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

摘要

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.%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10.0～25.0 μg/kg;添加浓度在10.0～1000.0 μg/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％.