,263,108,246,318,176,97,208,339

11

23.90

25.60

81,263,281,241,195,339,235,165,246,231,97,153

12

25.70

26.70

161,77,387,272,237,235,165

13

28.00

29.50

157,169,141,185,182,121

14

31.70

32.70

163,206,91,181,127

15

33.50

41.86

125,167,225,265,323,181,253,77,93

6, add recycling results

GC/MS detection of various pesticide residues in gastrodia elata, licorice, and yam (addition level 200 μg/kg) was added and recovered, and the standard amount was 10 μg/mL mixed with 60 μL.

NO.

Compound name

Recovery rate(%)

Gastrodia

Licorice

Yam

1

Dichlorvos

107.01

99.38

91.09

2

Extinction phosphorus

106.77

105.41

99.26

3

Fluorine

108.10

102.17

93.24

4

Phosphorus

103.61

101.60

99.49

5

--å…­å…­å…­

107.61

100.13

91.47

6

Dimethoate

103.05

82.82

96.51

7

--å…­å…­å…­

107.13

93.45

101.08

8

Lin Dan

109.71

95.86

97.87

9

Pentachloronitrobenzene

76.64

91.85

68.89

10

Acetate

104.45

114.91

94.63

11

Δ-六六六

111.66

82.89

110.14

12

Chlorazol

101.11

108.22

103.65

13

Different rice

112.63

85.62

98.30

14

Methyl chlorpyrifos

99.10

91.75

86.50

15

Methyl parathion

109.24

96.36

102.56

16

Heptachlor

93.51

82.82

92.20

17

Methyl chlorophosphate

106.79

95.56

93.34

18

Fly fly phosphorus

97.01

92.78

83.41

19

Sulphur

110.79

94.96

102.36

20

Methyl pyrimidine

112.90

106.55

85.79

twenty one

Aldrin

101.29

93.67

91.15

twenty two

Malathion

108.05

87.13

101.07

twenty three

Fenthion

116.11

96.03

96.14

twenty four

Dicofol

105.50

83.22

92.30

25

Chlorpyrifos

111.01

95.78

86.56

26

Parathion

112.63

101.92

100.83

27

Pyrimidine

104.56

93.78

94.60

28

Epoxy heptachlor

108.32

90.16

96.95

29

Triazolol

104.51

94.48

103.79

30

Procymidone

113.05

107.53

108.41

31

Killing phosphorus

113.55

94.78

103.74

32

Alpha-endosulfan

110.68

92.21

97.05

33

Chlordane

96.86

81.08

91.96

34

Dield

99.25

110.60

97.75

35

Profenofos

110.27

82.44

97.26

36

p,p'-DDE

99.13

84.26

91.35

37

Endrin

110.53

96.65

101.73

38

Beta-endosulfan

112.36

78.25

103.75

39

p,p'-DDD

103.73

91.52

101.97

40

o, p-DDT

110.49

78.78

91.31

41

Ethion

105.03

98.04

103.24

42

Triazophos

98.77

87.38

98.41

43

Endosulfan sulfate

106.94

91.43

107.35

44

p,p'-DDT

103.45

84.23

93.53

45

Phenylphos

88.58

119.11

91.89

46

Sulfox

88.46

93.37

85.93

47

Cyfluthrin-1

107.01

109.07

86.90

48

Cyfluthrin-2

106.77

100.38

93.41

49

Cyfluthrin-3

108.10

93.24

88.09

50

Cyfluthrin-4

103.61

84.80

98.07

51

Cypermethrin-1

107.61

83.09

94.66

52

Cypermethrin-2

87.30

85.79

95.60

53

Cypermethrin-3

113.05

92.14

99.68

54

Cypermethrin-4

117.13

96.88

105.17

55

Fenvalerate-1

109.71

101.89

81.34

56

Fenvalerate-2

86.64

82.44

87.73

57

Difenoconazole

104.45

103.85

104.10

58

Deltamethrin

111.66

96.27

104.44

Multiple pesticide residue standards (10 μg/mL) TIC map

Determination of various pesticide residues in traditional Chinese medicine - GC/MS related product information:

Item number

name

specification

Sample preparation

64565

ProElut QuE 15 mL Tube

15 mL, 50/pk

30039

FitMax needle filter Nylon

13 mm, 0.22 μm 100/pk

30040

FitMax needle filter Nylon

13 mm, 0.45 μm 100/pk

Standard

For related standard information, please call 400-608-7719

Column and guard column

8231

DM-5MS

30 m × 0.32 mm × 0.25 μm

HPLC Solvent? Buffer Salt? Ion Pair Reagent

50101

Acetonitrile HPLC grade

4 L

50132

Acetic acid HPLC grade

50 mL

General purpose chromatography products

52401B

Bottle holder / blue (spot)

50 holes

52401A

Bottle holder / white (spot)

50 holes

1034

Vial (brown/thread)

2 mL, 100/pk

1035

Sample cap/with pad (already assembled)

100/pk

H87900

GC syringe

5 μL

Red product number #30039, #30040, #1034, #1035 hot promotion