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A kind of determination method of chlorantraniliprole residues in vegetables and fruits

A technology for chlorantraniliprole and a determination method is applied in the field of determination of chlorantraniliprole residues, can solve the problems of high price, restrict the application of LC-MS/MS, take a relatively long time, etc., and achieves simple and convenient operation, Avoid matrix interference, high sensitivity effect

Active Publication Date: 2016-03-30
郭庆龙
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In recent years, there have been many studies on the detection methods of chlorantraniliprole residues in various food and agricultural products. The detection methods reported all use liquid chromatography (LC) or liquid chromatography tandem mass spectrometry (LC-MS / MS) to determine the residues of vegetables and chlorantraniliprole. The detection method of cyantraniliprole residues in fruits, using LC-MS / MS to determine pesticide residues in food and agricultural products has the advantages of fast, simple, and high sensitivity, but due to its high price, many testing institutions, enterprises or research institutes have not equipped The number of instruments or configurations is small, because when different compounds are detected by LC-MS / MS, different mobile phases or chromatographic columns need to be used, which requires constant replacement of chromatographic columns and mobile phases and takes a long time to balance the system , which to some extent restricts the application of LC-MS / MS
Gas chromatography-mass spectrometry (GC-EI-MS) equipped with electron bombardment ionization source has great advantages in analyzing pesticide residues in food and agricultural products. Since electron bombardment ionization source mass spectrometry is a universal detector, it can realize multi-residue analysis of hundreds of pesticides. It can be qualitative and quantitative at the same time, and the price is moderate. Therefore, various testing institutions and enterprises are equipped with gas chromatography-electron bombardment ion source-mass spectrometer (GC-EI-MS) to detect pesticide residues in food and agricultural products, but so far no See the report of the GC-EI-MS detection method of chlorantraniliprole residue in vegetables and fruits, therefore, establish gas chromatography-electron bombardment ion source-mass spectrometry (GC-EI-MS) qualitative and quantitative analysis in vegetables and fruits The detection method of chlorantraniliprole residue is of great significance

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  • A kind of determination method of chlorantraniliprole residues in vegetables and fruits
  • A kind of determination method of chlorantraniliprole residues in vegetables and fruits
  • A kind of determination method of chlorantraniliprole residues in vegetables and fruits

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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 4mL of supernatant in a nitrogen blowpipe, dry it with nitrogen at 40°C, add 1mL of acetone / n-hexane mixed solvent with a volume ratio of 1 / 1 to dissolve the residue, vortex and mix evenly to pass through the membrane, then transfer it to an injection bottle for GC - EI-MS determination.

[0039] (2) Preparation of standard working solution

[0040] Accurately weigh 25±0.1mg of t...

Embodiment 2

[0066] Example 2: Detection of chlorantraniliprole residues in green beans

[0067] (1) Sample pretreatment

[0068] 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 an injection bottle for GC-EI - MS determination.

[0069] (2) Preparation of standard working solution

[0070] Dilute the 10μg / mL stan...

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Abstract

The invention discloses a method for measuring the residual amount of chlorantraniliprole in vegetables and fruits. The method disclosed by the invention comprises the following steps: homogenizing and extracting chlorantraniliprole residual in a sample by using acetonitrile or an acetonitrile solution containing 1% of acetic acid, dispersing and purifying an extraction solution through ethanediamine-N-propoxysilane (PSA) and an octadecylsilan bonded phase (C18), detecting through gas chromatography-electron impact ion source-mass spectrum (GC-EI-MS), establishing a corrected standard curve by using a vehicle solution free from a pesticide to be measured, and quantifying by using an external standard method. According to the invention, the average recovery rate is 89.6%-103.5%; the average relative standard deviation (RSD) is 4.4%-7.7%; the detection limit is less than 0.62 microgram / kg; and the method disclosed by the invention has the advantages of being simple, convenient and rapid to operate, high in sensitivity, good in repeatability and accurate in qualitative and quantitative performance, and can satisfy the technological requirements on safety detection of corresponding products in the countries, such as America, Japan, European union and Canada, and provide strong technical support for sound development of food safety and foreign export trade in China.

Description

technical field [0001] The invention relates to a method for determining the residual amount of chlorantraniliprole in vegetables and fruits, more specifically, it uses gas chromatography-electron bombardment ion source-mass spectrometry (GC-EI-MS) to qualitatively and quantitatively determine the residues in vegetables and fruits. The method for the content of chlorantraniliprole 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-chloropyridin-2-yl)-1H-...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88
Inventor 郭庆龙范昆余冬冬管旭芳
Owner 郭庆龙
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