超高效液相色谱法快速测定原料乳中的双氰胺

Rapid Determination of Dicyandiamide in Raw Milk by Ultra High Performance Liquid Chromatography

建立了超高效液相色谱检测原料乳中双氰胺的分析方法。采用甲醇提取样品中的双氰胺,HILICS色谱柱为分析柱,流动相为乙腈-10 mmol/L乙酸铵(90∶10,体积比),流速0.4 mL/min,检测波长230 nm。双氰胺在0.006 mg/L～10.0 mg/L范围内具有良好的线性关系,标准曲线方程为y=90.336x+0.994 6,R2=0.999 9。方法检出限为0.05 mg/kg,不同添加水平平均回收率在87.0%～91.6%之间,变异系数<3.84%(n=6)。此方法操作简便,可在15min内完成快速检测,适用于原料乳中双氰胺残留的快速筛查。

An ultra high performance liquid chromatography method was developed for determination of dicyandiamide in saw milk. Dicyandiamide was extracted by methanol, the sample was isolated on a HILIC column,using a mobile phase made up of acetonitrile and 10mmol/L ammonium acetate （90∶10, V/V） at a flow rate of 0.4 mL/min, and detected at 230 nm. Dicyandiamide was well separated with a good linear relationship in the range of 0.006 mg/L-10.0 mg/L,caffeine standard curve equation：y=90.336x＋ 0.994 6,R2=0.999 9.The detection limit was 0.05 mg/kg, recovery rate was in the range of 87.0%-91.6%at several spiked levels, and the coefficient of variance of method was less than 3.84%（n=6）.This method is simple, the whole determination process was completed within 15 min, making it applicable for analysis in dicyandiamide monitoring programmes in saw milk.