色谱

色谱 ›› 2017, Vol. 35 ›› Issue (12): 1266-1275.DOI: 10.3724/SP.J.1123.2017.08021

• 研究论文 • 上一篇    下一篇

超高效液相色谱-四极杆/静电场轨道阱高分辨质谱同时检测水产品中64种兽药残留

李蓉1, 杨璐齐1,2, 张鹏云1, 罗阳丹1, 张朋杰1, 高永清2   

  1. 1. 中山出入境检验检疫局检验检疫技术中心, 广东 中山 528400;
    2. 广东药科大学食品科学学院, 广东 中山 528458
  • 收稿日期:2017-08-28 出版日期:2017-12-08 发布日期:2017-12-15
  • 通讯作者: 李蓉,Tel:(0760)88830078,E-mail:lirong828@126.com;高永清,Tel:(0760)88207955,E-mail:yongqingg@163.com
  • 基金资助:

    广东省省级科技计划项目（2015A050502010，2014A040401011）；国家质检总局科技计划项目（2015IK260）；中山市社会公益重大专项（2015B2295）.

Determination of 64 veterinary drug residues in aquatic products by ultra-high performance liquid chromatography-quadrupole/electrostatic field orbitrap high-resolution mass spectrometry

LI Rong1, YANG Luqi1,2, ZHANG Pengyun1, LUO Yangdan1, ZHANG Pengjie1, GAO Yongqing2   

  1. 1. Inspection and Quarantine Technology Center, Zhongshan Entry-Exit Inspection and Quarantine Bureau, Zhongshan 528400, China;
    2. School of Food Science, Guangdong Pharmaceutical University, Zhongshan 528458, China
  • Received:2017-08-28 Online:2017-12-08 Published:2017-12-15
  • Supported by:

    Science and Technology Planning Project of Guangdong Province of China (Nos. 2015A050502010, 2014A040401011); Science and Technology Planning Project of General Administration of Quality Supervision Inspection and Quarantine of the People's Republic of China (No. 2015IK260); Social Public Welfare Major Project of Zhongshan City (No. 2015B2295).

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摘要：

建立了同时测定水产品中64种兽药残留的超高效液相色谱-四极杆/静电场轨道阱高分辨质谱分析方法。样品经乙腈-水溶液（80：20，v/v）提取，经乙腈饱和的正己烷和乙二胺-N-丙基硅烷（PSA）吸附剂净化。使用可加热电喷雾（HESI）离子源，全扫描/数据依赖二级扫描（Full MS/ddMS2）Top 1模式检测，外标法定量。结果表明，64种兽药在各自的浓度范围内线性关系良好（r2 ≥ 0.9967），在3种水产品基质（鱼、虾、贝类）中3个不同浓度加标水平的平均回收率为56.2%~126.4%，相对标准偏差为1.3%~29.8%，方法的定量限为0.2~10 μg/kg。该方法简便、准确、灵敏，适用于批量水产品中多种兽药残留的快速筛查。

关键词: 残留, 超高效液相色谱, 高分辨质谱, 兽药, 水产品

Abstract:

A method has been developed for the simultaneous determination of 64 veterinary drugs in aquatic products using ultra-high performance liquid chromatography-quadrupole/electrostatic field orbitrap high-resolution mass spectrometry. The samples were extracted with an acetonitrile/water mixture (80/20, v/v), cleaned up by normal hexane saturated with acetonitrile and primary secondary amine (PSA) adsorbent, quantified with external standard method. The drugs were analyzed in full scan/data dependent mass spectrum 2 (Full MS/ddMS2) Top 1 mode. The calibration curves of the 64 drugs were linear with the correlation coefficients more than 0. 9967. The average recoveries of the 64 analytes ranged from 56.2% to 124.6%, and the relative standard deviations (RSDs) were 1.3%-29.8% in the three kinds of matrixes (fish, shrimp and shell) at three levels. The limits of quantification were 0.2-10 μg/kg. The method is simple, rapid, sensitive, reliable and suitable for the screening of residues in aquatic products.

Key words: aquatic products, high-resolution mass spectrometry (HRMS), residue, ultra-high performance liquid chromatography (UHPLC), veterinary drug

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