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  

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

作　　者：胡婷[1] 彭涛[2] 李晓娟[2] 陈冬东[2] 代汉慧[2] 周玥宁[3] 夏曦[1] 丁双阳[1] 朱爱玲[1] 江海洋[1] 

机构地区：[1]中国农业大学动物医学院,北京100193 [2]中国检验检疫科学研究院,北京100123 [3]山西大学化学化工学院,太原030006

出　　处：《分析化学》2012年第2期236-242,共7页Chinese Journal of Analytical Chemistry

基　　金：国家质检总局科技项目基金(No2009IK314)资助项目

摘　　要：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%。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.

关 键 词：非甾体抗炎药 离子交换固相萃取 超高效液相色谱-串联质谱 多残留 动物组织 

分 类 号：S859.84[农业科学—临床兽医学]