基质分散固相萃取-液相色谱-串联质谱法检测动物源性食品中硝基咪唑药物及其代谢物

引用本文: 方力, 邱凤梅, 余新威, 张志超. 基质分散固相萃取-液相色谱-串联质谱法检测动物源性食品中硝基咪唑药物及其代谢物[J]. 色谱, 2018, 36(5): 431-438. doi: 10.3724/SP.J.1123.2017.12028 shu

Citation: FANG Li, QIU Fengmei, YU Xinwei, ZHANG Zhichao. Determination of nitroimidazoles and their metabolites in animal-derived foods by liquid chromatography-tandem mass spectrometry coupled with dispersive solid phase extraction[J]. Chinese Journal of Chromatography, 2018, 36(5): 431-438. doi: 10.3724/SP.J.1123.2017.12028 shu

基质分散固相萃取-液相色谱-串联质谱法检测动物源性食品中硝基咪唑药物及其代谢物

1.
浙江省海产品健康危害因素关键技术研究重点实验室, 舟山市疾病预防控制中心, 浙江舟山 316021;
2.
岱山县疾病预防控制中心, 浙江岱山 316200
基金项目:
舟山市科技计划项目（2017B31127）；舟山市医药卫生科技计划项目（2017A01）；国家星火计划项目（2015GA700094）.

摘要: 建立了基质分散固相萃取-液相色谱-串联质谱（dSPE-LC-MS/MS）定量检测4种动物源性食品基质中硝基咪唑类药物及其代谢物的方法。样品（2.0 g）用乙酸乙酯提取后浓缩，经正己烷脱脂、50 mg乙二胺-N-丙基硅烷（PSA）吸附剂吸附净化后，过0.22 μm亲水聚四氟乙烯（PTFE）滤膜。采用C18柱分离，在电喷雾电离（ESI）源和选择反应监测（SRM）模式下检测，基质匹配内标法定量。在0.5~20.0 μg/L范围内，硝基咪唑类药物及其代谢物呈现良好的线性关系，相关系数（r²）>0.99；方法的检出限为0.1~0.5 μg/kg；在1.0、3.0和10.0 μg/kg的加标水平下，硝基咪唑类药物及其代谢物的回收率为84.2%~120.8%，相对标准偏差为2.0%~16.2%（n=6）。该法准确、快速，成本低，易操作，能够满足动物源性食品中硝基咪唑类药物及其代谢物残留的监测要求。

关键词:

English

Determination of nitroimidazoles and their metabolites in animal-derived foods by liquid chromatography-tandem mass spectrometry coupled with dispersive solid phase extraction

1.
Key Laboratory of Health Risk Factors for Seafood of Zhejiang Province, Zhoushan Municipal District Center for Disease Control and Prevention, Zhoushan, 316021, China;
2.
Daishan Center for Disease Control and Prevention, Daishan, 316200, China
Received Date: 28 December 2017
Fund Project:
Science and Technology Plan Project of Zhoushan (No. 2017B31127)

Abstract: A method for the quantitative analysis of nitroimidazoles and their metabolites in four kinds of animal-derived foods by liquid chromatography-tandem mass spectrometry (LC-MS/MS) coupled with dispersive solid phase extraction (dSPE) was established. The samples (2.0 g) were extracted with ethyl acetate. The extracts were degreased with hexane and purified with 50 mg primary-secondary amine (PSA), and then filtered through a hydrophilic polytetrafluoroethylene (PTFE) membrane. The analytes were separated on a C18 column, and detected in selected reaction monitoring (SRM) mode via positive electrospray ionization. The matrix matching and internal standard method was used. The nitroimidazoles and their metabolites showed good linearity in the range of 0.5-20.0 μg/L with correlation coefficients greater than 0.99. The limits of detection of the nitroimidazoles and their metabolites in animal-derived foods were between 0.1 and 0.5 μg/kg. The recoveries varied between 84.2% and 120.8%, with relative standard deviations (n=6) ranging from 2.0% to 16.2% at spiked levels of 1.0, 3.0, and 10.0 μg/kg. The proposed method is accurate, fast, cheap, easy, and can satisfy the requirements of monitoring nitroimidazoles and their metabolites in animal-derived foods.

Key words:

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1.
沈阳化工大学材料科学与工程学院沈阳 110142

基质分散固相萃取-液相色谱-串联质谱法检测动物源性食品中硝基咪唑药物及其代谢物

English

Determination of nitroimidazoles and their metabolites in animal-derived foods by liquid chromatography-tandem mass spectrometry coupled with dispersive solid phase extraction

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

基质分散固相萃取-液相色谱-串联质谱法检测动物源性食品中硝基咪唑药物及其代谢物

English

Determination of nitroimidazoles and their metabolites in animal-derived foods by liquid chromatography-tandem mass spectrometry coupled with dispersive solid phase extraction

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

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CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

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CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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