液相色谱-串联质谱法测定奶粉和液态奶中三聚氰酸

Determination of cyanuric acid in milk power and milk by Liquid Chromatography-Tandem Mass Spectrometry

目的:建立奶粉和液态奶中三聚氰酸的液相色谱-串联质谱检测方法(LC-MS/MS)。方法:样品加水混匀后加乙腈超声波提取,经固相萃取柱净化,采用亲水作用色谱柱分离,在电喷雾负电离多反应监测模式下进行定性和内标法定量。结果:本法线性范围为0μg/kg～500μg/kg,定量限为200μg/kg,3个添加水平的平均回收率在92.1%～104.3%,精密度(RSD%)为3.22%～7.61%。结论:该法简便、快速、准确,适于奶粉和液态奶中三聚氰酸的检测。

Objective：To establish a method for detemination of cyanuric acid in milk power and milk by LC-MS/MS.Methods： The target analyte was extracted ultrasonically from samples after mixing with water and acetonitrile,and the supernatant was purified with solid phase extraction column,and separated using hydrophilic interaction column,and qualification and quantification by internal standard was done with negative ion electrospray ionization in multiple reaction monitoring mode.Results： The calibration curve of the method was linear in the range of 0 μg/kg^500 μg/kg.The limits of quantification were 200 μg/kg.The recoveries from milk and milk powder at three concentration levels ranged from 92.1% to 104.3% with RSD of 3.22% to 7.61%.Conclusion： The method is simple,rapid,accurate and suitable for the determination of cyanuric acid in milk powder and milk.