Gas chromatography-negative chemical source-tandem mass spectrometry detection method for fipronil and metabolite amide fipronil of fipronil in bird egg

A technology of product amide fipronil and mid-fipronil, which is applied to the detection of fipronil and its metabolite amide fipronil in poultry eggs. In the field of poultry eggs, it can solve the problems of cumbersome pretreatment and poor anti-interference ability , to achieve the effect of ensuring accuracy and good recovery rate

Inactive Publication Date: 2018-09-14
韩超
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Problems solved by technology

[0005] The existing literature reports on the determination of fipronil residues mainly include gas chromatography (GC), gas chromatography-single quadrupole mass spectrometry (GC-MS), and liquid chromatography-tandem mass spectrometry (LC-MS-MS). GC and GC-MS methods have poor anti-interference ability and cumbersome pre-treatment

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  • Gas chromatography-negative chemical source-tandem mass spectrometry detection method for fipronil and metabolite amide fipronil of fipronil in bird egg
  • Gas chromatography-negative chemical source-tandem mass spectrometry detection method for fipronil and metabolite amide fipronil of fipronil in bird egg
  • Gas chromatography-negative chemical source-tandem mass spectrometry detection method for fipronil and metabolite amide fipronil of fipronil in bird egg

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[0041] Depend on Figure 1 to Figure 12 It can be seen that the present invention discloses a gas chromatography-negative chemical source-tandem mass spectrometry detection method for fipronil and its metabolite amide fipronil in poultry eggs, comprising the following steps:

[0042] (1) Extraction of the sample to be tested: Weigh 5.0-10.0g poultry egg sample, then add 10mL acetonitrile and extract homogeneously for 1min at a centrifugation speed of 15000r / min, then add QuEChERS salting-out bag and shake vigorously to mix, and then add 10000r / min After centrifuging at a high speed for 1 min, extract the supernatant, add extractant to the remaining solution, repeat the above steps and combine the obtained supernatant, place the obtained supernatant in a 40°C water bath and concentrate under reduced pressure until dry, and finally add 1.0-2.0mL acetonitrile to reconstitute dissolved to obtain the liquid to be purified;

[0043] (2) Purification of the solution to be purified: ...

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Abstract

The invention discloses a gas chromatography-negative chemical source-tandem mass spectrometry detection method for fipronil and a metabolite amide fipronil of the fipronil in a bird egg. By means ofthe method, the residual amounts of the fipronil and the metabolite amide fipronil of the fipronil in the bird egg can be accurately determined. Acetonitrile is added into a bird egg sample to extracta target and obtain to-be-purified liquid, the to-be-purified liquid is subjected to liquid-liquid partition degreasing through n-hexane and purification through a matrix dispersion purification tube, qualitative analysis is conducted on the target under a monitoring mode of a gas chromatography-negative chemical source-tandem mass spectrometer according to retention time and ion pair informationcomparison, and quantification is conducted through an internal standard method. The method is high in analysis speed, high in sensibility and good in reproducibility and accuracy, and the novel detection method is provided for guaranteeing the bird egg quality safety.

Description

technical field [0001] The invention belongs to the field of food testing and relates to QuEChERS extraction and purification-gas chromatography-negative chemical source-tandem mass spectrometry (GC-NCI-MS / MS), specifically referring to a kind of fipronil and its metabolite amide fipronil in poultry eggs Nitrile detection method, especially for poultry eggs such as eggs. Background technique [0002] Fipronil is a new type of highly active phenylpyrazole insecticide with broad-spectrum insecticidal effect. It was widely used in my country in the late 1990s. Animal studies have shown that long-term ingestion of fipronil may damage the liver, thyroid, and kidneys. Fipronil can generate more toxic fipronil, fipronil sulfide, fipronil sulfone and amide fipronil through photolysis, reduction, oxidation, and hydrolysis in the environment. [0003] The Codex Alimentarius Commission (CAC) stipulates that the residue limit of fipronil and its metabolites in eggs is 0.02 mg / kg, and ...

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/72
CPCG01N30/02G01N30/72
Inventor 韩超胡贝贞侯建波陈瑶沈燕周秀锦陈祥准
Owner 韩超
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