高效液相色谱法分析原料乳和奶粉中三聚氰胺

Determination of melamine in raw milk and milk powder by HPLC

建立了二极管阵列检测器-高效液相色谱测定原料乳及奶粉中三聚氰胺的方法。奶粉样品经三氯乙酸超声提取,乙酸铅沉淀蛋白,三氯甲烷除去脂肪和非极性杂质,PROELUTPXCSPE阳离子交换固相萃取小柱进一步除去样品基质干扰,氨化甲醇洗脱。实验对色谱分离条件进行了优化,三聚氰胺的质量浓度在1.0～100.0μg/mL范围内与色谱峰面积呈良好的线性关系,回归方程为y=89.763x-113.72,相关系数为R2=0.9988。加标回收率为90.5%～105.0%,相对标准偏差(RSD)小于4.0%。该方法简单、快速,结果准确可靠。

A diode array detector-high performance liquid chromatography of melamine in raw milk and milk powder method.Milk samples were trichloroacetic acid ultrasonic extraction,protein precipitation of lead acetate,chloroform to remove fat and non-polar impurities,PROELUT PXC SPE cation exchange solid phase extraction column to further remove the sample matrix interference,ammoniated methanol elution.Experiments on the chromatographic separation conditions were optimized,the concentration of melamine in the range of 1.0~100.0 μg/mL chromatographic peak area was linear regression equation was y=89.763x-113.72,correlation coefficient R2=0.9988.The recovery rate was 90.5%~105.0% and relative standard deviation（RSD）less than 4.0%.The method is simple,fast,accurate and reliable.