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禽蛋中头孢噻肟残留的高效液相色谱-串联质谱法测定
引用本文:罗辉泰,黄晓兰,吴惠勤,朱志鑫,黄芳,林晓珊.禽蛋中头孢噻肟残留的高效液相色谱-串联质谱法测定[J].分析测试学报,2010,29(8).
作者姓名:罗辉泰  黄晓兰  吴惠勤  朱志鑫  黄芳  林晓珊
作者单位:中国广州分析测试中心,广东省分析测试技术公共实验室,广东,广州,510070
摘    要:建立了高效液相色谱-串联质谱(LC-MS/MS)测定禽蛋中头孢噻肟药物残留的方法。禽蛋样品中的头孢噻肟用纯水提取,乙腈沉淀蛋白,Oasis HLB(500 mg,6 mL)固相萃取柱净化,8 mL甲醇洗脱。采用Zorbax XDB-C18(2.1 mm×50 mm,3.5μm)色谱柱,以0.2%甲酸水-乙腈为流动相,0.3 mL/min梯度洗脱,经高效液相色谱分离后,采用电喷雾质谱正离子模式电离,多反应选择离子检测(MRM)模式测定。检测离子对为m/z456.1/396.1、m/z456.1/324.1,其中m/z456.1/396.1为定量离子对。在1.35~135μg/L范围内标准曲线的线性关系良好,相关系数为0.999 3;在1.0、50.0、100μg/kg3个添加水平的平均加标回收率为87%~99%,相对标准偏差为1.9%~3.9%;方法检出限为0.3μg/kg,定量下限为1.0μg/kg。该方法简便、灵敏、准确、可靠,适用于禽蛋中头孢噻肟药物残留的分析。

关 键 词:头孢噻肟  高效液相色谱  串联质谱  禽蛋  残留

Determination of Cefotaxime Residue in Poultry Egg by High Performance Liquid Chromatography-Tandem Mass Spectrometry
LUO Hui-tai,HUANG Xiao-lan,WU Hui-qin,ZHU Zhi-xin,HUANG Fang,LIN Xiao-shan.Determination of Cefotaxime Residue in Poultry Egg by High Performance Liquid Chromatography-Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2010,29(8).
Authors:LUO Hui-tai  HUANG Xiao-lan  WU Hui-qin  ZHU Zhi-xin  HUANG Fang  LIN Xiao-shan
Institution:LUO Hui-tai,HUANG Xiao-lan,WU Hui-qin,ZHU Zhi-xin,HUANG Fang,LIN Xiao-shan(Guangdong Provincial Public Laboratory of Analysis and Testing Technology,China National Analytical Center(Guangzhou),Guangzhou 510070,China)
Abstract:A confirmative method to determine cefotaxime residue in poultry egg by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) under multiple reaction monitoring(MRM)mode was developed.The cefotaxime in sample was extracted with water.Sample preparation involved the protein precipitation with acetonitrile and the clean-up on an Oasis HLB(500 mg,6 mL) solid phase extraction(SPE) cartridge.The analyte was eluted from the SPE cartridge with 8 mL methanol.The separation of cefotaxime was pe...
Keywords:cefotaxime  high performance liquid chromatography(HPLC)  tandem mass spectrometry(MS/MS)  poultry egg  residue  
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