高效液相色谱—二级管阵列法测定含乳食品中三聚氰胺含量

目的建立二级管阵列检测器-高效液相色谱测定含乳食品中三聚氰胺含量的方法。方法样品经提取、沉淀蛋白、固相萃取柱净化后,高效液相色谱测定。用BioBasicSCX色谱柱分离、乙腈-磷酸二氢钾（0.05mol/L,pH3.0）作为流动相、二级管阵列检测器进行检测。结果标准曲线在25.0800.0μg/ml范围内线性关系良好,相关系数r=0.9999,回归方程为y=0.1094x-0.049;相对标准偏差（RSD）为1.38%;加标回收率为89.9%90.2%;方法检出限为0.07mg/kg。结论本法精密度、准确度、灵敏度均能满足含乳食品中三聚氰胺含量分析的要求,适用于含乳食品中三聚氰胺含量的测定。

Determination of Melamine in Milk Food by High Performance Lquid Chromatography With Diode Array Detection

Objective To establish a method for the determination of melamine in milk food by high performance liquid chromatography with diode array detection.Method The sample was extracted,and protein was precipitated,the supernatant was cleaned-up by solid-phase extraction;the melamine in the sample solution was separated with BioBasic SCX column,the acetonitrile-potassium dihydrogen phosphate（0.05mol/L,pH 3.0） as mobile phase and detected at 236 nm with a diode array detector.Results Melamin content ranging from 25-800μg/ml has a good linearity（r = 0.9999）,the regression equation y = 0.1094x-0.049：RSD = 1.38%,the recoveries were 89.91-90.19 %,the limit of detection was 0.07mg/kg.Conclusion The method had a high sensitivity,precision,accuracy,and can be used for detemination of melamine in dairy food.