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Gas chromatography-tandem mass spectrometry detection method for clotrimazole residues in animal-derived food

A gas chromatography and tandem mass spectrometry technology, which is applied in the field of gas chromatography-tandem mass spectrometry detection of clotrimazole residues in animal-derived foods, can solve problems such as lack of substantial judgment basis, and achieve rapid extraction, good reproducibility, and extraction efficiency. high effect

Active Publication Date: 2020-03-17
ZHEJIANG SHUREN COLLEGE ZHEJIANG SHUREN UNIV
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Problems solved by technology

[0006] The current detection methods, through liquid chromatography and gas chromatography, can only be qualitatively and quantitatively determined by retention time and response peak area, lacking substantial basis for judgment

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  • Gas chromatography-tandem mass spectrometry detection method for clotrimazole residues in animal-derived food
  • Gas chromatography-tandem mass spectrometry detection method for clotrimazole residues in animal-derived food
  • Gas chromatography-tandem mass spectrometry detection method for clotrimazole residues in animal-derived food

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Embodiment Construction

[0028] The specific embodiments of the present invention will be described in further detail below in conjunction with the accompanying drawings.

[0029] The invention provides an accelerated solvent extraction-gel permeation chromatography purification-gas chromatography-tandem mass spectrometry detection method for clotrimazole residue in food of animal origin, comprising the following steps.

[0030] The extraction of step (1) sample, as figure 1 As shown, the chemical formula of clotrimazole is C 22 h 17 N 2 Cl: Weigh 3.0 g of the sample (animal muscle, fat and viscera) and transfer it to a ceramic mortar, add 60 μL of 1.0 μg / mL d5-clotrimazole standard solution, add 5 g of 60-mesh diatomaceous earth and grind it thoroughly, transfer the grinding A good sample was subjected to accelerated solvent extraction in a 10mL extraction cell. The extraction conditions were: extraction solvent cyclohexane / ethyl acetate (1:1, v / v), extraction temperature 100°C, heating for 5 minu...

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Abstract

The invention discloses a gas chromatography-tandem mass spectrometry detection method for clotrimazole residues in animal-derived food. According to the method, the clotrimazole residues in animal muscle, fat and viscera samples are extracted with a cyclohexane / ethyl acetate mixed solvent accelerated solvent, an extracting solution is purified through gel permeation chromatography and then detected in a gas chromatography-tandem mass spectrometry multi-reaction monitoring mode and quantification is conducted through an isotope internal standard method. Under optimized conditions, clotrimazolehas a good linear relationship within the range of 1.0-100 [mu] g / L, the correlation coefficient is 0.9995 and the limit of quantitation of the method is 1.0 [mu] g / kg. The average recovery rate of the method is 76.5%-107.4% and the relative standard deviation is not greater than 6.2%. The method is high in extraction efficiency, good in purification effect, high in sensitivity and good in repeatability and can be used for measuring the residual quantity of clotrimazole in animal muscles, fat and viscera.

Description

technical field [0001] The invention relates to the field of food safety detection, and relates to accelerated solvent extraction-gel permeation chromatography purification-gas chromatography-tandem mass spectrometry, and specifically refers to a gas chromatography-tandem mass spectrometry detection method for clotrimazole residues in animal source foods. Background technique [0002] Clotrimazole is an imidazole antifungal drug. Studies have shown that the use of clotrimazole as an antifungal drug during animal feeding may cause clotrimazole residues in the muscle, fat or viscera of some animals. However, my country's current Ministry of Agriculture Announcement No. 235 "Maximum Residue Limits of Veterinary Drugs in Animal Foods" has no regulations on the use limits of such antifungal agents including clotrimazole, and the published regulations and testing standards have not involved Clotrimazole. The newly promulgated GB 2763.1-2019 "National Food Safety Standard Maximum R...

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/14
CPCG01N30/02G01N30/06G01N30/14G01N2030/062G01N2030/146
Inventor 韩超胡贝贞叶明立沈燕付长春魏云潇王婷婷
Owner ZHEJIANG SHUREN COLLEGE ZHEJIANG SHUREN UNIV
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