离子交换固相萃取-超高效液相色谱-串联质谱法同时测定动物组织中的8类非甾体抗炎药残留

采用离子交换固相萃取-超高效液相色谱-串联质谱法同时测定了动物组织中的8类14种非甾体抗炎药(Non-steroidal anti-inflammatory drugs,NSAIDs)残留。动物组织样品经乙腈-乙酸乙酯(1∶1,V/V)提取、乙腈饱和正己烷除脂、Oasis MCX阳离子交换固相萃取柱除杂后,用液相色谱-质谱联用仪电喷雾电离,多反应监测模式检测。本方法的检出限为3.0～10.0μg/kg;定量限为10.0～25.0μg/kg;添加浓度在10.0～1000.0μg/kg范围内,牛肉组织中的回收率为62.9%～108.4%,相对标准偏差小于10%;猪肉组织中的回收率为63.4%～117.0%,相对标准偏差小于9%。

Ion Exchange Solid Phase Extraction Coupled with Liquid Chromatography Tandem Mass Spectrometry for Determination of 8 Classes of Non-steroidal Anti-inflammatory Drugs Residues in Animal Tissues

An ultraperformance liquid chromatography tandem mass spectrometric(UPLC-MS/MS) method was established for the simultaneous determination of residues of 8 classes of 14 non-steroidal anti-inflammatory drugs(NSAIDs) in animal tissues.The samples were extracted with acetonitrile-ethyl acetate(1 ∶ 1,V/V),defatted with n-hexane,and then purified by MCX solid phase extraction(SPE) cartridge.Analysis was carried out on UPLC-ESI-MS/MS working with multiple reaction monitoring mode with polarity switching.Limits of detection were between 3.0 μg/kg and 10.0 μg/kg,and limits of quantification were between 10.0 μg/kg and 25.0 μg/kg.At spiked levels of 10.0-1000.0 μg/kg,in bovine and swine muscle the recoveries were 62.9%-108.4% and 63.4%-117.0%,respectively,and relative standard deviations(RSD) of the method were less than 10% and 9%,respectively.