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

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。

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

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.