气相色谱-氮磷检测器测定牛奶及奶粉中三聚氰胺

目的:建立应用气相色谱-氮磷检测器测定牛奶及奶粉中三聚氰胺含量的方法。方法:样品用三氯乙酸提取,MCX阳离子固相萃取柱净化后,采用DB-1701毛细管柱和氮磷检测器进行检测。结果:方法线性范围在0.05μg/ml～5μg/ml,定量限为0.1 mg/kg(牛奶)和0.25 mg/kg(奶粉),相对标准偏差为2.1%～7.9%,回收率为86.4%～108%。结论:本方法不经衍生化处理直接测定三聚氰胺,简便、快速,灵敏度较高。

Determination of melamine in milk and milk powder by GC-NPD

Objective:To establish a method for determination of melamine residues in milk and milk powder by gas chromatography-nitrogen phosphorus detector.Methods:Melamine in the sample was extracted with trichloroacetic acid,purified with MCX cation exchange solid phase extraction column,determined by DB-1701 capillary column and GC-NPD.Results:The method linear range was 0.05 μg/ml~5 μg/ml,the limits of quantification were 0.1 mg/kg(milk)and 0.25 mg/kg(milk powder),the relative standard deviation was 2.1%~7.9%,the recovery rate was 86.4%~108%.Conclusion:The method was simple,rapid and sensitive for determination of melamine without derivatization process.