建立了超高效液相色谱-四极杆-飞行时间质谱（UPLC-Q-TOF/MS）快速筛查畜禽类产品中50种违禁药物残留的检测方法。畜禽类产品经β-葡萄糖醛酸酶/芳基硫酸酯酶酶解，依次用乙酸乙酯-叔丁基甲醚提取后，利用HLB净化，采用UPLC-Q-TOF/MS电喷雾正离子模式检测。通过建立在线谱库检索的方法实现50种违禁药物的快速筛选和准确定性，再结合同位素内标法实现准确定量。目标物质量浓度在2~200 μg/L范围内线性关系良好，相关系数均大于0.99，检出限为0.1~0.5 μg/kg，定量限为0.3~1.5 μg/kg，三个不同浓度的加标回收率在81.74%~114.22%之间，相对标准偏差为1.41%~8.91%。研究建立的筛查数据库在无需标准品的情况下实现了50种违禁药物的快速筛查、定性确证和定量分析。该方法适用于畜禽类产品中低浓度的违禁药物残留量的快速筛查和准确定量。

A method for quick screening of 50 illegal drugs in livestock by ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry (UPLC-Q-TOF/MS) had been established. Livestock products were first hydrolyzed by β-glucuronidase/arylsulfatase, then extracted with ethyl acetate-methyl tert-butyl ether, purified by HLB, and determined by UPLC-Q-TOF/MS in positive ion mode. A high-resolution database was established for quick screening and accurate characterization. Precise quantification by isotope internal standard method can be achieved. The correlation coefficient of the calibration curves of each illegal drugs standards exceeded 0.99 in the range of 2~200 μg/L. The detection limit of various drugs could reach 0.1~0.5 μg/kg, and the limit of quantification was 0.3~1.5 μg/kg. The average recovery at three different concentration levels varied from 81.74% to 114.22%, and the relative standard deviation was 1.41%~8.91%. The established database realizes the quick screening and analysis of 50 illegal drugs without the need for standard products. This method is suitable for quick screening and simultaneous determination of low-concentration residues in livestock products.

浙江省市场监管局科技计划项目（20210126）；浙江省基础公益研究计划分析测试项目（LGC19C200001）；国家市场监督管理总局技术保障专项项目（2019YJ020）