Method for determining endosulfan in feed by gas chromatography-tandem mass spectrometry

A technology of tandem mass spectrometry and gas chromatography, which is applied in the detection field of pretreatment and gas chromatography-tandem mass spectrometry, can solve the problems of few reports on the detection of endosulfan, and achieve the effect of simple operation, economical process and strong universal applicability

Inactive Publication Date: 2018-05-15
淮安出入境检验检疫局综合技术服务中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The detection of endosulfan in many methods is aimed at the matrix of tea, vegetables, fruits and aquatic products, but there are few reports on the detection of endosulfan in feed matrix

Method used

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  • Method for determining endosulfan in feed by gas chromatography-tandem mass spectrometry
  • Method for determining endosulfan in feed by gas chromatography-tandem mass spectrometry
  • Method for determining endosulfan in feed by gas chromatography-tandem mass spectrometry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Example 1: Detection of 10 μg / Kg level addition blank feed sample

[0020] (1) Sample pretreatment steps: Take the feed pulverizer and crush it, pass it through a 0.25mm aperture (60 mesh) sieve, mix it thoroughly and put it into a grinding bottle for later use; accurately weigh 20g (accurate to 0.01g) of the crushed feed sample to In a 100 mL homogenizing cup, add 10 μg / Kg level standard, add 40 mL chromatographically pure acetonitrile and homogenize for 2 min; transfer the liquid to a funnel for filtration, take 10 mL of the filtrate and blow it to dryness with nitrogen in a test tube , add 1mL n-hexane to be purified; add 2 cm high anhydrous Na to the SPE cartridge 2 SO 4 , activated with 3mL n-hexane-acetone solution (volume ratio 10:1, the same below); transfer the concentrated solution to a small column, and then wash the nitrogen blowpipe with 2mL n-hexane-acetone solution 2~3 times each time, and wash The liquid was transferred into the column, eluted with 8 m...

Embodiment 2

[0024] (1) Sample pretreatment steps: Accurately weigh 25 g (accurate to 0.01 g) of crushed feed samples into a 100 mL homogenizing cup, add 50 mL of chromatographically pure acetonitrile and homogenize for 2 min; transfer the liquid to a funnel for filtration, and take Spin 10 mL of the filtrate in a 50 mL pear-shaped flask to dryness with a rotary evaporator, add 1 mL of n-hexane for purification; add 1 cm high anhydrous Na 2 SO 4 , activated with 2 mL n-hexane-acetone solution (volume ratio 10:1, the same below); transfer the concentrated solution to a small column, and wash the nitrogen blowpipe with 2 mL n-hexane-acetone solution 2 to 3 times each time, and place The washing solution was transferred to the column, and eluted with 10 mL of n-hexane-acetone solution. The filtrate was spun to dryness with a rotary evaporator, and the volume of n-hexane was adjusted to 1 mL, and passed through a 0.22 μm needle-type nylon filter membrane in a chromatographic injection bottle f...

Embodiment 3

[0026] Example 3: Detection of some feed samples

[0027] (1) Sample pretreatment steps: Take the feed and crush it with a pulverizer, pass it through a 0.25mm aperture (60 mesh) sieve, mix it thoroughly and put it into a grinding bottle for later use; accurately weigh 30g (accurate to 0.01g) of the crushed feed sample To a 100 mL homogeneous cup, add 60 mL of chromatographically pure acetonitrile and homogenize for 2 min; transfer the liquid to a funnel for filtration, take 10 mL of the filtrate and blow it to dryness with nitrogen in a test tube, add 2 mL of n-hexane to be purified; SPE small column Add 2 cm height of anhydrous Na 2 SO 4, activated with 3 mL n-hexane-acetone solution (volume ratio 10:1, the same below); transfer the concentrated solution to a small column, and then wash the nitrogen blowpipe with 2 mL n-hexane-acetone solution 2~3 times each time, and place Transfer the washing solution into the column, elute with 12 mL of n-hexane-acetone solution, blow t...

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Abstract

The invention discloses a method for determining endosulfan in a feed by gas chromatography-tandem mass spectrometry. The method comprises the following steps of pretreating a sample, and detecting; weighing a certain amount of sample, extracting the endosulfan in the sample by using an organic solvent (chromatographic pure acetonitrile) as an extracting agent, concentrating by a nitrogen blowinginstrument, purifying the concentrated liquid by a Florisil diatomite SPE (solid-phase extraction) column, and using the gas chromatography-tandem mass spectrometry to perform qualitative and quantitative treatment. The method has the advantages that the organic solvent (chromatographic pure acetonitrile) is used as the extracting agent, and the sample is concentrated, and purified by the Florisildiatomite SPE column, so that the pretreatment is simple and convenient, and the consumption time is short; the gas chromatography-tandem mass spectrometry adopts a MRM (multiple reaction monitoring)mode to determine, so that the sensitivity and precision are high, and the qualitative and quantitative treatment is accurate; the universality is strong, the method is suitable for the feed sampleswith different proportional ratios, and the requirement of quickly separating and detecting the endosulfan in the feed sample can be met.

Description

technical field [0001] The invention relates to a method for determining the pesticide residue endosulfan in feed, in particular to the pretreatment of the complex matrix of feed and the detection method of gas chromatography-tandem mass spectrometry. Background technique [0002] With the development of the livestock and poultry industry, the production of feed has also increased significantly, and the quality of feed production has also attracted much attention. Every year, the export volume of livestock and poultry products is affected by pesticide and veterinary drug residues. The raw materials of feed mainly come from crops, so the pesticide residues in feed are the main factors causing pesticide residues in livestock and poultry products. Pesticide residues in feed not only have toxic, teratogenic, and carcinogenic effects on livestock and poultry, but also enter the human body through livestock and poultry products and endanger health. Controlling pesticide residues...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 何正和魏云计何健朱臻怡秦娴冯民
Owner 淮安出入境检验检疫局综合技术服务中心
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