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Method for determining chlorantraniliprole residues in vegetables

A technology for the determination of chlorantraniliprole and its determination method, which is applied in the field of determination of chlorantraniliprole residues in vegetables by high performance liquid chromatography-tandem mass spectrometry, which can solve the problem of high requirements for sample purification, difficult determination of samples, solvent Consumption and other problems, to achieve the effect of easy analysis of large batches of samples, reduce analysis costs, and reduce analysis time

Inactive Publication Date: 2018-11-13
辽宁通正检测有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although liquid chromatography is mature and easy to promote, it consumes a lot of solvents and costs a lot, and the first three methods have high requirements for sample purification, and it is difficult to measure samples with complex matrices. Simple, qualitative and quantitative accuracy, high sensitivity, low purification requirements, etc., therefore, the quantitative and qualitative detection of chlorantraniliprole in vegetables by high performance liquid chromatography-tandem mass spectrometry is of great significance

Method used

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  • Method for determining chlorantraniliprole residues in vegetables
  • Method for determining chlorantraniliprole residues in vegetables
  • Method for determining chlorantraniliprole residues in vegetables

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0078] Example 1: Determination of Chlorantraniliprole Residues in Cabbage

[0079] The detection limit of this method is 0.001mg / kg.

[0080] Sample pretreatment:

[0081] Weigh 15g (accurate to 0.01g) of the prepared cabbage sample in a centrifuge tube with a stopper as a blank sample, and weigh 15g (accurate to 0.01g) of a prepared cabbage sample in a stoppered centrifuge tube as a spiked sample (respectively Add 15ng, 150ng standard substance), accurately add 15mL of acetonitrile, and then homogenize and extract at high speed on a homogenizer for 2 minutes, add 6.0g of anhydrous magnesium sulfate to dehydrate, 1.5g of sodium chloride for salting out, after vortexing and shaking, Centrifuge at 6000r / min for 5min, take 1.0mL supernatant to a 10mL volumetric flask, add 4mL acetonitrile and dilute to the mark with water, mix well and pass through a 0.22μm organic filter membrane, and use high performance liquid chromatography equipped with an electrospray ion source - Detect...

Embodiment 2

[0117] Embodiment 2: Determination of chlorantraniliprole residual amount in cucumber

[0118] The detection limit of this method is 0.001mg / kg.

[0119] Sample pretreatment:

[0120] Weigh 15g (accurate to 0.01g) of the prepared cucumber sample in a centrifuge tube with a stopper as a blank sample, and weigh 15g (accurate to 0.01g) of a prepared cucumber sample in a stoppered centrifuge tube as a spiked sample (respectively Add 500ng, 1000ng), accurately add 15mL of acetonitrile, homogenize and extract at high speed on a homogenizer for 2 minutes, add 6.0g of anhydrous magnesium sulfate to dehydrate, 1.5g of sodium chloride for salting out, after vortexing and shaking, use 6000r / min centrifuged for 5min, take 1.0mL supernatant to a 10mL volumetric flask, add 4mL acetonitrile and dilute to the mark with water, mix well and pass through a 0.22μm organic filter membrane. Mass spectrometer detection.

[0121] The ion chromatogram of the spiked sample with medium concentration...

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Abstract

The invention provides a method for determining chlorantraniliprole residues in vegetables. Acetonitrile is used to homogeneously extract chlorantraniliprole residues in a sample, anhydrous magnesiumsulfate is added to remove water, sodium chloride salting-out is carried out, a supernatant is obtained after whirling, oscillation and centrifugation, acetonitrile is added to the supernatant, wateris used for fixing the volume, the mixture is passed through a 0.22[mu]m filter membrane after uniform mixing, then the mixture is detected by a high performance liquid chromatography-tandem mass spectrometer equipped with an electrospray ion source and is monitored by multiple events in sections, then the mixture is quantified by an external standard method, and a standard series working curve isprepared with blank matrix liquid without components to be detected. According to the method, the addition recovery rate is between 97.6% and 117.9%, the average relative standard deviation (RSD) isbetween 1.5% and 6.0%, and when the addition detection limit is 0.001mg / kg, the signal-to-noise ratio of an instrument is greater than 3. Through verification, the method is simple, rapid and reliablein operation, accurate in qualitative and quantitative analysis, high in sensitivity, good in repeatability, and easy to realize analysis of a large batch of samples. The minimum limit value of chlorantraniliprole residues in vegetables in China is 0.01mg / kg, and the method meets this requirement.

Description

technical field [0001] The invention relates to the field of detection methods for pesticide residues in edible agricultural products. Specifically, high-performance liquid chromatography-tandem mass spectrometry is used to measure the residual amount of chlorantraniliprole in vegetables, and the purpose of simple and fast operation and accurate qualitative and quantitative results has been achieved. . The invention belongs to the technical field of determination of pesticide residues. Background technique [0002] Chlorantraniliprole is a new type of high-efficiency and broad-spectrum o-formamidobenzamide insecticides. It can control various non-Lepidoptera pests such as Coleoptera Weevilidae, Chrysoopteridae; Diptera Liminidae; Bemisia tabaci and so on. Because the chemical structure of chlorantraniliprole has a new insecticidal principle that other insecticides do not have, it can efficiently activate insect fish muddy (muscle) receptors. Excessive release of calcium i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/72G01N30/06G01N30/14
CPCG01N30/02G01N30/06G01N30/14G01N30/72G01N2030/146G01N2030/042
Inventor 考志强王雪莹陈英续张进柏中波王应男张国莹
Owner 辽宁通正检测有限公司
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