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%~11...

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Published in分析化学 Vol. 40; no. 2; pp. 236 - 242
Main Author 胡婷 彭涛 李晓娟 陈冬东 代汉慧 周瑚宁 夏曦 丁双阳 朱爱玲 江海洋
Format Journal Article
LanguageChinese
Published 中国农业大学动物医学院,北京,100193%中国检验检疫科学研究院,北京,100123%山西大学化学化工学院,太原,030006 2012
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ISSN0253-3820
DOI10.3724/SP.J.1096.2012.10597

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Summary: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%。
Bibliography:Non-steroidal anti-inflammatory drugs; Ion exchange solid phase extraction; Ultra performance liquid chromatography tandem mass spectrometry; Multi-residue; Animal tissues
22-1125/O6
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%,respecti
ISSN:0253-3820
DOI:10.3724/SP.J.1096.2012.10597