色谱

色谱 ›› 2018, Vol. 36 ›› Issue (5): 431-438.DOI: 10.3724/SP.J.1123.2017.12028

• 研究论文 • 上一篇    下一篇

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

方力1, 邱凤梅2, 余新威1, 张志超1   

  1. 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
  • 收稿日期:2017-12-28 出版日期:2018-05-08 发布日期:2014-03-21
  • 通讯作者: 方力.E-mail:fangli123@126.com
  • 基金资助:

    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）.

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

FANG Li1, QIU Fengmei2, YU Xinwei1, ZHANG Zhichao1   

  1. 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:2017-12-28 Online:2018-05-08 Published:2014-03-21
  • Supported by:

    Science and Technology Plan Project of Zhoushan (No. 2017B31127); Medical and Health Science and Technology Plan Project of Zhoushan (No. 2017A01); National Spark Program Project (No. 2015GA700094).

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被引次数

1

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: 动物源性食品, 基质分散固相萃取, 硝基咪唑及其代谢物, 液相色谱-串联质谱

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: animal derived foods, dispersive solid phase extraction (dSPE), liquid chromatography-tandem mass spectrometry (LC-MS/MS), nitroimidazoles and their metabolites

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