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。
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 aeetonitrile 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 eleetrospray ionization and multiple reaetion monitor（MRM）mode. The calibration curves showed good linearity in the range of 25 -5 000 μg/kg for melamine and eyanuric acid, and 50 - 10 000 μg/kg for ammeline and ammelide. The limits of detection and limits of quantification were in the range of 5 - 20 μg/kg and 50 - 100 μg/kg, respectively. The recoveries of melamine and its three derivatives from milk sample spiked three concentration levels ranged from 81% to 97% with RSDs of 4. 1% -9.3% . The method is simple, rapid, and aeeurate, and is suitable for the determination of melamine, ammeline, ammelide, and eyaeuric acid in milk and milk powder.
出处
《分析测试学报》
CAS
CSCD
北大核心
2008年第12期1288-1292,1297,共6页
Journal of Instrumental Analysis
