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Simultaneous Detection of 50 Kinds of Pesticide Residues (including organophosphorus, organochlorine, pyrethroids, carbamates, etc.) in apple using QuEChERS Method

Application Introduction

As a key part in evaluating food safety, pesticide residues in apples have already been included in food safety inspection plans of America, Japan and EU and are under routine testing every year.

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Introduction

As a key part in evaluating food safety, pesticide residues in apples have already been included in food safety inspection plans of America, Japan and EU and are under routine testing every year. Currently, an increasing number of pesticide residues in apples are being tested with the detection limit constantly being lowered. This article introduces the QuEChERS method for the extraction and detection of 50 pesticide residues that are commonly found in apples such as organophosphorus, organochlorine, dimethrin and carbamates.

Experimental

Sample extraction

Weigh 15g of apple sample with a good homogeneity, and transfer it into a 50mL vegetable & fruit extraction tube. Add 15mL of acetic acid-acetonitrile solution (concentration: 1%), Add Bonna-Agela MAS-QuEChERS vegetable & fruit extraction kits (P/N: MS-MG5050) and 4 glass beads to the tube in turn. Keep violently oscillating the tube manually for 1min and keep centrifuging the tube at 8,000rpm for 5min, and then reserve 10 mL of supernate for purification.

Sample purification

Add the aforesaid supernate to be purified to a 15mL Bonna-Agela MAS-QuEChERS vegetable & fruit cleanup tube (P/N: MS-9PA1011). Keep oscillating the tube manually for 1 min and keep centrifuging the tube at 8,000 rpm for 5 min. Then blow 5ml of supernate with nitrogen to nearly dry at 40 °C, dissolve it with 1mL of acetone for the next GC detection.

Blow additional 5ml of supernate with nitrogen to nearly dry at 40 °C, and dissolve it with 1mL of acetonitrile for the next LC detection.

Instrumentation

Chromatographic columns: pre-columns (1.0 m, inner diameter: 0.53 mm, deactivating quartz capillary columns)

Column A: DA-50+ chromatographic column, 30 m × 0.53 mm × 1.0 μm

Column B: DA-1 chromatographic column, 30 m × 0.53 mm × 1.50 μm

Injection port temperature: 220 °C

Detector temperature: 250 °C

Column temperature: 150 °C (kept for 2 min) to 250 °C (kept for 12 min)(8 °C/min rise)

Carrier gas: nitrogen (purity ≥ 99.999%, flow rate: 10 mL/min)

Combustion gas: hydrogen (purity ≥ 99.999%, flow rate: 75 mL/min)

Oxidizing gas: air (flow rate: 100 mL/min)

Sample size: 1 µL

Injection mode: Splitless injection. The duplicated samples are injected simultaneously by a dual-automatic sample injector.

Results and Discussion

Table 1 Results of Organophosphorus Pesticide Residues in apple using QuEChERS method by GC-FPD (spiked sample 0.02 μg/mL)

Substance

Recoveries/%

RSD/%

RT/min

Methamidophos

82.2

0.8

5.789

Acephate

76.4

6.4

7.152

Phorate

76.5

4.8

8.677

Omethoate

95.6

4.5

9.089

Diazinon

86.3

1.4

9.539

Dimethoate

85.5

16.5

11.273

Parathion-methyl

102.4

7.5

13.780

Chlorpyrifos

86.5

1.2

14.649

Malathion

99.2

6.2

15.073

Isofenphos-methyl

88.5

3.8

16.641

Isocarbophos

95.6

3.5

17.184

Triazophos

92.1

8.6

22.672

Phosalone

97.5

4.4

27.166

Phosmet

106.1

3.9

27.542

Table 2 Results of Organochlorine and Pyrethroid Pesticide Residues in apple using QuEChERS method by GC-ECD (spiked sample 0.02 μg/mL)

Substance

Recoveries/%

RSD/%

RT/min

α-BHC

84.8

13.8

5.715

γ-BHC

87.3

13.4

6.327

Pentachloronitrobenzene

83.5

11.0

6.425

Chlorothalonil

85.5

8.4

6.879

Traidimefon

91.7

3.9

8.518

Procymidone

93.6

2.6

9.388

O,P`DDE

89.5

2.4

9.603

P,P`DDE

92.3

1.1

10.179

O,P`DDD

94.0

2.3

10.333

P,P`DDD

95.3

2.6

10.934

Bifenthrin

95.0

1.0

12.572

Fenpropathrin

96.4

0.5

12.678

Cyhalothrin

99.3

3.6

13.537

Permethrin

95.5

0.1

14.349

Fenvalerate

94.7

0.9

16.529

β-BHC

81.3

25.9

6.216

δ-BHT

84.7

12.2

6.777

Vinclozolin

90.3

14.9

7.531

O,P`DDT

83.3

17.5

10.334

P,P`DDT (P,P`DDT)

81.6

18.7

10.935

Dicofol

83.9

17.7

11.781

Iprodione

77.3

31.4

12.336

Cyfluthrin

80.3

27.6

15.119

Flucythrinate

101.3

33.7

15.529

Tau-fluvalinate

92.7

8.6

17.002

Deltamethyrin

91.5

8.6

17.852

Table 3 Results of Carbamate Pesticide Residues in apple using QuEChERS method by LC-MS/MS (spiked sample 0.02 μg/mL)

Substance

Recoveries/%

RSD/%

Aldicarb sulfone

84.0

5.0

Methomyl

81.0

6.8

Aldicarb sulfoxide

75.0

4.3

Imidacloprid

80.0

7.1

3-hydroxycarbofuran

70.0

11.3

Aldicarb

70.0

4.7

Acetamiprid

70.0

6.8

Carbfuran

71.0

2.4

Fipronil

70.0

2.3

Carbaryl

70.0

10.1


Conclusion

This experiment establishes the QuEChERS method for detecting the pesticide residues in the apple, and detects the samples with standard addition (concentration: 0.1 μg/kg) on the basis of GC-LC MS-MS method. The resulted recovery rates are between 70% and 120%, conforming to the national standard requirements. The QuEChERS method is relatively stable, showing that this method can be applied to the preparation of pesticide residues in apple.

Order Information

Products

Specification

Cat.No

MAS-QuEChERS Extraction Kits

6 g MgSO4(Anhydrous), 1.5 g NaAc.3H2O with 50 mL   centrifuge tube

MS-MG5050

MAS-QuEChERS Cleanup Tube

400 mg C18, 400 mg PSA, 1200 mg MgSO4(Anhydrous),   with 15 mL centrifuge tube

MS-9PA1011

Syringe   Filter (Nylon)

0.22   μm, diameter 13 mm, 200/pk

AS021320

Disposable Syringe

2 mL, no needle

LZSQ-2ML

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

 

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