亲水作用色谱-电喷雾串联质谱法测定生鲜牛乳及奶粉中的双氰胺

Determination of Dicyandiamide in Milk and Milk Powder by Hydrophilic Interaction Chromatography-Electrospray Ionization Tandem Mass Spectrometry

建立了检测生鲜牛乳及奶粉中双氰胺的亲水作用色谱-电喷雾串联质谱(HILIC-ESI-MS/MS)分析方法。样品经乙腈提取后经亲水作用色谱柱分离,电喷雾串联四级杆质谱检测。结果显示,双氰胺标准曲线在0.5～100μg/L浓度范围内线性良好。相关系数(r)大于0.99;在5～50μg/kg添加水平下,回收率在80.1%～88.2%之间,相对标准偏差(RSD)均小于10%(n=6);方法操作简便、灵敏度高,适用于生鲜牛乳及奶粉中双氰胺的筛查及确证分析。

A simple, sensitive method has been developed for the quantification of dicyandiamide in milk and powder. Dicyandiamide extracted by acetonitrile from sample and analyzed by hydrophilic interaction chromatography- electrospray ionization tandem mass spectrometry （HILIC -ESI- MS/MS）. The sample was separated on hydrophilic column （150 mm ×2.1 mm i. d. ,1.7 μm） using a mobile phase of acetonitrile/0. 2% FA. Results showed that in the range of O. 5 to 100 μg/L the standard curves for dicyandiamide were in good linearity , the correlation coefficients （r） was O. 9996. The recoveries were between 80.1% and 88.2% ,and the relative standard deviation （RSD） for the determination of chlorpromazine were less than 10% （n = 6）. The limits of quantity （S/N ≥ 10） and limits of detection（ S/N ≥3 ） by the present method for dicyandiamide were found to be 5 μg/kg and 2 μg/kg, respectively. The method was accurate, high sensitive and stable for the determination of dicyandiamide in milk and milk powder