液相色谱-四极杆/静电场轨道阱质谱快速筛查和确证畜禽肉及水产品中160种兽药残留  

Rapid screening and confirmation of 160 veterinary drugs in livestock and poultry meat and aquatic products by liquid chromatography-quadrupole/orbitrap mass spectrometry

作　　者：谢瑜杰 仝凯旋 彭涛[1] 吴兴强[1] 于晓萱 门雪 范春林[1] 陈辉[1] XIE Yujie;TONG Kaixuan;PENG Tao;WU Xingqiang;YU Xiaoxuan;MEN Xue;FAN Chunlin;CHEN Hui(Chinese Academy of Inspection&Quarantine,Key Laboratory of Food Quality and Safety for State Market Regulation,Beijing 100176,China)

机构地区：[1]中国检验检疫科学研究院,国家市场监管重点实验室(食品质量与安全),北京100176

出　　处：《分析试验室》2023年第6期748-759,共12页Chinese Journal of Analysis Laboratory

基　　金：中国检科院基本科研业务费项目(2020JK010)资助。

摘　　要：应用液相色谱-四极杆/静电场轨道阱质谱(LC-Q-Orbitrap/MS)建立了畜禽肉及水产品中磺胺类、喹诺酮类、四环素类等14类160种兽药残留快速筛查方法。均浆后的样品(猪、鸡、鱼)中加入80%(V/V)乙腈-水溶液(含0.2%(V/V)甲酸)振荡提取,Oasis PRiME HLB固相萃取柱净化,在全扫描/数据依赖二级质谱扫描(Full MS/dd-MS2)模式下采集,基质匹配外标法定量。结果表明,160种兽药在0.25~100μg/L范围内线性关系良好,线性相关系数(R2)≥0.99,方法筛查限(SDL)和定量限(LOQ)均为0.5~20μg/kg。除敌敌畏、卡巴氧和二嗪磷回收率低于60%外,其余兽药在猪肉、鸡肉和鱼肉中1倍、 2倍和10倍定量限3个加标水平下的总体回收率为65.0%~119.6%,相对标准偏差(RSD)为0.73%~20%。方法应用于75批市售畜禽肉及水产品检测,共筛查出6类8种兽药。本方法可同时筛查畜禽肉及水产品中多种兽药残留。A method had been developed for the simultaneously screening and determination of 14 types of 160veterinary drugs,including sulfonamides,quinolones and tetracyclines in livestock and poultry meat and aquatic products by liquid chromatography-quadrupole/orbitrap mass spectrometry(LC-Q-Orbitrap/MS).The homogenized samples(including pork,chicken and fish)were extracted using 80%(V/V)acetonitrile-water solution(with 0.2%(V/V)formic aid)and purified using Oasis PRiME HLB solid phase extraction column.The residues were analyzed by Full MS/dd-MS2 mode and quantified by external standard with matrix matched method.The results showed that satisfactory linearities were achieved for 160 veterinary drugs in the concentration ranges of 0.25-100μg/L with the coefficients greater than 0.99.Both the screening detection limits(SDLs)and limits of quantification(LOQs)were 0.5-20μg/kg.The recoveries of target compounds(excluding dichlorvos,carbamox and diazinon)in pork,chicken and fish at spiked levels of LOQ,2×LOQ and 10×LOQ ranged from 65.0%to 119.6%,with the relative standard deviations(RSDs)ranging from 0.73%-20%.The method was applied to determine 75 real samples,and 6 types of 8 veterinary drugs were detected.This method could be applied to simultaneously screen 160 veterinary drug residues in livestock and poultry meat and aquatic products.

关 键 词：畜禽肉 水产品 兽药 多残留分析 液相色谱-四极杆/静电场轨道阱质谱 筛查 确证 

分 类 号：O657.63[理学—分析化学] TS252.7[理学—化学]