高效液相色谱一串联质谱法测定鱼肉中8种喹诺酮类药物的残留量

目的建立鱼肉中恩诺沙星、丹诺沙星、环丙沙星、诺氟沙星、培氟沙星、沙拉沙星、双氟沙星、氧氟沙星等8种喹诺酮类药物残留量的高效液相色谱-串联质谱检测方法。方法以氘代试剂为内标,样品经酸性乙腈提取后,用正己烷脱脂,旋转蒸发浓缩,采用LC-MS/MS多反应监测(MRM)正离子模式测定。结果 8种喹诺酮的水平为1.0μg/kg和3.0μg/kg时回收率为88.4%～114.9%,检出限(S/N=3)为0.03～0.1μg/kg。结论该方法简便快捷,精密度好,准确度高,可满足鱼肉中多种喹诺酮类药物残留的定性、定量检测要求。

Simultaneous determination of 8 quinolone residues in fish meat by high performance liquid chromatography-tandem mass spectrometry

Objective To establish a method for simultaneous determination of 8 qunolone residues(enrofloxacin,danofloxacin,ciprofloxacin,norfloxacin,pelfoxacin,sarafloxacin,difloxacin,ofloxacin) in fish meat by high performance liquid chromatography-tandem mass spectrometry(LC-MS/MS).Methods Deuterium substituted reagents used as internal standards were added to fish meat samples before extraction.Samples were extracted with acidified acetonitrile,cleaned-up by hexane,and concentrated with a rotary evaporator.The mass spectrometer was operated in the positive ion mode using multiple reaction monitoring(MRM).Results The average recoveries of 8 qunolone compounds added at 1.0 and 3.0 μg/kg were in the range of 88.4%-114.9%.The detection limits of compounds with the method were ranged from 0.03 to 0.1 μg/kg.Conclusion The method is suitable for quantitative and qualitative detection of quinolone residues in fish samples,with advantages of quick,simple and repeatable.