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Method for determining fipronil and fipronil metabolite residual quantity in eggs

A technology for medium fipronil and residues, which is applied in the field of physical and chemical detection of pesticide residues, can solve problems such as egg samples that have not yet been used, and achieve the effects of high extraction efficiency, simple processing operations and high degree of automation

Inactive Publication Date: 2017-08-11
AGRI PRODS PROCESSING RES INST CHINESE ACAD OF TROPICAL AGRI SCI
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Problems solved by technology

[0004] At present, there is no liquid chromatography-tandem mass spectrometry method for the simultaneous determination of fipronil and its metabolites in eggs in China. The literature reports mainly include gas chromatography, gas-mass spectrometry, and liquid-mass spectrometry for the determination of one of the pesticides. Simultaneous determination of fipronil and its metabolites in eggs by high performance liquid chromatography tandem mass spectrometry has not been reported
In the foreign literatures that have been reported, gas chromatography-mass spectrometry (GC / MS) was used to detect fipronil in vegetables, but it has not been used in egg samples

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  • Method for determining fipronil and fipronil metabolite residual quantity in eggs
  • Method for determining fipronil and fipronil metabolite residual quantity in eggs

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Embodiment 1

[0033] Example 1 Using the method of the present invention, the residual amounts of fipronil, flupronil, fipronil sulfone and fipronil sulfoxide in 5 egg samples were determined respectively according to the following steps:

[0034] (1) Sample preparation: 5 egg samples were minced and homogenized, and frozen at -18°C to obtain frozen samples;

[0035] (2) Sample pretreatment: Accurately weigh 2 g of the homogenized egg sample in step (1), place it in a 50 mL polypropylene centrifuge tube, add 5 mL of acetonitrile as the crude extract, homogenize for 1 min, shake for 10 min, and place in a 50 mL polypropylene centrifuge tube. Centrifuge at 8000 r / min at 4°C, extract the supernatant into a chicken heart bottle to obtain the extract; repeat the extraction once with 5 mL of acetonitrile for the precipitate, combine the two extracts, add 2 mL of isopropanol, and place in a rotary evaporator Concentrate at 50°C until nearly dry to obtain a concentrated solution; add 2.0mL of a mix...

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Abstract

The invention relates to a method for determining fipronil and fipronil metabolite residual quantity in eggs. The method for determining the fipronil and fipronil metabolite residual quantity in eggs comprises the steps of sample preparation; sample pretreatment; organic solvent extraction; pigment impurity removal through a solid phase extraction column, wherein nitrogen is blown to be almost dry, residues are dissolved through a mobile phase, and the solution is filtered through a filter membrane for UPLC-TQD analysis; standard solution preparation; high performance liquid chromatography-tandom mass spectrometer determination and the like. The method is easy to implement, rapid, high in automatic degree, high in extraction efficiency, good in recovery and repeatability and capable of simultaneously determining the fipronil and fipronil metabolite residual quantity in eggs.

Description

technical field [0001] The invention relates to a method for determining fipronil and its metabolite residues in eggs, in particular to a high-performance liquid chromatography-tandem mass spectrometer method for determining four pesticide residues in eggs, and belongs to the technical field of physical and chemical detection of pesticide residues. Background technique [0002] In recent years, with the development of my country's national economy, people's requirements for food safety and quality have gradually increased in their daily lives. However, as far as the current social situation is concerned, food safety accidents still occur from time to time. Food safety is a major issue related to the national economy and the people's livelihood. It is the most basic health issue related to everyone, and it is the core link of the future development of the food industry. Therefore, it is particularly important to strengthen the detection of various chemical substances in food ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/72G01N30/06G01N30/12G01N30/34
Inventor 郭宏斌杨春亮叶剑芝林玲
Owner AGRI PRODS PROCESSING RES INST CHINESE ACAD OF TROPICAL AGRI SCI
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