通过式固相萃取结合超高效液相色谱-四极杆/静电场轨道阱高分辨质谱快速筛查畜禽肉中108种兽药残留  

Rapid Screening and Confirmation of 108 Kinds of Veterinary Drug Residues in Livestock and Poultry Meat by Solid Phase Extraction Purification and Liquid Chromatography Coupled with Quadrupole/Orbitrap Mass Spectrometry

作　　者：郭添荣 万渝平 孙利[2] 叶梅 许森 韩世鹤 吴文林 GUO Tian-Rong;WAN Yu-Ping;SUN Li;YE Mei;XU Sen;HAN Shi-He;WU Wen-Lin(Chengdu Institute of Food Inspection,Chengdu 611130,China;Chinese Academy of Inspection and Quarantine,Beijing 100176,China;Shanghai Key Laboratory of Functional Materials Chemistry,East China University of Science and Technology,Shanghai 200237,China;Chengdu Institute of Biology,Chinese Academy of Sciences,Chengdu 610041,China)

机构地区：[1]成都市食品检验研究院,成都611130 [2]中国检验检疫科学研究院,北京100176 [3]华东理工大学上海市功能性材料化学重点实验室,上海200237 [4]中国科学院成都生物研究所,成都610041

出　　处：《分析化学》2022年第2期271-277,共7页Chinese Journal of Analytical Chemistry

基　　金：国家市场监督管理总局技术保障专项项目(No.2021YJ009);四川省科技计划应用基础研究项目(No.21YYJC0962);成都市技术创新研发项目(No.2021-YF05-00811-SN)资助。

摘　　要：采用通过式固相萃取消减样品中杂质干扰,基于超高效液相色谱-四极杆/静电场轨道阱高分辨质谱(UHPLC-Q/Orbitrap HRMS)联用技术建立了同时快速筛查畜禽肉中108种兽药残留的分析方法。样品匀质后,经乙腈溶液(80%,V/V,含0.2%甲酸)提取,Oasis PRiME HLB固相萃取柱通过式净化,氮吹后复溶。采用Agilent Eclipse plus C_(18)色谱柱(150 mm×3.0 mm,1.8μm)分离,以乙腈和20 mmol/L乙酸铵溶液(含0.1%甲酸)体系为流动相进行梯度洗脱,加热电喷雾离子源正负离子同时扫描模式,一级全扫描/数据依赖二级扫描(Full MS/dd-MS^(2))监测模式检测,基质匹配标准曲线法定量。结果表明,108种兽药在0.5~2000 ng/mL范围内线性关系良好,相关系数(R)≥0.9950;方法检出限(LOD)为0.1~20μg/kg,定量限(LOQ)为0.2~100μg/kg;不同畜禽肉在3个添加水平下(n=6)的加标回收率在68.7%~112.5%之间,相对标准偏差(RSD)在0.9%~9.7%之间。本方法简便快捷、覆盖目标物广、通量高且准确可靠,适用于畜禽肉中兽药多残留的快速筛查与确证分析。An analytical strategy for simultaneous and rapid screening of 108 kinds of veterinary drug residues in livestock and poultry meat was established by using solid-phase extraction(SPE)to reduce impurity interference in samples and based on ultra-high performance liquid chromatography-quadrupole/orbitrap high resolution mass spectrometry(UHPLC-Q/Orbitrap HRMS).The homogenized samples were extracted by 80%acetonitrile aqueous solution(containing 0.2%formic acid),purified by Oasis PRiME HLB solid phase extraction column,and redissolved by nitrogen blowing.The target analytes were separated from the samples by an Agilent Eclipse plus C_(18)(3.0 mm×150 mm,1.8μm)chromatographic column,with acetonitrile and 0.1%acetic acid-ammonium formate(20 mmol/L)aqueous solution system as the mobile phase in gradient elution.Under the heated electrospray ionization positive and negative ions simultaneous scan mode,the target analytes were analyzed by the full scan of primary mass spectrometry plus data-dependent secondary mass spectrometry(Full MS/dd-MS^(2)),and quantitatively detected by a matrix matching quantitative standard curve method.The results showed that 108 kinds of veterinary drugs had a good linear relationship in the range of 0.5-2000 ng/mL,and the correlation coefficients(R)were over 0.9950.The limits of detection(LODs)were 0.1-20μg/kg,and the limits of quantitation(LOQs)were 0.2-100μg/kg.The standard recoveries of different livestock and poultry meat under three levels of addition(n=6)were 68.7%-112.5%,and the relative standard deviation(RSDs)were 0.9%-9.7%.This method was simple,rapid and accurate,with wide coverage and high-throughput,and was suitable for rapid screening and confirmative analysis of veterinary drug residues in livestock and poultry meat.

关 键 词：畜禽肉 兽药残留 通过式固相萃取 四极杆/轨道阱高分辨质谱 快速筛查 

分 类 号：O657.63[理学—分析化学] TS251.7[理学—化学]