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Analysis of Multi-Pesticide Residues in Potato Using MAS-QuEChERS Kits by LC-MS/MS (AOAC 2007.01)

Application Introduction

The severe pesticide pollution caused by massive application of pesticides, especially organic pesticides, has become a severe threat to human health.

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Introduction

The severe pesticide pollution caused by massive application of pesticides, especially organic pesticides, has become a severe threat to human health. Among the pesticides currently used, some can be biodegraded to innocuous substances within a short time; organochlorine pesticides, including DDT, are difficult to biodegrade due to their strong residual character; organophosphorus pesticides and carbamate pesticides are easy to decompose under the influence of external conditions after application due to their unstable chemical property, but some types of them are highly-toxic and extremely-toxic pesticides, such as methamidophos, parathion, aldicarb, carbofuran and isocarbophos. It is difficult to avoid human and animal poisoning caused by excessive pesticide residues if these highly-toxic and extremely-toxic pesticides are applied to vegetables continuously harvested with relatively short growth periods. The QuEChERS method is time-saving and labor-saving, and the sample’s influence on instrument is lowered after the pigments, organic acid and other impurities of sample are removed through the extraction.

Experimental

Sample Extraction

Weight 10 g homogenized potato sample into a 50 mL centrifuge tube. Add 10 mL 0.1% acetic acid acetonitrile for extraction. Add the MAS-QuEChERS Extraction Kits (P/N: MSMG5052) and four glass homogenizers into the sample. Shake vigorously for 1 min, and centrifuge at 6000 r/min for 5 min.

Sample Cleanup

Take 1 mL supernatant into a 2 mL MAS-QuEChERS Cleanup Tube (P/N: MS-9PP0265). Shake for 1 min and centrifuge at 6000 r/min for 5 min. Transfer the supernatant and dilute with water. The solution was then filtered by Nylon filter for LC-MS/MS analysis.

Instrumentation

Chromatographic columns: Unisol C18 (3 μm, 100 Å, 3.0 × 50 mm);

Mobile phases:

Phase A: Ammonium formate aqueous solution (concentration: 5 mM)

Phase B: Formic acid -methanol solution (concentration: 5 mM);

Column temperature: 30 °C;

Sample size: 5 µL;

Gradient elution conditions (see Table 1)

Ion source: ESI+; ESI voltage: 4500 V;

Atomized gas pressure: 50 psi; Curtain gas pressure: 10 psi;

Auxiliary gas pressure: 50 psi; Ion source temperature: 400 °C;

Collecting mode: MRM.

Table 1 Gradient Condition

Time/min

Flow rate (mL/min)

A/%

B/%

0.0

0.4

95

5

0.5

0.4

95

5

1.0

0.4

60

40

3.0

0.4

15

85

4.5

0.4

5

95

6.0

0.4

5

95

6.1

0.4

95

5

12.0

0.4

95

5

Table 2 MS Parameters

Analytes

Q1

Q3

DP/V

CE/V

Methamidophos

142

94

54

19

25

54

18

Acephate

184

143

50

10

125

50

26

Omethoate

214

182.9

56

16

109

56

36

Aldicarb sulfoxide

207

132

51

10

89

51

20

Aldicarb Sulfone

223

148

63

12

76.1

63

10

Methomyl

163

106

38

13

88

38

13

Thiamethoxam

292

211

60

18

181

60

32

Imidacloprid

256.1

209

60

23

175

60

26

3-Hydroxycarbofuran

238

181

65

14

163

65

20

Dichlorvos

221

109

70

23

127

70

25

Trichlorfon

274

109

32

25

220.9

32

22

Acetamiprid

223

126

70

27

99

70

47

Dimethoate

230

125

56

29

199

56

13

Carbendazim

192

160

80

25

132

80

41

Aldicarb

116.1

89

51

10

70

51

20

Carbofuran

222.1

165

70

17

123.1

70

29

Carbaryl

202.1

145

54

15

127

54

40

Isofenphos-methyl

273

231

39

13

121.1

39

33

Azoxystrobin

404.1

372

70

20

344.1

70

34

Phosmet

318

160

38

16

133

38

49

Dimethomorph

388.1

301

115

29

165

115

43

Malathion

331

127

64

17

285

64

13

Triadimefon

294

197

81

21

225

81

17

Pyrimethanil

200

107

91

34

82

91

37

Triazophos

314

162

70

25

119.1

70

47

Fipronil

454

436.9

50

15

367.9

50

31

Iprodione

330.1

245

50

21

288

50

18

Diflubenzuron

311

158

72

21

141.2

72

47

Isocarbophos-H2O

273.1

231

67

15

121

67

32

Chlorbenzuron

309

156

75

20

139

75

44

Diazinon

305

169

80

27

153

80

28

Fenthion

279.1

169

78

23

247

78

18

Phoxim

299.1

77

67

46

129

67

16

Phosalone

368

182

71

20

322

71

13

Prochloraz

376.2

308

65

17

70.1

65

43

Phorate

261.1

75.2

34

14

199

34

11

Difenoconazole

406.1

251

120

37

337

120

23

Profenofos

373

302.9

80

25

345.2

80

18

Emamectin   B1a

886.5

158.1

120

37

302.1

120

39

Fenpropathrin

350.2

97.1

71

43

125.1

71

15

Chlorpyrifos

350

198

82

29

97

82

49

Pendimethalin

282.1

212

45

15

194

45

25

Chlorfluazuron

540

383

80

27

158

80

24

Pyridaben

365

309

110

17

147

110

31

Bifenthrin

440.3

181.1

40

17.6

166.2

40

56

Results and Discussion

Table 1 Recoveries and reproducibility of pesticides in potato samples (spiked sample 0.03 mg/kg)

Pesticides

Retention   time/min

Recoveries/%

RSD/%

Methamidophos

1.96

83.9

13.1

Acephate

3.13

89.2

1.5

Omethoate

3.50

96.8

4.1

Aldicarb sulfoxide

3.62

99.6

1.3

Aldicarb Sulfone

3.75

102.8

1.9

Methomyl

3.98

87.9

6.1

Thiamethoxam

4.06

90.1

1.3

Imidacloprid

4.32

88.4

3.1

3-Hydroxycarbofuran

4.44

91.5

1.4

Dichlorvos

4.47

91.5

4.1

Trichlorfon

4.48

78.6

6.0

Acetamiprid

4.50

96.9

2.3

Dimethoate

4.51

95.2

4.2

Carbendazim

4.79

61.7

9.6

Aldicarb

4.83

96.2

0.7

Carbofuran

5.05

101.9

1.0

Carbaryl

5.16

100.4

0.4

Isofenphos-methyl

5.34

92.1

1.1

Azoxystrobin

5.45

97.3

2.8

Phosmet

5.51

82.5

0.9

Dimethomorph

5.66

90.2

2.7

Malathion

5.67

87.9

1.8

Triadimefon

5.68

87.3

2.0

Pyrimethanil

5.70

70.9

5.3

Triazophos

5.75

91.6

3.0

Fipronil

5.85

89.0

21.2

Iprodione

5.91

80.8

20.7

Diflubenzuron

5.95

64.0

1.4

Isocarbophos-H2O

5.97

78.7

3.4

Chlorbenzuron

6.05

58.4

2.9

Diazinon

6.10

96.2

0.9

Fenthion

6.11

79.1

3.7

Phoxim

6.15

96.7

1.8

Phosalone

6.18

69.7

0.0

Prochloraz

6.19

86.3

0.2

Phorate

6.24

86.0

14.2

Difenoconazole

6.27

87.8

1.6

Profenofos

6.51

82.4

1.4

Emamectin B1a

6.70

63.7

2.9

Fenpropathrin

6.79

70.4

0.3

Chlorpyrifos

6.82

91.9

0.1

Pendimethalin

6.89

61.6

0.6

Chlorfluazuron

7.02

39.6

4.7

Pyridaben

7.28

68.2

1.6

Bifenthrin

7.80

90.3

17.0

Figure 1 Chromatogram of 0.01 µg/mL standard solution of pesticides

Figure 2 Chromatogram of potato blank sample

Figure 3 Chromatogram of 0.03 mg/kg fortified potato extract

Conclusion

The detection results show that, the recoveries of 33 kinds of pesticide residues among the 45 kinds are conforming to the requirement and RSD is no more than 20% using MAS-QuEChERS Kits, proving this method is stable and applicable to the detection of the 33 kinds of pesticide residues in the potato.

Order Information

Products

Specification

Cat.No

MAS-QuEChERS Extraction Kits

6 g MgSO4 (Anhydrous), 1.5 g NaAc(Anhydrous) with   50 mL centrifuge tube

MS-MG5052

MAS-QuEChERS Cleanup Tube

50 mg PSA, 50 mg C18, 8 mg PC, 150 mg MgSO4(Anhydrous)   with 2 mL centrifuge tube

MS-9PP0265

Glass homogenizers

Diameter: 10 mm

HG-01

Unisol C18

3 µm, 100 Å, 3.0 × 50 mm

UO930503-0

1.5 mL vials

Screw neck vials, 12 × 32 mm

AV1001-6

Caps and Septa

Screw neck cap, center hole; red silicone/white PTEE septa, slitted

AV2200-0

Nylon Syringe Filters

13 mm, 0.22 μm

AS021320

Disposable Syringe

2 mL, no needle

LZSQ-2ML

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