色谱

色谱 ›› 2018, Vol. 36 ›› Issue (4): 400-407.DOI: 10.3724/SP.J.1123.2017.11003

• 技术与应用 • 上一篇    下一篇

超高效液相色谱-串联质谱法同时检测动物组织中15种保水功能药物

刘洪斌1, 姚喜梅2, 田亚平1, 张鹭1, 蔡英华1, 姜艳彬1, 李颖1   

  1. 1. 中国动物疫病预防控制中心, 北京 102609;
    2. 中国标准化协会, 北京 100048
  • 收稿日期:2017-11-05 出版日期:2018-04-08 发布日期:2014-02-26
  • 通讯作者: 李颖,Tel:(010)59198901,E-mail:liying@163.com
  • 基金资助:

    “十二五”国家科技支撑重点项目（2014BAD13B05）.

Simultaneous determination of 15 water-holding functional drugs in animal tissues using ultra performance liquid chromatography-tandem mass spectrometry

LIU Hongbin1, YAO Ximei2, TIAN Yaping1, ZHANG Lu1, CAI Yinghua1, JIANG Yanbin1, LI Ying1   

  1. 1. China Animal Disease Control Center, Beijing 102609, China;
    2. China Association for Standardization, Beijing 100048, China
  • Received:2017-11-05 Online:2018-04-08 Published:2014-02-26
  • Supported by:

    Key Project in the National Science & Technology Pillar Program during the Twelfth Five-Year Plan Period (No. 2014BAD13B05).

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摘要：

建立了超高效液相色谱-串联质谱检测动物组织中15种保水功能药物残留的分析方法。样品经含1.0%（v/v）甲酸的乙腈溶液提取和Oasis PRiME HLB SPE柱净化后，采用Acquity UPLC BEH C18色谱柱（50 mm×2.1 mm，1.7 μm）分离，以甲醇和0.1%（v/v）甲酸水溶液为流动相进行梯度洗脱，在电喷雾电离（ESI）源、正离子模式下，采用MRM监测模式进行数据采集。在1.0~50.0 μg/kg范围内，15种保水功能药物的线性关系良好，相关系数均≥0.9949；定量限均低于1.0 μg/kg。通过添加回收试验表明，动物组织中15种保水功能药物的平均回收率为60.0%~111.0%，批内RSD为0.56%~11.5%，批间RSD为2.31%~14.8%。该方法满足动物组织中该药物多残留的检测要求，为应对动物源性食品中筛查风险隐患和监控非法添加提供了新思路。

关键词: 保水功能药物, 残留, 超高效液相色谱-串联质谱, 动物组织

Abstract:

A method based on ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed for the determination of 15 water-holding functional drugs in animal tissues.The analytes were extracted with acetonitrile containing 1.0%(v/v) methanol, purified by Oasis PRiME HLB SPE column, and analyzed by Acquity UPLC BEH C18 column (50 mm×2.1 mm, 1.7 μm) using methanol and 0.1%(v/v) formic acid aqueous solution as the mobile phases.The analytes were detected using an electrospray ionization (ESI) source under the MRM mode.The calibration curves of the analytes were linear in the range of 1.0-50.0 μg/kg (r ≥ 0.9949), and the limits of quantification were all less than 1.0 μg/kg in animal tissues.The recoveries of the 15 water-holding functional drugs ranged from 60.0%-111.0% in animal tissue samples, with the intra and inter RSDs of 0.56%-11.5% and 2.31%-14.8%, respectively.The method can meet the requirements for the determination of the drug residues in animal tissues.It provides a new idea to identify potential hazards in animal-derived foods and to monitor illegal addition.

Key words: animal tissues, residues, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), water-holding functional drugs

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