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A method for the determination of chlorantraniliprole residues in fruits and vegetables

A technology for the determination of chlorantraniliprole and its determination method, which is applied in the field of determination of chlorantraniliprole residues in fruits and vegetables, can solve the problems of low sensitivity of anti-interference ability, and achieve the goal of avoiding matrix interference, good repeatability and high sensitivity Effect

Inactive Publication Date: 2016-01-20
云南商测质量检验技术服务有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Now various testing institutions and enterprises have purchased gas chromatography-mass spectrometers (GC-MS), and are generally equipped with negative chemical ion sources (NCI). Now many types of pesticides contain electronegative groups, organochlorines and pseudo Pyrethrin pesticide molecules mostly contain strong electronegative groups such as -F, -Cl, -Br or -COO-; organophosphorus pesticide molecules mostly contain =S, -OR, -P, -O-, -Cl, or -P=O and other electronegative groups; and most of the new pesticides developed in recent years contain -F groups. Therefore, the use of GC-NCI-MS can facilitate the multi-residue analysis of various pesticides. Compared with MS, it can obtain better anti-interference ability, lower sensitivity and better selectivity. Chlorantraniliprole is an electronegative compound, but so far no chlorantraniliprole residues have been seen in vegetables and fruits The report of the GC-NCI-MS detection method of amount, therefore, the detection method of establishing gas chromatography-negative chemical ion source-mass spectrometry (GC-NCI-MS) qualitative and quantitative analysis of chlorantraniliprole residues in vegetables and fruits has important meaning

Method used

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  • A method for the determination of chlorantraniliprole residues in fruits and vegetables
  • A method for the determination of chlorantraniliprole residues in fruits and vegetables
  • A method for the determination of chlorantraniliprole residues in fruits and vegetables

Examples

Experimental program
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Effect test

Embodiment 1

[0036] Example 1: Detection of chlorantraniliprole residues in apples

[0037] (1) Sample pretreatment

[0038] Weigh 10.0 g of well-mixed apples into a 50 mL centrifuge tube, accurately add 20 mL of acetonitrile, homogeneously extract for 1 min, add 3 g of anhydrous magnesium sulfate and 2 g of sodium chloride, vortex for 1 min, and centrifuge at 7000 r / min for 5 min. After centrifugation, take 6mL of acetonitrile extract and transfer to a solution containing 900mg anhydrous magnesium sulfate, 300mgC 18 and 150mgPSA in a centrifuge tube, vortex for 1min, and centrifuge at 5000r / min for 5min. Take 4 mL of the supernatant in a nitrogen blowpipe, dry it with nitrogen at 40°C, add acetone / n-hexane mixed solvent with a volume ratio of 1 / 1 to dissolve the residue, vortex and mix evenly, pass through the membrane, and transfer it to the sample bottle for GC- NCI-MS assay.

[0039] (2) Preparation of standard working solution

[0040] Accurately weigh 25±0.1mg of the standard pro...

Embodiment 2

[0065] Example 2: Detection of chlorantraniliprole residues in green beans

[0066] (1) Sample pretreatment

[0067] Weigh 10.0 g of well-mixed green beans into a 50 mL centrifuge tube, accurately add 20 mL of acetonitrile solution containing 1% acetic acid, extract homogeneously for 1 min, add 3 g of anhydrous magnesium sulfate and 2 g of sodium acetate, vortex for 1 min, and 7000r / min Centrifuge for 5min. After centrifugation, take 6mL of acetonitrile extract and transfer to a solution containing 900mg anhydrous magnesium sulfate, 300mgC 18 and 150mgPSA in a centrifuge tube, vortex for 1min, and centrifuge at 5000r / min for 5min. Take 4mL of the supernatant in a nitrogen blowpipe, dry it with nitrogen at 40°C, add acetone / n-hexane mixed solvent with a volume ratio of 1 / 1 to dissolve the residue, vortex and mix well, then transfer it to the sample bottle to wait for GC-NCI - MS determination.

[0068] (2) Preparation of standard working solution

[0069] Dilute the 10μg / ...

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Abstract

The invention discloses a method for measuring the residual quantity of chlorantraniliprole in fruit and vegetable. The method comprises performing homogeneous extraction on chlorantraniliprole residue in a sample through acetonitrile or an acetonitrile solution containing 1% of acetic acid; performing dispersed purification on extracted solution through ethylenediamine-N-propyl silicane (PSA) and octadecyl silane bonded phase (C18) matrix; then performing gas chromatograph-negative chemical ionization-mass spectrometry (GC-NCI-MS) detection, establishing a calibration standard curve through blank matrix solution not containing pesticide to be measured, and performing quantitation through the external standard method. The method for measuring the residual quantity of the chlorantraniliprole in fruit and vegetable achieves an average recovery rate of 90.7-101.9%, an average relative standard deviation (RSD) of 5.4-9.6% and a detection limit lower than 0.77 mu g / kg, has the advantages of being convenient and rapid to operate, high in sensitivity and repeatability and accurate in quantitation and quantification, can meet the technical requirements of the corresponding product safety inspection of nations such as the U.S., Japan, the European Union and Canada, and provides powerful technical support for food safety of people and healthy development of export trade in China.

Description

technical field [0001] The invention relates to a method for determining the residual amount of chlorantraniliprole in fruits and vegetables, more specifically, the qualitative and quantitative determination of residual chlorine in vegetables and fruits by gas chromatography-negative chemical ion source-mass spectrometry (GC-NCI-MS) The invention discloses a method for the content of benzamide, which belongs to the technical field of determination of pesticide residues. Background technique [0002] Chlorantraniliprole (Chlorantraniliprole), trade name Kang Kuan, is a new type of o-formamidobenzamide insecticide developed by DuPont. Mothidae, Fruit Mothidae, Leaf Rolleridae, Melydidae, Plutella Plutella, Graciidae, Thymothidae, etc. all have very good control effects, and can also control Coleoptera Weevilidae and Chromophyidae; Muscidae; Bemisia tabaci and other non-Lepidoptera pests. The chemical name is: 3-bromo-N-[4-chloro-2-methyl-6-[(methylcarbamoyl)benzene]-1-(3-chl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88
Inventor 郭庆龙许美玲董丽君韩井伟
Owner 云南商测质量检验技术服务有限公司
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