候美玲*，董宪兵，李红丽，吴彦蕾
（重庆市食品药品检验检测研究院，重庆 400020）
摘要：本文建立了超高效液相色谱-串联质谱法（UPLC-MS/MS）同时检测畜禽肉中4类抗生素及镇定剂类兽药残留。样品经酸化乙腈提取，正己烷去油脂后，过固相萃取柱净化，氮吹后用20%甲醇定容，经ACQUITY UPLC HSST3柱分离，正负离子多反应监测采集数据，同位素内标法定量。实验结果表明，29种兽药在0.5-200 ng/mL范围内线性关系良好，相关系数r在0.993以上，检出限为0.5-5.0 μg/kg，分别进行低、中、高三水平加标实验，平均回收率为63.2-112.7%，相对标准偏差RSD为2.2-14.2%（n＝6），该方法简单、高效、成本低，适用于日常检测工作。
关键词：畜禽肉；超高效液相色谱-串联质谱法；抗生素；镇静剂
中图分类号：TS207.3 文献标识码：A 文章编号：1674-506X（2020）03-0113-0005
Simultaneous Determination of Antibiotics and Tranquilizers Veterinary Drugs Residues in Livestock and Poultry Meat by Ultra High Performance Liquid Chromatography-tandem Mass Spectrometry
HOU Mei-ling*, DONG Xian-bin, LI Hong-li, WU Yan-lei
（Chongqing Institute for Food and Drug Control, Chongqing 400020, China）
Abstract：A method was established to rapidly determine veterinary drugs residues including four categories of antibiotics and tranquilizersin livestock and poultry meat by ultra high performance liquid chromatography-tandem mass spectrometry. The samples were extracted by acidification acetonitrile, degreased by n-hexane, purified by solid phase extraction column, fixed volume by 20% methanol after nitrogen blowing, separated by acquity UPLC HSS T3 column, monitored and collected data by multi reaction of positive and negative ions, and quantified by isotope internal standard method.. The 29 veterinary drugs showed a good linear relationship in the range of 0.5- 200 ng/mL (r＞0.993). The limits detection of quantification were 0.5- 5.0 μg/kg, and 3 different concentrations (low, middle, high) were used in the experiment, the average recoveries of the three spiked levels ranged between 63.2% to 112.7% with the relative standard deviations (RSDs) of 2.2-14.2% (n＝6). This method has the advantages of simple operation, sensitivity and accuracy, suitable for simultaneous determination of qualitative and quantitative analysis of multiple veterinary residues in livestock and poultry.
Keywords：livestock and poultry; ultra-pressure liquid chromatography electrospray tandem mass spectrometry
(UPLC-MS/MS); antibiotics; tranquilizers
doi：10.3969/j.issn.1674-506X.2020.03-022
收稿日期：2019-12-30
基金项目：国家重点研发计划资助（2017YFC1602000）
作者简介：候美玲（1987-），女，硕士，中级工程师。研究方向：食品质量与安全。
*通讯作者
引文格式：候美玲,董宪兵,李红丽,等.超高效液相色谱-串联质谱法（UPLC-MS/MS）同时检测畜禽肉中抗生素及镇静剂类兽药残留[J].食品与发酵科技,2020,56(3):113-117,126.
