色谱

色谱 ›› 2015, Vol. 33 ›› Issue (4): 354-362.DOI: 10.3724/SP.J.1123.2014.12005

• 研究论文 • 上一篇    下一篇

分散固相萃取-高效液相色谱-串联质谱法同时测定畜禽肉中63种兽药残留

罗辉泰1,2, 谢梦婷1, 黄晓兰1, 吴惠勤1, 朱志鑫1, 黄芳1, 林晓珊1, 欧阳钢锋2   

  1. 1. 中国广州分析测试中心, 广东省分析测试技术公共实验室, 广东 广州 510070;
    2. 中山大学化学与化学工程学院, 广东 广州 510275
  • 收稿日期:2014-12-02 修回日期:2015-01-07 出版日期:2015-04-08 发布日期:2015-03-30
  • 通讯作者: 黄晓兰
  • 基金资助:

    广州市科技计划项目(11BppZXcc6100034).

Multiresidue analysis of 63 veterinary drugs in meat by dispersive solid-phase extraction and high performance liquid chromatography-tandem mass spectrometry

LUO Huitai1,2, XIE Mengting1, HUANG Xiaolan1, WU Huiqin1, ZHU Zhixin1, HUANG Fang1, LIN Xiaoshan1, OUYANG Gangfeng2   

  1. 1. Guangdong Provincial Public Laboratory of Analysis and Testing Technology, China National Analytical Center (Guangzhou), Guangzhou 510070, China;
    2. School of Chemistry and Chemical Engineering, Sun Yat-sen University, Guangzhou 510275, China
  • Received:2014-12-02 Revised:2015-01-07 Online:2015-04-08 Published:2015-03-30

PDF

267

被引次数

26

摘要：

建立了分散固相萃取-高效液相色谱-串联质谱(dispersive-SPE-HPLC-MS/MS)同时测定畜禽肉中 β-内酰胺类、喹诺酮类、磺胺类、磺胺类增效剂和抗寄生虫类共5类63种兽药残留的新方法。样品经0.1 mol/L Na2EDTA溶液及含1% (体积分数)乙酸的乙腈溶液涡旋提取,提取液经C18分散固相萃取净化后,用Poroshell EC-C18色谱柱(100 mm×2.1 mm, 2.4 μm)分离,在电喷雾离子源正离子模式下以动态多反应监测(DMRM)方式采集数据并做定性筛查和定量分析。63种药物在相应的浓度范围内线性关系良好,相关系数均大于0.99;不同畜禽肉(猪肉、牛肉及鸡肉)在3个不同添加水平下的平均回收率为62.2%~112.0%,相对标准偏差(RSD)为3.1%~16.3%,检出限(LOD, S/N≥3)和定量限(LOQ, S/N≥10)分别为0.1~3.0 μg/kg和0.5~10.0 μg/kg。该方法简便快速、灵敏可靠,适用于畜禽产品中兽药多残留的同时快速定性筛查和定量分析。

关键词: β-内酰胺类兽药, 分散固相萃取, 高效液相色谱-串联质谱法, 磺胺类兽药, 磺胺类增效剂兽药, 抗寄生虫类兽药, 喹诺酮类兽药, 畜禽肉

Abstract:

A novel multiresidue analytical method has been developed and validated for the determination of five classes of veterinary drugs including 18 β-lactams, 15 quinolones, 21 sulfonamides, 3 sulfonamide potentiators and 6 antiparasitics in meat using dispersive solid-phase extraction (dispersive-SPE) and high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The analytes were extracted with a vortex mixer by 0.1 mol/L Na2EDTA solution and acetonitrile containing 1% (v/v) acetic acid, and then the extracts were purified using dispersive-SPE with C18 sorbent. Electrospray ionization mass spectrometry was operated in positive mode using dynamic multiple reaction monitoring (DMRM) for the qualitative and quantitative analysis of the 63 analytes after the separation on a Poroshell EC-C18 column (100 mm×2.1 mm, 2.4 μm). The correlation coefficients of linear calibration curves were over 0.99 in the corresponding concentration ranges. The average recoveries of the 63 analytes ranged from 62.2% to 112.0%, and the relative standard deviations (RSDs) were 3.1%-16.3% in spiked meat (pork, beef and chicken muscle) at three levels. The limits of detection (LODs, S/N≥3) and the limits of quantification (LOQs, S/N≥10) were 0.1-3.0 μg/kg and 0.5-10.0 μg/kg, respectively. The method is simple, rapid, sensitive, reliable and suitable for the determination of residues in animal products.

Key words: β-lactam drugs, antiparasitic drugs, dispersive solid-phase extraction (dispersive-SPE), high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), meat, quinolone drugs, sulfonamide drugs, sulfonamide potentiator drugs

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