在线净化液相色谱串联质谱法测定动物源食品中金刚烷胺的残留  

Determination of Amantadine Residues in Foods of Animal Origin by On-line Cleanup Liquid Chromatography-Tandem Mass Spectrometry

作　　者：艾连峰[1] 马育松[1] 陈瑞春[1] 郭春海[1] 康占省[1] 

机构地区：[1]河北出入境检验检疫局,石家庄050051

出　　处：《分析化学》2013年第8期1194-1198,共5页Chinese Journal of Analytical Chemistry

基　　金：国家质检总局科技计划项目(No.2013IK154);河北检验检验局科研项目(No.HE2011K005)资助

摘　　要：建立了在线净化液相色谱串联质谱法测定动物源食品中金刚烷胺的残留。样品用甲醇-1%三氯乙酸或乙腈提取,提取液用阳离子交换在线净化柱(Cyclone MCX)净化,5%氨水-甲醇溶液将分析物洗脱转入至Capcell Pak MG C18分析柱,经色谱分离后,用串联质谱检测。方法的定量限(LOQ)牛奶为0.25μg/kg,动物组织和鸡蛋为0.5μg/kg,在0.1～20μg/L浓度范围内呈良好线性,线性相关系数大于0.9995。方法在3个水平的添加回收率为83.3%～93.6%,相对标准偏差在3.5%～5.9%之间。方法简单快速,回收率高,重现性好,适用于动物源食品中金刚烷胺残留的定量及确证分析。A new method using online cleanup technology combined with tandem mass spectrometry（MS/MS） has been developed for determination of amantadine residues in foods of animal origin.The manual sample preparation was limited to extraction of simples by methanol-1%trichloroactic acid（50 ∶ 50,V/V） or acetonitrile.The extract was online purified on cyclone MCX column where the sample matrix was washed away while the analytes were retained.Subsequently,the analytes were eluted from the extraction column onto the analytical column（Capcell Pak MG C18 column） by means of 5% ammonia hydroxide methanol solution prior to chromatographic separation and MS/MS detection.The limit of quantization（LOQ） for milk was 0.25 μg/kg,and for animal tissues and egg was 0.5 μg/kg.The linearity is satisfactory with a correlation coefficient of 0.9995 at concentrations ranging from 0.1 to 20 μg/L.Average recoveries of the analytes fortified at three levels were range from 83.3% to 93.6%,and the relative standard deviations were range from 3.5% to 5.9%.The method is suitable for quantitative analysis and confirmation of amantadine residues in foods of animal origin.

关 键 词：在线净化液相色谱串联质谱 金刚烷胺 残留 动物源食品 

分 类 号：S859.84[农业科学—临床兽医学]