色谱

色谱 ›› 2017, Vol. 35 ›› Issue (10): 1062-1067.DOI: 10.3724/SP.J.1123.2017.06029

• 研究论文 • 上一篇    下一篇

液相色谱-串联质谱法测定猪肉中咪唑类药物及其代谢物

杨旺火, 吴少明, 蔡小明, 冯丽凤, 陈言凯, 李燕平, 梁敏   

  1. 福建省产品质量检验研究院, 国家加工食品质量监督检验中心, 福建 福州 350002
  • 收稿日期:2017-06-28 出版日期:2017-10-08 发布日期:2017-10-18
  • 通讯作者: 杨旺火,Tel:(0591)83762015,E-mail:wujifeijinshuywh@126.com.

Determination of imidazoles and their metabolites in pork by liquid chromatography-tandem mass spectrometry

YANG Wanghuo, WU Shaoming, CAI Xiaoming, FENG Lifeng, CHEN Yankai, LI Yanping, LIANG Min   

  1. National Quality Supervision and Testing Center for Processed Food, Fujian Inspection and Research Institute for Product Quality, Fuzhou 350002, China
  • Received:2017-06-28 Online:2017-10-08 Published:2017-10-18

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摘要：

建立了高效液相色谱-串联质谱同时测定猪肉中29种咪唑类药物及其代谢物残留的检测方法。样品采用乙酸乙酯提取，浓缩复溶后加入乙腈饱和正己烷净化除脂，以0.3%（体积分数）甲酸水溶液和乙腈为流动相，反相C18色谱柱梯度洗脱分离，采用电喷雾正离子（ESI+）源多反应监测（MRM）模式进行检测。29种化合物在0.05~20.0 μg/L范围内线性关系良好，相关系数r2＞0.99。在1.0~5.0 μg/kg添加范围内，平均回收率为65.4%~103%，相对标准偏差（RSD）为1.3%~6.8%。方法检出限为0.02~0.3 μg/kg，定量限为0.1~1 μg/kg。该方法简便、快速、灵敏，适用于猪肉中咪唑类及其代谢物残留的检测。

关键词: 残留, 咪唑类药物, 液相色谱-串联质谱, 猪肉

Abstract:

A method for the determination of 29 imidazoles and their metabolites in pork by liquid chromatography-tandem mass spectrometry has been developed. The samples were extracted with ethyl acetate, and then defatted with n-hexane after concentration of the extracts. The analytes were separated on a C18 reversed-phase column with 0.3% (v/v) formic acid aqueous solution and acetonitrile as mobile phases, and finally analyzed using electrospray ionization in positive ion mode (ESI+) with multiple reaction monitoring (MRM). The linear ranges of the 29 compounds were from 0.05 to 20.0 μg/L with the correlation coefficients (r2) more than 0.99. The average recoveries and relative standard deviations were 65.4%-103% and 1.3%-6.8% respectively in the spiked ranges of 1.0-5.0 μg/kg. The limits of detection and the limits of quantification were 0.02-0.3 μg/kg and 0.1-1 μg/kg respectively for the 29 imidazoles. The method is simple, rapid and sensitive. It is suitable for the detection of imidazoles and their metabolites in pork.

Key words: imidazoles, liquid chromatography-tandem mass spectrometry (LC-MS/MS), pork, residue

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