本文研究了用液相色谱串联飞行时间质谱建立生乳中29 种兽药残留的快速检测方法。生乳样品采用0.2%甲酸乙腈溶液提取上清液,采用Dikma ProElut QuECHERS净化管净化后测定。目标化合物通过Waters ACQUITY UPLC HSS T3色谱柱分离,以乙腈和1.0%甲酸水溶液为洗脱剂进行程序洗脱,正离子扫描模式检测。结果表明,通过对数据进行靶向分析,20.0 min内生乳中29 种兽药残留能够同时被检测出来,其中Mass Error在±2.0 mg/kg之内,Library Score得分均在90 分以上,准确性高,操作简便。

The aim of this study was to establish a rapid method for 29 veterinary drug residues in raw milk by ultra liquid chromatography coupled with quadrupole-time of flight mass spectrometry（UPLC-Q-TOF-MS）.The supernatant of raw milk was extracted from 0.2% formic acid acetonitrile solution and determined after purification by Dikma ProElut Quechers.The target compounds were separated by Waters ACQUITY UPLC HSS T3 column,and were eluted with acetonitrile and 1.0% formic acid aqueous solution,and detected in positive ion scanning mode. The results showed that through targeted analysis of the data,29 veterinary drug residues in raw milk could be detected at the same time within 20.0 minutes,of which the mass error was within ± 2 ppm and the library score was more than 90 points. The method has high accuracy and simple operation,and can meet the simultaneous and rapid determination of veterinary drug residues in raw milk sample 29.