Li Rong, Yang Luqi, Zhang Pengyun, Luo Yangdan, Zhang Pengjie, Gao Yongqing
Inspection and Quarantine Technology Center, Zhongshan Entry-Exit Inspection and Quarantine Bureau, Zhongshan 528400, China.
School of Food Science, Guangdong Pharmaceutical University, Zhongshan 528458, China.
Se Pu. 2017 Dec 8;35(12):1266-1275. doi: 10.3724/SP.J.1123.2017.08021.
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/ddMS) 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.
已开发出一种使用超高效液相色谱-四极杆/静电场轨道阱高分辨率质谱同时测定水产品中64种兽药的方法。样品用乙腈/水混合液(80/20,v/v)萃取,经乙腈饱和正己烷和伯仲胺(PSA)吸附剂净化,采用外标法进行定量。药物在全扫描/数据依赖质谱2(Full MS/ddMS)Top 1模式下进行分析。64种药物的校准曲线呈线性,相关系数大于0.9967。64种分析物在三种基质(鱼、虾和贝类)中的三个添加水平下的平均回收率为56.2%至124.6%,相对标准偏差(RSD)为1.3% - 29.8%。定量限为0.2 - 10 μg/kg。该方法简便、快速、灵敏、可靠,适用于水产品中残留的筛查。