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。 |
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 |
DOI: |
投稿时间:2013-05-15修订日期:2013-07-11 |
基金项目: |
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Determination of Dicyandiamide in Milk and Milk Powder by Hydrophilic Interaction Chromatography-Electrospray Ionization Tandem Mass Spectrometry |
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(Shanghai Municipal Institute of Veterinary Drug and Feedstuff Control) |
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. |
Key words: hydrophilic interaction chromatography-electrospray ionization tandem mass spectrometry dicyandiamide milk milk powder |