液相色谱-串联质谱法测定猪组织中58种兽药残留  

Determination of 58 Veterinary Drugs Residues in Pig Tissues by Liquid Chromatography-Tandem Mass Spectrometry

作　　者：熊增星 刘青 连琦 张文中 胡文斌 XIONG Zengxing;LIU Qing;LIAN Qi;ZHANG Wenzhong;HU Wenbin(Jiangxi Institute of Food Inspection and Testing,Nanchang 330001;SCIEX China,Shanghai 200233)

机构地区：[1]江西省食品检验检测研究院,南昌330001 [2]上海爱博才思分析仪器贸易有限公司,上海200233

出　　处：《食品工业》2022年第5期272-277,共6页The Food Industry

摘　　要：建立QuEChERS净化超高效液相色谱-串联质谱法同时检测猪的多种组织中58种常见禁用兽药残留的分析方法。样品经80%乙腈水溶液提取,Qu ECh ERS分散固相萃取净化。采用Waters Acquity UPLC HSS T_(3)(100 mm×2.1 mm,1.7μm)色谱柱分离,以乙腈和0.1%甲酸水(含5 mmol/L乙酸铵)作为流动相洗脱,质谱采用电喷雾正离子模式扫描及多反应监测采集方式(MRM)监测,外标法定量。结果表明,58种化合物在1.0~00.0 ng/m L浓度范围内线性关系良好,相关系数均大于0.99,方法检出限在0.3~1.5μg/kg之间,定量限在1.0~5.0μg/kg之间。分别在1.0,2.0和5.0μg/kg水平下进行三梯度加标试验,平均回收率为63.9%~130.6%,相对标准偏差为(S;,n=6)为0.08%~10.15%。该方法具有操作简便、检验过程快速、灵敏度高、结果可靠、重现性好等特点,适用于猪组织中多种兽药残留量的快速筛查。An ultra-performance liquid phase-tandem mass spectrometry(UPLC-MS/MS)method was developed for simultaneous determination of 58 veterinary drugs residues in multiple pig tissues.The samples were extracted by 80%acetonitrile solution,and the extracts were purified on QuEChERS dispersive solid-phase.The 58 veterinary drugs were analyzed by Waters Acquity UPLC HSS T3(100 mm×2.1 mm,1.7μm)using acetonitrile and 0.1%formic acid(contain 5mmol/L ammonium acetate)as the mobile phases,electrospray source positive ion scanning and retention time-dependent multiple reaction monitoring mode(MRM)detection,external standard method for quantification.The results showed that there was a good linear relationship between 58 veterinary drugs in the linear range of 1.0-100.0 ng/mL,with the correlation coefficients all greater than 0.99.The detection limits were 0.3-1.5μg/kg,and the quantification limits were 1.0-5.0μg/kg.The average recovery rates were 63.9%-130.6%and the relative standard deviations(SRSD,n=6)form 0.08%to 10.15%at the three standard levels of 1.0,2.0 and 5.0μg/kg.The method was simple,less time consumption and sensitive,and the results are reliable and reproducible.The method was successfully used for rapid screening of various veterinary drug residues in pig tissues.

关 键 词：QuEChERS净化 超高效液相色谱-串联质谱法 猪组织 禁用兽药残留 快速筛查 

分 类 号：O657.63[理学—分析化学] TS251.7[理学—化学]