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Simultaneous Detection of 152 Kinds of Pesticide Residues in Cabbage and Apple by LC-MS/MS using QuEChERS

Application Introduction

The QuEChERS method is established according to AOAC standard to extract and detect 152 types of pesticides in two matrices - cabbages and apples - at the same time.

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Introduction

The QuEChERS method is established according to AOAC standard to extract and detect 152 types of pesticides in two matrices - cabbages and apples - at the same time.

Experimental

Sample extraction

Cabbage: Weigh 15 g of cabbage sample with a good homogeneity, and transfer it into a 50 mL vegetable & fruit extraction tube. Add 15mL of acetic acid-acetonitrile solution (concentration: 1%), Bonna-Agela MAS-QuEChERS vegetable & fruit extraction package (P/N: MS-MG5052) and 4 glass beads to the tube in turn. Keep violently oscillating the tube manually for 1min and keep centrifuging the tube at 8000 rpm for 5 min, and then reserve 1 mL of supernate for purification.

Apple: Weigh 15 g of apple sample with a good homogeneity, and transfer it into a 50 mL vegetable & fruit extraction tube. Add 15mL of acetic acid-acetonitrile solution (concentration: 1%), Bonna-Agela MAS-QuEChERS vegetable & fruit extraction package (P/N: MS-MG5052) and 4 glass beads to the tube in turn. Keep violently oscillating the tube manually for 1min and keep centrifuging the tube at 8000 rpm for 5 min, and then reserve 1 mL of supernate for purification.

Sample purification

Cabbage: Add the aforesaid cabbage supernate to be purified to a 2 mL Bonna-Agela MAS-QuEChERS vegetable & fruit purification tube (P/N: MS-PA0250). Keep oscillating the tube manually for 1min and keep centrifuging the tube at 8,000rpm for 5min. Then filter proper amount of supernate with a 0.22 μm nylon membrane for LC-MS detection.

Apple: Add the aforesaid apple supernate to be purified to a 2 mL Bonna-Agela MAS-QuEChERS vegetable & fruit purification tube (P/N: MS-9PA0203). Keep oscillating the tube manually for 1min and keep centrifuging the tube at 8000 rpm for 5 min. Then filter proper amount of supernate with a 0.22 μm nylon membrane for LC-MS detection.

Preparation of matrix-mixed standard working solution

Dilute the high-concentration pesticide-mixed standard solution with blank sample matrix solution to the matrix-mixed standard working solution (concentration: 0.03 μg/mL).

Instrumentation

Chromatographic columns: Venusil® ASB C18 (5 μm, 150 Å, 2.1 × 150 mm);

Mobile phases:

Phase A: Formic acid aqueous solution (concentration: 0.1%)

Phase B: Formic acid -acetonitrile solution (concentration: 0.1%);

Column temperature: 30 °C;

Sample size: 10 µL;

Gradient elution conditions (see Table 1)

Ion source: ESI+; ESI voltage: 5500 V;

Atomized gas pressure: 50 psi; Curtain gas pressure: 15 psi;

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

Collecting mode: MRM.

Table 1 LC Gradient Elution Chart

Time/min

Flow rate

(mL/min)

A/%

B/%

0.00

0.3

99

1

3.00

0.3

70

30

6.00

0.3

60

40

9.00

0.3

60

40

15.00

0.3

40

60

19.00

0.3

1

99

23.00

0.3

1

99

23.01

0.3

99

1

40.00

0.3

99

1


Figure 3 LC-MS/MS Chromatogram of Cabbage Matrix-mixed Standard Working Solution (concentration: 0.03 μg/mL)

Figure 4 LC-MS/MS Chromatogram of Cabbage Matrix Sample with Standard Addition (content: 0.03 mg/kg)

Figure 5 Blank LC-MS/MS Chromatogram of Apple Matrix

Figure 6 LC-MS/MS Chromatogram of Apple Matrix-mixed Standard Working Solution (concentration: 0.03 μg/mL)

Figure 7 LC-MS/MS Chromatogram of Apple Matrix Sample with Standard Addition

(concentration: 0.03 mg/kg)

Table 3 LC-MS/MS Standard Addition Recovery Experiment Results of 152 kinds of Pesticide Residues in Apple and Cabbage (n=3) (adding level: 0.03 mg/kg)

Substance

Apple

Cabbage

Recovery rate (%)

RSD(%)

Recovery rate (%)

RSD(%)

RT/min

Chlordimeform

81.5

7.0

88.6

7.1

1.4

Aldicarb-sulfoxide

85.6

4.4

83.5

5.1

12

Dinotefuran

99.3

1.6

94.6

8.6

12.1

Aldicarb-sulfone

81.0

8.9

73.2

7.1

12.2

Oxamyl

86.0

4.0

84.0

8.3

12.7

Demeton-S-methylsulfoxide

105.1

4.9

97.7

9.1

12.9

Monocrotophos

86.2

5.3

93.5

8.7

13.1

Trichlorfon

81.3

3.9

91.3

9.7

13.3

Thiofanox-sulfoxide

85.7

6.9

85.0

3.2

13.9

Clothianidin

79.6

3.5

67.0

9.1

14.3

Dimethoate

91.5

3.2

75.2

8.4

14.5

Thiofanox-sulfone

81.9

4.0

74.0

9.1

14.6

ImazamethabenzMethyl

97.4

7.7

66.4

7.5

15

Acetamiprid

69.5

2.2

64.4

5.6

15.2

Cymoxanil

71.0

8.2

72.8

4.9

15.2

Flumetsulam

93.8

9.0

106.2

6.9

15.3

Oxycarboxin

94.5

2.8

63.0

5.0

15.5

Aldicarb

97.2

2.5

83.5

8.7

15.8

Carbetamide

66.0

6.2

68.6

5.5

16

Imazethapyr

83.0

5.8

60.6

8.6

16

Tebuthiuron

101.2

5.0

75.3

6.2

16.1

Thiacloprid

101.1

8.4

65.1

6.3

16.1

Fenpropimorph

108.2

8.9

88.1

3.7

16.2

Phosphamidon

97.9

8.2

98.4

8.8

16.2

Phoxim

75.5

8.0

99.6

9.5

16.2

Spiroxamine

85.4

6.4

102.9

7.9

16.2

Metolcarb

90.5

4.2

107.4

6.9

16.3

Isouron

87.3

6.6

74.5

5.8

16.6

Thidiazuron

83.2

5.2

70.3

9.4

16.6

Cyanazine

109.1

3.9

69.9

7.9

16.7

Demeton-S-methyl

79.0

9.3

88.7

7.9

16.9

Foramsulfuron

87.0

4.1

94.5

7.7

16.9

Azamethiphos

78.2

7.1

101.7

5.0

17

Thiophanate-methyl

90.0

4.3

92.7

9.3

17.2

Lenacil

78.6

9.8

82.6

8.6

17.2

Imazaquin

85.9

6.9

74.0

9.0

17.3

Thifensulfuron-methyl

81.3

6.7

75.6

6.5

17.3

Carbofuran

61.9

4.0

75.8

8.8

17.4

Cinosulfuron

93.0

4.3

77.2

9.0

17.7

Metsulfuron-methyl

90.9

3.1

75.3

9.9

17.7

Florasulam

78.8

6.8

78.9

4.5

17.8

Substance

Apple

Cabbage

Recovery rate (%)

RSD(%)

Recovery rate (%)

RSD(%)

RT/min

Methabenzthiazuron

77.4

7.0

74.8

9.8

18

Thiodicarb

96.5

1.8

60.3

7.0

18.1

Triasulfuron

74.1

9.4

69.7

8.6

18.1

Chlortoluron

87.5

9.8

69.7

6.0

18.2

Carbaryl

78.0

5.8

67.4

2.2

18.2

Diuron

83.4

6.2

75.0

8.7

18.3

Fluometuron

78.8

0.5

75.0

5.3

18.3

Carboxin

78.6

9.6

70.7

9.3

18.4

Amidosulfuron

92.0

9.6

86.1

7.1

18.4

Chlorsulfuron

82.3

7.1

79.7

6.9

18.5

Monolinuron

92.2

7.3

86.9

8.1

18.5

Cyprodinil

79.5

4.6

90.9

8.9

18.5

Ethiofencarb

96.0

9.0

107.2

6.3

18.5

Rimsulfuron

79.3

4.9

106.4

7.1

18.5

Forchlorfenuron

83.9

7.0

66.6

7.7

18.7

Ethametsulfuron-methyl

90.4

9.0

75.3

9.9

18.8

Furametpyr

84.5

6.4

80.2

7.0

18.9

Isoproturon

104.4

7.5

71.9

6.8

19.1

Dimethirimol

84.2

1.8

109.7

7.6

19.3

Metosulam

82.3

7.9

79.6

5.4

19.3

Bupirimate

93.4

2.5

109.1

8.0

19.3

Azimsulfuron

91.2

5.7

75.5

7.4

19.4

Mesosulfuron-methyl

92.0

0.4

88.2

9.2

19.4

Azaconazole

76.7

7.1

83.0

0.7

19.8

Flumorph

95.8

8.3

82.2

8.6

19.8

Demeton

83.8

2.5

75.6

9.9

19.9

Thiophanate

88.2

5.8

77.1

8.4

20.3

Cloransulam-methyl

83.4

9.1

77.8

5.2

20.3

Sulfosulfuron

101.8

9.8

92/8

3.4

20.3

Chlorantraniliprole

97.3

5.2

69.0

7.8

20.6

Bensulfuron-methyl

66.8

2.3

70.9

6.5

20.6

Nicosulfuron

99.2

5.5

81.2

9.0

20.6

Fensulfothion

86.3

9.1

74.4

8.2

20.7

Flazasulfuron

97.3

9.8

77.8

7.2

20.8

Diclosulam

85.3

2.6

84.3

4.0

20.9

Imazosulfuron

103.8

9.6

62.0

6.9

20.9

Spinetoram

80.8

4.5

81.0

8.5

21.1

Propoxycarbazone

76.3

2.9

91.8

7.3

21.3

Methiocarb

105.3

9.2

74.6

8.4

21.3

Iodosulfuron-methyl

70.6

7.8

76.4

8.3

21.4

Diethofencarb

97.8

1.9

68.9

5.6

21.4

Linuron

82.0

0.2

68.9

4.3

21.5

Substance

Apple

Cabbage

Recovery rate (%)

RSD(%)

Recovery rate (%)

RSD(%)

RT/min

Prochloraz

97.4

9.4

75.7

9.4

21.5

Desmedipham

90.1

3.0

66.4

5.3

21.7

Phenmedipham

109.4

2.2

66.4

8.3

21.8

Ethiprole

76.0

3.6

75.4

6.5

21.9

Promecarb

76.6

0.8

86.9

8.8

21.9

Iprovalicarb

84.1

0.9

84.7

7.5

22.1

Prosulfuron

92.6

8.2

74.1

8.3

22.2

Pyrazosulfuron-ethyl

97.0

8.6

80.6

8.0

22.2

Paraoxon-methyl

89.7

5.7

85.9

3.6

22.5

Fenamiphos

76.4

1.0

81.0

8.9

22.6

Spirotetramat

78.6

8.9

78.9

9.1

22.6

Chloroxuron

66.3

6.4

77.5

5.2

22.7

Cumyluron

99.5

3.6

74.5

7.7

22.7

Mefenacet

92.9

3.1

82.3

7.4

22.7

Fenhexamid

82.6

4.8

78.2

6.2

22.7

Mepanipyrim

95.8

6.1

75.5

8.2

22.8

Halosulfuron Methyl

80.3

8.2

80.6

7.6

22.9

Azoxystrobin

69.3

1.4

74.2

1.7

23

Boscalid

95.4

5.1

76.4

9.6

23

Fluopicolide

86.0

5.7

85.7

4.5

23.3

Mandipropamid

90.9

9.7

74..9

5.8

23.4

Metolachlor

87.7

9.2

86.9

7.9

23.5

Triflusulfuron-methyl

89.9

9.7

69.8

9.5

23.5

Diflubenzuron

79.5

3.3

76.1

7.7

23.7

Methoxyfenozide

78.3

2.8

76.5

4.9

23.7

Cyclosulfamuron

79.6

5.0

83.2

9.5

23.9

Ametoctradin

92.9

7.1

75.5

7.1

24

Cafenstrole

107.4

8.7

80.9

6.2

24.1

Thenylchlor

89.5

5.8

80.6

5.0

24.1

Fenbuconazole

95.4

5.1

78.8

9.5

24.2

Chlorbenzuron

97.8

4.5

66.7

7.2

24.2

Fenoxycarb

104.9

3.1

76.5

8.0

24.3

Rotenone

98.7

6.1

67.4

8.3

24.4

Edifenphos

88.6

1.6

72.5

3.5

24.5

Alanycarb

66.8

2.4

61.0

4.3

24.6

Tebufenozide

109.1

9.3

80.6

5.0

24.7

Propisochlor

81.1

4.1

88.7

7.2

24.8

Fluthiacet-Methyl

99.1

2.3

74.5

6.1

24.9

Pyrazoxyfen

101.9

9.9

84.4

7.0

24.9

Isoxadifen-Ethyl

91.0

4.3

71.7

9.4

25.1

Flubendiamide

91.2

1.0

77.9

6.1

25.1

Triflumuron

103.4

7.3

83.9

9.0

25.2

Substance

Apple

Cabbage

Recovery rate (%)

RSD(%)

Recovery rate (%)

RSD(%)

RT/min

Pyraclofos

83.9

3.5

78.6

7.9

25.3

Bensulide

74.7

2.6

73.5

7.6

25.6

Chlorimuron-ethyl

72.4

4.8

72.8

6.5

25.6

Pyraclostrobin

97.8

3.3

75.1

7.5

25.7

Clofentezine

70.9

9.6

68.8

8.6

25.8

Pencycuron

87.8

4.7

81.9

6.0

25.8

Difenoconazole

89.1

1.3

77.2

9.1

25.8

Coumaphos

87.8

7.2

81.6

7.0

25.9

Cycloxydim

85.8

7.0

69.3

9.8

26

Haloxyfop-R-methyl

91.8

9.0

85.9

7.4

26.1

Diflufenican

71.7

7.5

79.4

6.9

26.2

Hexaflumuron

90.2

8.1

89.1

8.8

26.2

Isoxathion

96.7

8.0

77.3

4.6

26.2

Indoxacarb

95.8

8.3

67.2

9.0

26.3

Quizalofop-ethyl

86.9

5.5

76.9

6.5

26.3

Clethodim

74.1

2.0

67.1

3.8

26.4

Sethoxydim

92.6

6.3

68.3

1.6

26.5

Imibenconazole

89.2

8.2

70.7

9.9

26.6

Cinidon-ethyl

78.5

1.3

72.3

9.4

26.7

Furathiocarb

81.9

3.0

86.9

7.7

26.7

Tralkoxydim

74.0

2.8

68.3

8.9

26.9

Flucarbazone-sodium

75.3

9.8

69.2

9.1

27.3

Temephos

74.2

2.2

65.6

8.0

27.3

Flufenoxuron

73.2

9.8

72.7

5.9

27.3

Butralin

75.5

8.0

107.1

6.6

27.4

Spiromesifen

79.6

3.0

74.8

9.5

28

Carbosulfan

84.5

5.3

77.0

9.9

29

Conclusion

 

This experiment establishes the QuEChERS pretreatment method for pesticide residues in cabbage and apple in accordance with standard AOAC2007.01, and detects the samples (standard addition amount: 0.03mg/kg) on the basis of LC-MS/MS method. The resulted recovery rates are between 60% and 110%, conforming to the national standard requirements. Moreover, the data obtained by QuEChERS method are relatively stable, showing this method can be applied to the detection of pesticide residues in cabbage and apple.

Order Information

Products

Specification

Cat.No

Venusil®   ASB C18

5 μm, 150 Å, 2.1   × 150 mm

VS951502-0

MAS-QuEChERS   Extraction Kits

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

MS-MG5052

MAS-QuEChERS   Cleanup Kits

50 mg C18, 50 mg   PSA, 150 mg MgSO4(Anhydrous), with 15 mL centrifuge tube

MS-9PA0203

MAS-QuEChERS   Cleanup Kits

2 mL Centrifuge   tube for 1 mL sample, 50 mg PSA, 150 mg MgSO4

MS-PA0250

Guard cartridge   holder

Suitable for 4.6 ×   10 mm and 2.1 × 10 mm

SH-100

Direct-coupled   protect column core

5 μm, 150 Å, 2.1×10 mm, 4/pk

VS950102-0S

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

Syringe Filter (Nylon)  

Monofilm, 13 mm,   0.22 μm

AS021320

Disposable   Needle-Free injection systems

2 mL, 100/pk

LZSQ-2ML

 

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