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动物源食品中代谢物丙硫菌唑-去硫的农药残留分析方法

Approach for Pesticide Residue Analysis for Metabolite Prothioconazole-desthio in Animal Origin Food.

作者信息

Liu Hui, Yao Guojun, Liu Xueke, Liu Chang, Zhan Jing, Liu Donghui, Wang Peng, Zhou Zhiqiang

机构信息

Department of Applied Chemistry and Beijing Advanced Innovation Center for Food Nutrition and Human Health, China Agricultural University , Yuanmingyuan West Road 2, Beijing 100193, People's Republic of China.

出版信息

J Agric Food Chem. 2017 Mar 22;65(11):2481-2487. doi: 10.1021/acs.jafc.7b00062. Epub 2017 Mar 13.

Abstract

Food safety problems such as damage to immune, nervous, and endocrine systems leading to cancer and malformations have received increasing attention. To achieve the maximum residue limits, the most discussed method of high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) is widely used with a advantage of high precision and resolution. Prothioconazole is a broad-spectrum thiocarbamate fungicide. It can rapidly metabolize to prothioconazole-desthio in different matrixes. Rapid and effective methods for the determination of prothioconazole-desthio in five kinds of different animal food were developed. Samples were extracted with acetonitrile or acetonitrile/water and determined by HPLC-MS/MS. The limit of detection and limit of quantification values of prothioconazole-desthio were 0.015 and 0.05 mg/kg for porcine liver and kidney, 0.0015 and 0.005 mg/kg for pork, and 0.003 and 0.01 mg/kg for eggs, together with 0.0012 and 0.004 mg/kg for milk of the detected method, respectively. A good linear regression trend can be observed in a certain concentration range for all of the animal food. At fortified levels, recoveries were between 83.6 and 105%, with relative standard deviations of 1.5-10.3%. A sample survey of 150 samples with 30 samples for each kind of animal food across the country was conducted and found that there was no prothioconazole-desthio detected in all samples.

摘要

食品安全问题,如对免疫、神经和内分泌系统造成损害,进而导致癌症和畸形,已受到越来越多的关注。为实现最大残留限量,人们最常讨论的高效液相色谱 - 串联质谱法(HPLC-MS/MS)因具有高精度和高分辨率的优势而被广泛使用。丙硫菌唑是一种广谱硫代氨基甲酸酯类杀菌剂。它能在不同基质中迅速代谢为去硫丙硫菌唑。本文建立了快速有效的方法来测定五种不同动物食品中的去硫丙硫菌唑。样品用乙腈或乙腈/水提取,然后通过HPLC-MS/MS进行测定。该检测方法中,猪肝和猪肾中去硫丙硫菌唑的检出限和定量限分别为0.015和0.05mg/kg,猪肉中为0.0015和0.005mg/kg,鸡蛋中为0.003和0.01mg/kg,牛奶中为0.0012和0.004mg/kg。在一定浓度范围内,所有动物食品均呈现出良好的线性回归趋势。在加标水平下,回收率在83.6%至105%之间,相对标准偏差为1.5% - 10.3%。对全国范围内150份样品(每种动物食品30份)进行了抽样调查,结果发现所有样品中均未检测到去硫丙硫菌唑。

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