色谱

色谱 ›› 2012, Vol. 30 ›› Issue (05): 463-467.DOI: 10.3724/SP.J.1123.2012.01020

• 研究论文 • 上一篇    下一篇

液相色谱-串联质谱法检测畜禽产品中维吉尼亚霉素M1和S1残留

邱元进*, 杨方, 刘正才, 林永辉, 刘素珍   

  1. 福建出入境检验检疫局, 福建 福州 350001
  • 收稿日期:2012-01-13 修回日期:2012-03-13 出版日期:2012-05-28 发布日期:2012-06-07
  • 通讯作者: 邱元进,硕士,工程师. Tel: (0591)87065545, E-mail: yjqiuzju@163.com.
  • 基金资助:

    福建省科技攻关重点项目(2010Y0001)和国家质检总局科研项目(2009IK143).

Determination of virginiamycin M1 and S1 residues in livestock and poultry products by liquid chromatography-tandem mass spectrometry

QIU Yuanjin*, YANG Fang, LIU Zhengcai, LIN Yonghui, LIU Suzhen   

  1. Fujian Entry-Exit Inspection and Quarantine Bureau, Fuzhou 350001, China
  • Received:2012-01-13 Revised:2012-03-13 Online:2012-05-28 Published:2012-06-07
  • Contact: Yuan-Jin QIU

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摘要： 建立了畜禽产品中维吉尼亚霉素M1和S1药物残留检测的液相色谱-串联质谱分析方法。样品以甲醇-乙腈溶液(1:1, v/v)提取,上清液经0.01 mol/L磷酸二氢铵溶液稀释后,Oasis HLB固相萃取小柱净化,Luna C18色谱柱分离,以乙腈和含0.1%(体积分数)甲酸的5 mmol/L乙酸铵水溶液作为流动相进行梯度洗脱,电喷雾正离子模式电离(ESI+),多反应监测(MRM)模式检测,外标法定量。该方法对两物质线性范围均为0.15～10.0 μg/L,相关系数r2均大于0.999;定量下限均为0.25 μg/kg。在不同基质中,0.25、0.50、2.5 μg/kg3个添加水平的平均回收率范围为71.2%～98.4%,精密度范围为3.6%～15.4%。该方法具有快速简便、灵敏度高、准确性强等特点,适用于畜禽产品中维吉尼亚霉素的检测。

关键词: 残留, 维吉尼亚霉素M1, 维吉尼亚霉素S1, 畜禽产品, 液相色谱-串联质谱(LC-MS/MS)

Abstract: A liquid chromatography-tandem mass spectrometry method was established for the determination of virginiamycin M1 and S1 residues in livestock and poultry products. The sample was extracted by methanol-acetonitrile solution (1:1, v/v). The supernatant was diluted with 0.01 mol/L ammonium dihydrogen phosphate solution, then purified and concentrated on an Oasis HLB cartridge. The separation of virginiamycin M1 and S1 was performed on a Luna C18 column with the mobile phases acetonitrile and 5 mmol/L ammonium acetate aqueous solution (containing 0.1% (v/v) formic acid) in a gradient elution mode. The identification and quantification of the drugs were carried out by positive electrospray ionization (ESI+) in the multiple reaction monitoring (MRM) mode using external standard method. The calibration curves showed good linearity in the range of 0.15~10.0 μg/L with correlation coefficients (r2) above 0.999. The limits of quantities (LOQs) were both 0.25 μg/kg. The average recoveries of the two drugs spiked at 0.25, 0.5 and 2.5 μg/kg levels in different matrices were between 71.2% and 98.4%, and the relative standard deviations (RSDs) were between 3.6% and 15.4%. The method is simple, rapid, sensitive and accurate. It is suitable for the confirmation and quantification of virginiamycin M1 and S1 residues in livestock and poultry products.

Key words: livestock and poultry, residue, virginiamycin M1, virginiamycin S1, liquid chromatography-tandem mass spectrometry (LC-MS/MS)