固相萃取/LC-MS/MS法检测动物源性食品中的金刚烷胺  

Determination of amantadine residues in food of animal origin by Solid-phase extraction/LC-MS/MS

作　　者：云环[1] 张朝晖[1] 罗生亮[2] 张杉[1] 

机构地区：[1]北京出入境检验检疫局,北京100026 [2]南昌航空大学环境与化学工程学院,南昌330063

出　　处：《现代仪器》2009年第6期42-45,共4页Modern Instruments

摘　　要：建立测定动物源性食品中金刚烷胺的固相萃取/液相色谱一电喷雾串联质谱分析方法。以甲醇-1%三氯乙酸(50+50,v/v)作提取溶剂,采用超声波辅助溶剂萃取法萃取动物源性食品,萃取液用Waters Oasis MCX固相萃取柱进行净化浓缩。以ThermoHypersil Gold C_(18)色谱柱为分离柱,在正离子模式下以电喷雾电离串联质谱仪进行测定。对流动相组分和流动相添加剂对质谱的离子化效率进行考察,在1.0～50.0 ng/mL范围内线性关系良好(r?0.99)。样品在5.0 μg/k,10.0μg/k和20.0 μ g/kg添加水平的回收率为75.9%～108.5%,相对标准偏差小于8.0%;方法的检出限为5.0μg/kg。本方法具有很高的灵敏度和准确度,能够满足动物源性食品中的金刚烷胺残留量的快速、高灵敏检测分析。A comprehensive analytical method based on solid-phase extraction/high liquid chromatography- electrospray ionization tandem mass spectrometry with positive ionization mode has been developed for measur- ing amantadine residues in food of animal origin.Samples were extracted by Ultrasonic wave Assistant Extraction (UAE) with a mixed solvent of methanol-1% trichloroacetic acid(50/50,v/v).Sample purification and concentra- tion were performed by solid-phase extraction (SPE) with Waters Oasis MCX column.Then the reconstituted sample solution was analyzed by LC-MS/MS under positive ion mode,with Thermo Hypersil Gold C_(18) column as the analytical column.The effects of mobile phase and additives on ionization were assessed.The linear range was 1.0～50.0 ng/mL,the correlation coefficients (r) were under 0.99.The recoveries ranged from 83.4%～99.4% and the relative standard deviations were below 8.0% following analysis of spiked at concentrations 5.0μg/kg,10.0 μg/ kg and 20.0 μg/kg.The detection limits of the method was 5.0 μg/kg.Conditions suitable for the qualitative and quantitative confirmation of amantadine residues in food of animal origin are specified.

关 键 词：固相萃取柱 LC-MS/MS 检测分析 动物源性食品 金刚烷胺 质谱分析方法 相对标准偏差 流动相添加剂 电喷雾电离 正离子模式 串联质谱仪 超声波辅助 液相色谱 线性关系 添加水平 提取溶剂 溶剂革取 测定 准确度 相组分 

分 类 号：TH7[机械工程—仪器科学与技术]