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.
出处
《食品与生物技术学报》
CAS
CSCD
北大核心
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)
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
ultra performance Liquid chromatography coupled with quadrupole-time of flight mass spectrometry （UHPLC-Q-TOF-MS）, milk, veterinary drug, rapid screening
