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| 亲水色谱-串联质谱法对牛奶与奶粉中三聚氰胺及其衍生物含量的测定 | |
| 引用本文： | 祝伟霞,袁萍,杨冀州,刘亚风,郭俊峰,魏蔚,张书胜.亲水色谱-串联质谱法对牛奶与奶粉中三聚氰胺及其衍生物含量的测定[J].分析测试学报,2008,27(12). |
| 作者姓名： | 祝伟霞 袁萍 杨冀州 刘亚风 郭俊峰 魏蔚 张书胜 |
| 作者单位： | 1. 河南出入境检验检疫局,河南,郑州,450003;郑州大学,化学系,河南,郑州,450001 2. 河南出入境检验检疫局,河南,郑州,450003 3. 郑州大学,化学系,河南,郑州,450001 |
| 摘 要： | 建立了牛奶和奶粉中三聚氰胺及其3种衍生物（三聚氰酸、三聚氰酸一酰胺、三聚氰酸二酰胺）的亲水色谱-串联质谱检测方法（HILIC-MS/MS）。牛奶样品直接用乙腈超声波提取;奶粉样品先用水溶解后再加乙腈超声波提取,高速离心后以乙腈-水为流动相,采用亲水作用色谱柱分离这4种化合物,在电喷雾正、负电离切换多反应监测模式下进行定性与定量分析,三聚氰酸一酰胺与三聚氰酸二酰胺含量在50～10000μg/kg之间、三聚氰胺与三聚氰酸在25～5000μg/kg之间,均获得良好的线性。方法检出限（LOD）为5～20μg/kg,定量下限（LOQ）为50～100μg/kg,3个添加水平的平均回收率为81%～97%。该方法简便、快速、准确,可满足牛奶及奶粉中三聚氰胺、三聚氰酸、三聚氰酸一酰胺、三聚氰酸二酰胺测定的需要。 |
| 关 键 词： | 亲水作用色谱-串联质谱 牛奶 奶粉 三聚氰胺 三聚氰胺衍生物 |
Determination of Melamine and Its Derivatives in Milk and Milk Powder by Hydrophilic Liquid Chromatography-Tandem Mass Spectrometry |
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| ZHU Wei-xia,YUAN Ping,YANG Ji-zhou,LIU Ya-feng,GUO Jun-feng,WEI Wei,ZHANG Shu-sheng.Determination of Melamine and Its Derivatives in Milk and Milk Powder by Hydrophilic Liquid Chromatography-Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2008,27(12). | |
| Authors: | ZHU Wei-xia YUAN Ping YANG Ji-zhou LIU Ya-feng GUO Jun-feng WEI Wei ZHANG Shu-sheng |
| Abstract: | A HILIC-MS/MS method was developed to determine melamine and its three derivatives,cyanuric acid,ammelide and ammeline in milk and milk powder.The milk sample was directly extracted by acetonitrile with the help of ultrasonic,and milk powder was resolved in water before extraction by acetonitrile.After centrifugation,the extracts were separated on HILIC column by using acetonitrile-water as mobile phase.The analytes were identified and quantitated by LC-tandem MS under the positive/negative electrospray ion... |
| Keywords: | HILIC-MS/MS milk milk powder melamine melamine derivatives |
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