LC-MS/MS法测定猪肉中7种喹诺酮类药物的残留  

Determination of quinolones residues in animal derived food by LC-MS/MS

作　　者：梁艳[1] 熊梅瑾 张静静[1] 陈聪[1] 叶利明[1] 

机构地区：[1]四川大学华西药学院,四川成都610041 [2]成都市食品药品检验所,四川成都610044

出　　处：《华西药学杂志》2012年第6期715-717,共3页West China Journal of Pharmaceutical Sciences

摘　　要：目的采用HPLC-MS/MS法测定猪肉样品中7种喹诺酮类药物的残留。方法用乙腈提取样品基质中药物的残留,经正己烷脱脂、MCX固相萃取柱净化,以保留时间和离子对(母离子和两个碎片离子)信息比较进行定性,以母离子和响应值高的碎片离子进行定量,采用正离子MRM监测模式。结果 7种喹诺酮类药物浓度为2～200μg.kg-1时与峰面积的线性关系良好,最低检测限为0.1～0.5μg.kg-1,定量限为1.0～1.5μg.kg-1;方法回收率为92%～110%,精密度较好,日内和日间RSD均小于15%。结论所用方法分析速度快、灵敏度高、特异性好,可用于猪肉中喹诺酮类药物残留的定量和定性检测。OBJECTIVE To establish an LC-MS/MS method for the determination of seven quinolones residues in pork.METHODS Sample was extracted with acetonitrile,and was defatted with hexane.Sample was purified by using MCX solid extraction cartridge.The qualification analysis was done by using retention time and diagnostic ion pairs（parent ion and two fragment ions）,and the quantification analysis was based on the peak intensity of parent ion and a fragment ion with higher signal.A mass spectrometer was operated in the positive ion mode using multiple reaction monitoring（MRM）.RESULTS The standard curve was linear in the concentration range of 2.0-200 μg·kg-1.The detection limit of the method was in the range of 0.1-0.5 μg·kg-1 and the limit quantification ranged from 1.0 μg·kg-1 to 1.5 μg·kg-1.The average recoveries of quinnolones ranged from 92% to 110%.Both the intra-day and inter-day RSD were less than 15%.CONCLUSION This method is simple,rapid,sensitive and accurate.It is suitable for the detection of seven quinolones residues in pork.

关 键 词：高效液相色谱-串联质谱法 喹诺酮类 药物残留 

分 类 号：R917[医药卫生—药物分析学]