超高效液相色谱-串联质联用法筛查猪肉中66种药物残留

Simultaneous Determination of 66 Kindsof Veterinary Drugs in Porcine Muscle Using Ultra Performance Liquid Chromatography coupled with tandem Mass Spectrometry Simultaneous Determination of 66 Kindsof Veterinary Drugs in Porcine Muscle Using Ultra Performance Liquid Chromatography coupled with tandem Mass Spectrometry

关键词:  超高效液相色谱-串联质谱  兽药  筛查  猪肉

Key words:  UPLC-MS/MS  veterinary drugs  simultaneous determination  porcine muscle

摘要:

建立了猪肉中磺胺类、氟喹诺酮类、四环素类、大环内酯类、林可胺类、硝基咪唑类、氯霉素类、解热镇痛类、抗病毒类、镇定剂类和头孢类等11类66种药物液相色谱-串联质谱（UPLC-MS/MS）检测方法。样品经乙腈-甲醇（V/V，95:5）和乙腈-水（V/V，15:2）溶液分别提取后，Agela Cleanert?PEP-2固相萃取柱净化后采用UPLC-MS/MS测定，外标法定量。结果表明，猪肉中66药物检测限为0.2～5 μg/kg，定量限为0.5～20μg/kg。在2～100μg/kg添加浓度范围内药物回收率35%～140%之间，批内相对标准偏差均小于20％。本方法可实现对多种兽药的同时检测，为动物源性食品中药物残留监控提供快速、灵敏的分析手段，具有很重要的现实意义。

Abstract:

A method based on ultra performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS) was developed for simultaneous determination of 66 kinds veterinarydrugsof sulfonamides，fluoroquinolones，tetracyclines，macrolides，lincosamides，nitroimidazoles，chloramphenicols，antipyretic analgesics，antiviral agents，tranquilizers，cephalosporin etc. from 11 classes in porcine muscle.The analyte was extracted with acetonitrile-methanol (V/V，95:5) and acetonitrile -water(V/V，15:2)，and was cleaned up by the AgelaCleanert? PEP-2cartridge.Quantification of the analyte was achieved by UPLC-MS/MS with multiple reaction monitoring (MRM) using external standard method.The results indicated that the detection limits and quantification limits of the method were 0.2～5μg/kg and 0.5～20 μg/kg.The average recoveries of the drugs ranged from 35%~140% at spiked levels of 2~100μg/kg with RSD less than 20%.The method can achieve the simultaneous analysis of different compound groups，and wasreliable and sensitive for monitoring drug residues in animal derived food ，which has a very important practical significance.