固相萃取-超高效液相色谱-串联质谱同时检测动物源性食品兽药残留

Simultaneous Determination of Veterinary Drug Residues in Animal-origin Food by Solid Phase Extraction-Ultra Performance Liquid Chromatography-Mass Spectrometry

利用固相萃取-高效液相色谱-串联质谱方法对喹诺酮类与青霉素类2类15种兽药在动物源性食品中的残留情况进行检测。样品经丙醇-乙酸乙酯(5∶5)提取,由不经活化的prime HLB固相萃取柱净化,使用甲醇-5 mmol/L乙酸铵水溶液(含0.1%甲酸)作为流动相,电喷雾离子源分段多反应监测扫描模式检测。15种兽药检出限为0.5~2.0μg/kg,定量限为2.0~5.0μg/kg,各基质中回收率为71.3%~96.5%,相对标准偏差为2.1%~9.2%。采用此方法,能有效提高多残留兽药的检测效率,可良好应用于食品安全问题中兽药残留的快速分析。

15 Kinds of veterinary drug residues in animal-origin food were detected by solid phase extraction-ultra performance liquid chromatography-mass spectrometry. Samples were extracted by acetone-ethyl acetate, and were purified by a prime HLB solid phase extraction column. The eluate was detected by multiple reaction monitoring scanning with electronic spray ionization. The limits of quantitation for 15 veterinary drugs were in the range of 2.0-5.0 μg/kg, as well as the detection limits were 0.5-2.0 μg/kg. Recoveries from different food matrices were 71.3%-96.5% with relative standard deviations between 2.1%-9.2%. This method is significantly efficient in the determination of multiple veterinary drugs and suitable for rapid analysis of veterinary drugs.