色谱

色谱 ›› 2013, Vol. 31 ›› Issue (12): 1161-1166.DOI: 10.3724/SP.J.1123.2013.08022

• 研究论文 • 上一篇    下一篇

超高效液相色谱-串联质谱法同时测定鸡肉中的二氯二甲吡啶酚、磺胺类和喹诺酮类药物残留

宋伟1, 胡艳云1,2, 韩芳2, 吕亚宁2, 郑屏1,2, 周芳芳3, 陈晓妹1, 邱静2, 周晓莹2   

  1. 1. 安徽出入境检验检疫局技术中心, 安徽 合肥 230022;
    2. 食品安全分析与检测安徽省重点实验室, 安徽 合肥 230022;
    3. 安徽农业大学茶与食品科技学院, 安徽 合肥 230022
  • 收稿日期:2013-08-13 修回日期:2013-09-03 出版日期:2013-12-28 发布日期:2013-12-05
  • 通讯作者: 胡艳云
  • 基金资助:

    安徽省科技攻关项目（12010402c205）

Simultaneous determination of clopidol, sulfonamide and quinolone residues in chickens by ultra performance liquid chromatography-tandem mass spectrometry

SONG Wei1, HU Yanyun1,2, HAN Fang2, LV Yaning2, ZHENG Ping1,2, ZHOU Fangfang3, CHEN Xiaomei1, QIU Jing2, ZHOU Xiaoying2   

  1. 1. Technical Center of Anhui Entry-Exit Inspection and Quarantine Bureau, Hefei 230022, China;
    2. Anhui Province Key Laboratory of Analysis and Detection for Food Safety, Hefei 230022, China;
    3. College of Tea & Food Science and Technology, Anhui Agricultural University, Hefei 230022, China
  • Received:2013-08-13 Revised:2013-09-03 Online:2013-12-28 Published:2013-12-05

PDF

317

被引次数

17

摘要：

采用超高效液相色谱-串联质谱（UPLC-MS/MS）在正离子模式下通过多反应监测（MRM）方式同时测定了鸡肉组织中二氯二甲吡啶酚、磺胺嘧啶、磺胺二甲基嘧啶、磺胺对甲氧嘧啶、磺胺甲氧哒嗪、诺氟沙星、氧氟沙星、环丙沙星、恩诺沙星等9种药物残留。试样经乙腈均质提取，冷冻离心脱脂，旋转蒸发浓缩，用流动相复溶后经乙腈饱和的正己烷除油，随后进行UPLC-MS/MS定性定量分析。该方法测定9种药物的检出限为0.1 μg/kg，定量限为0.5 μg/kg。在添加水平分别为0.5、1.0和2.0 μg/kg时，9种药物的加标回收率为81.5%~97.6%，相对标准偏差（RSD）为2.1%~8.9%。该方法简便、准确，可作为鸡肉中9种药物残留检测的确证方法。

关键词: 超高效液相色谱-串联质谱法, 多残留, 二氯二甲吡啶酚, 磺胺, 鸡肉, 喹诺酮

Abstract:

An analytical method for the simultaneous determination of clopidol, sulfadiazine, sulfamethazine, sulfametoxydiazine, sulfamethoxypyridazine, norfloxacin, ofloxacin, ciprofloxacin, enrofloxacin in chickens by ultra performance liquid chromatography coupled with tandem quadrupole mass spectrometry (UPLC-MS/MS) in positive ion mode with multiple reaction monitoring (MRM) has been developed and validated. The samples were homogenized and extracted with acetonitrile. After defatted with high speed frozen centrifugation, the supernatant solution was evaporated and the residue was dissolved with the mobile phase and defatted with n-hexane. It was then analyzed with UPLC-MS/MS. The limit of detection of this method was 0.1 μg/kg, and the limit of quantification was 0.5 μg/kg. The average recoveries (spiked at the levels of 0.5, 1.0, 2.0 μg/kg) ranged from 81.5% to 97.6%, with the relative standard deviations between 2.1% and 8.9%. The results demonstrated that the method is simple, accurate and suitable for the identification and quantification of these drug residues in chickens.

Key words: chicken, clopidol, multiresidue, quinolonens, sulfonamides, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

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