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

关键词:  亲水作用色谱－电喷雾串联质谱法  双氰胺  生鲜牛乳  奶粉

Key words:  hydrophilic interaction chromatography-electrospray ionization tandem mass spectrometry  dicyandiamide  milk  milk powder

摘要:

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0.5～100 μg/L浓度范围内线性良好。相关系数(r)大于0.99；在5～50 μg/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。

Abstract:

A simple, sensitive method has been developed for the quantification of dicyandiamide in milk and milk 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?. Results showed that in the range of 0.5 to 100 μg/L the standard curves for dicyandiamide were in good linearity , the correlation coefficients (r) was 0.9996. 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.