超高效液相色谱-电喷雾串联质谱法同时测定猪肝中非甾体类抗炎药残留

采用超高效液相色谱-四极杆串联质谱仪(UPLC-MS/MS)同时测定了猪肝中18种非甾体类抗炎药(NSAIDs)的残留量.对NSAIDs多残留同时提取、净化技术进行了研究,对UPLC-MS/MS检测参数进行了优化.均质后的猪肝样品采用酸化乙腈提取,正己烷液-液分配(LLP)脱脂,经硅胶固相萃取(SPE)柱净化后,采用UPLC-MS/MS电喷雾电离(ESI),多反应监测(MRM)模式检测,以保留时间和子离子比定性,外标法定量.方法检出限(LOD)为0.2～10 μg/kg;定量限(LOQ)为1.0～50 μg/kg.在添加浓度在1.0～200 μg/kg范围内,NSAIDs的回收率在53.8%～92.7%之间,相对标准偏差(RSD)小于10.3%.方法操作简便,对动物肌肉、内脏、鸡蛋及牛奶中NSAIDs残留的检测具有普遍适用性.

Simultaneous Determination of Residues of Non-steroidal Anti-inflammatory Drugs in Swine Liver by Ultra-Performance Liquid Chromatography with Electrospray Ionization Quadrupole Rods Tandem Mass Spectrometric Detection

An ultra-performance liquid chromatography-quadrupole rods tandem mass spectrometric(UPLC-MS/MS) method was established for the simultaneous determination of residues of eighteen non-steroidal anti-inflammatory drugs(NSAIDs) in swine liver.A study of extraction and cleanup method in multi-residue analysis of NSAIDs was made,and parameters of UPLC-MS/MS were optimized.Homogenized samples were extracted with acidic acetonitrile.The extracts were defatted with n-hexane by liquid-liquid partition(LLP),and then ...