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  

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

作　　者：李蓉 杨璐齐 张鹏云 罗阳丹 张朋杰 高永清 Li Rong;Yang Luqi;Zhang Pengyun;Luo Yangdan;Zhang Pengjie;Gao Yongqing

机构地区：[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

出　　处：《色谱》2017年第12期1266-1275,共10页Chinese Journal of Chromatography

基　　金：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)~~

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≥0.996 7),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0.2~10μg/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。A method has been developed for the simultaneous determination of64veterinary drugs in aquatic products using ultra-high performance liquid chromatography-quadrupole/lectrostatic field orbitrap high-resolution mass spectrometry.The samples were extracted with an acetonitri/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 spectrum2(Full MS/ddMS2)Top1mode.The calibration curves of the64drugs were linear with the correlation coefficients more than0.9967.The average recoveries of the64analytes ranged from56.2%to124.6%,and the relative standard deviations(RSDs)were1.3%-29.8%in the three kinds of matrixes(fish,shrimp and shell)at three levels.The limits of quantification were0.2-10pg/kg.The method issimple,rapid,sensitive,reliable and suitable for the screening of residues in aquatic products.

关 键 词：超高效液相色谱 高分辨质谱 兽药 水产品 残留 

分 类 号：O658[理学—分析化学]