亲水作用色谱-串联质谱法同时测定液态奶中三聚氰酸和三聚氰胺  

Simultaneous determination of cyanuric acid and melamine in liquid milk by hydrophilic interaction chromatography combined with tandem mass spectrometry

作　　者：卢跃鹏 方慧文 胡筱静 江小明 李君 杨永 段建坤 骆丹 

机构地区：[1]国家饮料及粮油制品质量监督检验中心(武汉产品质量监督检验所),武汉430043 [2]岛津国际贸易(上海)有限公司上海分析中心,上海200052

出　　处：《分析试验室》2010年第11期94-97,共4页Chinese Journal of Analysis Laboratory

摘　　要：建立了亲水作用色谱-串联质谱同时测定液态奶中三聚氰酸和三聚氰胺的方法。液态奶样品经体积分数2.5%甲酸溶液提取、离心后乙腈稀释,亲水作用色谱柱分离,电喷雾串联四极杆质谱检测器检测,分别在负、正离子模式下测定三聚氰酸和三聚氰胺。三聚氰酸和三聚氰胺分别在0.5～100μg/L、0.1～50μg/L范围内线性关系良好。在0.25～15mg/kg、0.1～7.5mg/kg添加水平范围内,三聚氰酸平均回收率为84.5%～98.0%(RSD为2.1%～6.1%),三聚氰胺平均回收率为85.5%～88.9%(RSD为3.2～5.8%)。三聚氰酸、三聚氰胺定量限分别为0.25mg/kg、0.1mg/kg。A method using hydrophilic interaction chromatography combined with tandem mass spectrum was established for the determination of cyanuric acid and melamine in liquid milk.Liquid milk samples were extracted with 2.5% aqueous formic acid and centrifuged followed by dilution with acetonitrile.Both compounds were analysed with hydrophilic interaction chromatography.Electrospray ionization was used in both the negative ion(cyanuric acid) and positive ion(melamine) modes.The linear range of cyanuric acid and melamine were in the range of 0.5~100 μg/L and 0.1~50 μg/L,respectively.The recoveries of cyanuric acid and melamine were in the range of 84.5%~98.0% and 85.5%~88.9%,with relative standard deviations ranging between 2.1%~6.1% and 3.2%~5.8%,when spiked with analytes at 0.25~15mg/kg and 0.1~7.5mg/kg,respectively.The limits of quantification are 0.25mg/kg for cyanuric acid and 0.1mg/kg for melamine.

关 键 词：亲水作用色谱 质谱 三聚氰酸 三聚氰胺 

分 类 号：TS252.2[轻工技术与工程—农产品加工及贮藏工程]