超高效液相色谱-四极杆飞行时间质谱法快速筛查牛奶中28种禁用兽药残留  

Rapid Screening of 28 Banned Veterinary Drugs in Milk by Ultra Performance Liquid Chromatography Coupled with Quadrupole-Time of Flight Mass Spectrometry

作　　者：虞成华[1] 林琳[1] 杨晋青[1] 孙颖宜[1] 成姗[1] 葛宇[1] 

机构地区：[1]上海市质量监督检验技术研究院,上海200233

出　　处：《食品与生物技术学报》2017年第10期1064-1070,共7页Journal of Food Science and Biotechnology

基　　金：国家质量监督检验检疫总局科技计划项目(2014QK267)

摘　　要：应用超高效液相色谱-四极杆飞行时间质谱建立了牛奶中28种兽药残留的快速筛查分析方法。牛奶样品经含体积分数0.2%甲酸的乙腈溶液提取,采用Oasis PRi ME HLB固相萃取小柱净化。目标化合物经Agilent Eclipse Plus C18色谱柱(2.1 mm×100 mm,3.5μm)分离,以甲醇-甲酸水溶液为流动相进行梯度洗脱,使用电喷雾离子源,在正负离子模式下进行全扫描,可在20 min内实现对28种兽药的良好分离。结果表明,牛奶中28种兽药的定量下限(LOQ,S/N=10)在1~10μg/kg,平均回收率在68.9%~102.0%之间,相对标准偏差在4.30%~11.5%。An analytical method was established for the simultaneous determination of 28 veterinary drugs in milk by ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry （UHPLC-Q-TOF-MS）. The analytes in milk samples were extracted with aeetonitrile containing 0.2% formic acid. The extract solution was purified by the solid phase extraction cartridge with Oasis PRIME HLB. The target compounds were separated on an Agilent ZORBAX Eclipse Plus C 18 column by gradient elution using methanol -0.1% formic acid solution as mobile phase. And detected by MS in ESI~ and ESI mode. The 28 compounds could be separated in 20 min. As a result,the limits of quantitation （LOQ,S/N=10） of 28 compounds were 1 ~ 10μg/kg in milk. The average recoveries of 28 compounds spiked at three concentration levels in the range of 68.9% ~ 102.0% with relative standard deviations of 4.30%-11.5 %. The accurate mass databases of 28 compounds were established.

关 键 词：超高效液相色谱-四极杆飞行时间质谱 牛奶 兽药 快速筛查 

分 类 号：O657.63[理学—分析化学]