GC-MS法同时测定生鲜乳中三聚氰胺及其类似物的研究  

A gas chromatography mass spectrometry method developed for determination of melamine and its analogues in raw milk

作　　者：朱聪英[1] 应永飞[1] 罗成江[1] 周炜[1] 陈慧华[1] 韦敏珏[1] 林仙军[1] 

机构地区：[1]浙江省饲料监察所

出　　处：《中国饲料》2011年第22期27-31,共5页China Feed

基　　金：浙江省优先主题重点农业项目(2009C12055)资助

摘　　要：采用气相色谱-质谱(GC-MS)法,建立了生鲜乳中三聚氰胺及其类似物的定性定量测定方法。试样中的三聚氰胺及其类似物经(乙腈∶水∶二乙胺=5:4:1,V/V)提取,饱和乙酸铅溶液沉淀蛋白后,氮气吹干,用BSTFA进行衍生化,气相色谱-质谱法测定。采用色谱保留时间和质谱碎片离子丰度比定性,内标法定量。采用SCAN全扫描的方式进行仪器方法学研究,每种化合物确定4个碎片离子作为监测离子,进行SIM模式定性定量分析。该方法生鲜乳中4种化合物的检出限为0.1～0.2 mg/kg;在20.0～1000μg/L的浓度范围内,线性相关系数r均大于0.999。在生鲜乳中添加0.50～50 mg/kg的三聚氰胺及其类似物,其回收率为62.0%～110.0%,相对标准偏差为2.4%～13.9%。In this paper, a gas chromatography-mass spectrometry（GC-MS）method was developed for determination of melamine and its analogues,including ammelide, ammeline, and eyanuric acid in raw milk.These compounds were extracted with acetonitrile/water/DEA （5：4：l,V/V） from analyte,and the protein precipitator of lead ＇acetate was added.After centrifugation,an aliquot of the supernatant was evaporated by nitrogen blow,derivatized with BSTFA and then assayed by GC-MS.The detection limite of 4 compounds in raw milk were 0.1 - 0.2 mg/kg.The calibration curves were linear in the range of 20.0-1000 p.g/L and correlation coefficient were more than 0.999.Recoveries of melamine and its analogues were 62.0 % - 110.0 % and the inter-relative standard deviation were 2.4 % - 13.9 % at spike levels of 0.5 - 50.0 mg/kg.

关 键 词：气相色谱-质谱法 生鲜乳 三聚氰胺 类似物 

分 类 号：S816.17[农业科学—饲料科学]