固相萃取-亲水作用色谱法检测奶粉中的三聚氰胺

Determination of Melamine in Powdered Milk by Hydrophilic Interaction Liquid Chromatography Combined with Solid Phase Extraction

采用固相萃取-亲水作用色谱法对奶粉中的三聚氰胺进行测定。样品经0.1%TFA甲醇提取,Strata X-C固相萃取小柱净化,用Phenomenex Luna HILIC柱分离,乙腈-0.1%甲酸(90:10)为流动相,经液相色谱检测。结果表明,三聚氰胺在1～50μg/mL的浓度范围之间具有良好的线性关系(R2=0.9998),加标回收率大于90%。该方法简单,精密度和准确度高,适用于奶粉中三聚氰胺的测定。

A hydrophilic interaction liquid chromatography （SPE-HILIC） method combined with solid phase extraction for the determination of melamine in powdered milk was established. The sample was extracted with methanol, purified with Strata X-C solid phase extraction column and then analyzed by a Phenomenex Luna HILIC column with mobile phase of acetonitrile-0.1% formic acid （90： 10）. The calibration curve was linear within the range of 1～50 μg/mL （R2=0.9998）. And the recovery was over 90 %. The method was simple and accurate, which can be used to determine the melamine in powdered milk.