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Detection method for residual amount of chlorantraniliprole in aquatic vegetables

A technology for chlorantraniliprole and aquatic vegetables, which is applied in measurement devices, instruments, material analysis by electromagnetic means, etc., to achieve the effects of cost saving, environmental pollution reduction and high efficiency

Inactive Publication Date: 2016-10-12
中华人民共和国淮安出入境检验检疫局
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there are many domestic and foreign reports on the detection of chlorantraniliprole residues in vegetables and fruits, mainly using high-performance liquid chromatography and liquid chromatography-mass spectrometry, and the pre-treatment extraction solvent is mainly acetonitrile or acidic acetonitrile. And there is no report yet about the method for the detection of chlorantraniliprole residues in aquatic vegetables

Method used

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  • Detection method for residual amount of chlorantraniliprole in aquatic vegetables
  • Detection method for residual amount of chlorantraniliprole in aquatic vegetables
  • Detection method for residual amount of chlorantraniliprole in aquatic vegetables

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Example 1: Detection of chlorantraniliprole residues in lotus root

[0054] Sample pretreatment

[0055] Weigh 10.00g lotus root sample (accurate to 0.05g) and place it in a plastic centrifuge tube with a stopper, add ethyl acetate: acetone (v / v 7:3) 20mL, sonicate for 10min, add 3g sodium chloride and mix well, 4000r / Centrifuge for 10 min, take the supernatant, add 0.1g of PSA powder and vortex, let it stand until the PSA powder settles, take 2mL of the supernatant, rotatively evaporate in a water bath at 45°C or blow with nitrogen to dryness, and accurately add 1.00mL of methanol: water mixed solution (V / V 3:7) After dissolving, pass through a 0.22 μm organic filter membrane into a sampling bottle for instrumental analysis.

[0056] Chromatograms such as figure 1 shown.

[0057] Liquid Chromatography Conditions

[0058] Chromatographic column: Agilent ZORBAX SB-C18 column 150mm×2.1mm (i.d.); mobile phase: A0.1% formic acid aqueous solution, B methanol, gradient e...

Embodiment 2

[0066] Example 2: Detection of chlorantraniliprole residues in cattail

[0067] Sample pretreatment

[0068] Weigh 10.00 g of cattail (accurate to 0.05 g) and place it in a plastic centrifuge tube with stopper, add 20 mL of ethyl acetate: acetone (v / v 7: 3), ultrasonicate for 10 min, add 3 g of sodium chloride and mix well, 4000 r / min centrifuge for 10min, take the supernatant and add 0.1g of PSA powder to vortex, let it stand until the PSA powder settles, take 2mL of the supernatant, rotatively evaporate in a water bath at 45°C or blow with nitrogen until dry, add 1.00mL of methanol: water to mix accurately After the solution (V / V 3:7) was dissolved, it was passed through a 0.22 μm organic filter membrane into a sampling bottle for instrumental analysis.

[0069] Such as figure 2 As shown in the chromatogram, the liquid chromatography conditions are the same as in Example 1, and the mass spectrometry conditions are the same as in Example 1.

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Abstract

The invention provides a detection method characterized by good stability and high sensitivity for the residual amount of chlorantraniliprole in aquatic vegetables. The method comprises the steps of: (1) preparation of a standard solution; (2) preparation of a solvent; (3) a pretreatment extraction process; and (4) determination: taking the filtrate obtained in step (1) and step (3) to conduct liquid chromatography-tandem mass spectrometry determination. The detection method for the residual amount of chlorantraniliprole in aquatic vegetables uses a mixed solvent of ethyl acetate and acetone (V / V 7:3) to extract chlorantraniliprole residue in aquatic vegetables, purification by a dispersive solid-phase extraction N-propyl ethylenediamine (PSA) adsorbent is conducted, and then the characteristics of strong selectivity and anti-interference capability of liquid chromatography-tandem mass spectrometry are utilized to determine the residual amount. By using the ethyl acetate:acetone (V / V 7:3) mixed solvent, the extraction efficiency is high, and little extraction matrix interference exists. By using the PSA filler as the adsorbent, the extracted organic acid, pigments and other interfering substances can be removed so as to achieve the purpose of purification.

Description

technical field [0001] The invention relates to a method for detecting residues in aquatic vegetables, in particular to a method for detecting residues of chlorantraniliprole in aquatic vegetables. Background technique [0002] Chlorantraniliprole is a new type of high-efficiency broad-spectrum insecticide developed by DuPont. It can also control Coleoptera Weevilidae, Chrysoplastidae; Diptera Liminidae; Bemisia tabaci and other non-lepidopteran pests. Chlorantraniliprole can efficiently activate insect ryanodine receptors and destroy cytoplasmic Ca 2+ The environment is stable, leading to paralysis and death of insects. It has high activity against larvae of Lepidoptera pests, and has the ability to quickly prevent pests from eating, high-efficiency retention activity, rain resistance, and strong permeability. [0003] At present, there are many domestic and foreign reports on the detection of chlorantraniliprole residues in vegetables and fruits, mainly using high-perfor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N27/62
CPCG01N27/62G01N30/02G01N2030/027
Inventor 魏云计冯民朱臻怡王小晋何健魏斌朱珠
Owner 中华人民共和国淮安出入境检验检疫局