色谱

色谱 ›› 2010, Vol. 28 ›› Issue (10): 997-1000.DOI: 10.3724/SP.J.1123.2010.00997

• 技术与应用 • 上一篇    下一篇

高效液相色谱-串联质谱法测定鸡肉组织中癸氧喹酯残留

陈瑞清1,2, 俞道进1, 陈锋2, 黄一帆1*   

  1. 1. 福建农林大学动物科学学院, 福建 福州 350002; 2. 福建省农产品质量安全检验检测中心, 福建 福州 350003
  • 收稿日期:2010-07-01 修回日期:2010-08-18 出版日期:2010-10-28 发布日期:2010-10-28
  • 通讯作者: 黄一帆,教授,主要研究方向为天然药物研究与应用. E-mail: zjhyfang@163.com. 基金项目: 福建省科技重点项目(No. 2008Y0002).
  • 基金资助:

    无

Determination of decoquinate in chicken meat by high performance liquid chromatography-tandem mass spectrometry

CHEN Ruiqing1,2, YU Daojin1, CHEN Feng2, HUANG Yifan1*   

  1. 1. College of Animal Science, Fujian Agriculture and Forestry University, Fuzhou 350002, China; 2. Fujian Inspection and Testing Centre for Agricultural Product Quality and Safety, Fuzhou 350003, China
  • Received:2010-07-01 Revised:2010-08-18 Online:2010-10-28 Published:2010-10-28
  • Contact: CHEN Rui-Qing

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摘要： 建立了测定鸡肉组织中癸氧喹酯(DEC)残留的高效液相色谱-串联质谱(HPLC-MS/MS)方法。样品经乙腈提取,正己烷脱脂,固相萃取(SPE)小柱净化;采用0.1%甲酸乙腈溶液-0.1%甲酸水溶液(78:22, v/v)为流动相,电喷雾正离子电离(ESI+)模式,多反应监测(MRM)检测模式,以内标法进行定量。结果表明: DEC在1～200 μg/L范围内呈良好的线性关系,相关系数(r2)大于0.99; 1、10、100 μg/kg 3个添加水平的回收率为78.2%～107.4%,日内、日间相对标准偏差(RSD)均小于15%,方法检出限为0.25 μg/kg,定量限为0.5 μg/kg。该方法简便、灵敏、精确,可用于鸡肉组织中DEC药物残留的确证检测。

关键词: 残留, 高效液相色谱-串联质谱;癸氧喹酯, 鸡肉

Abstract: A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was developed for the determination of decoquinate (DEC) residue in chicken meat. The sample was extracted with acetonitrile, cleaned-up with hexane, and purified with solid phase extraction (SPE) cartridge. The mobile phase was acetonitrile (containing 0.1% formic acid) and water (containing 0.1% formic acid). The analyte was identified by positive electrospray ionization (ESI+) mode and multiple reaction monitoring (MRM) mode. The results showed as follows: The calibration curve showed good linearity within the concentrations of 1~200 μg/L with the correlation coefficient (r2)＞0.99. At the spiked levels of 1, 10 and 100 μg/kg, the recoveries of DEC were 78.2%~107.4%. The relative standard deviations (RSDs) of intra- and inter-days were both less than 15%. The limit of detection of DEC was 0.25 μg/kg and the limit of quantification was 0.5 μg/kg. The method is simple, sensitive and accurate in the determination of DEC residue, which can meet the requirements of the domestic and international legislations.

Key words: chicken meat, decoquinate, residue, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)