摘要
目的：建立乳及乳制品中三聚氰胺的自动固相萃取-高效液相亲水色谱检测方法。方法：样品经1%三氯乙酸超声提取、Oasis MCX SPE柱自动固相萃取后,采用乙腈：20 mmol/L乙酸铵（90：10）等度洗脱,在Atlantis Hilic Silica色谱柱上实现与杂质完全分离,紫外检测器210 nm检出,外标法定量。结果：方法定量限为0.2 mg/kg,加标回收率在87%～96%之间,测定的相对标准偏差在0.8%～3.4%。结论：本法准确、精密、自动化程度高,适合于实际样品的日常检测。
Objective：A approach for the determination of melamine in raw milk and dairy products by hydrophilic interaction liquid chromatography using automated solid phase extractin is described.Methods：Trichloroacetic acid solution was used to precipitate proteins and to dissociate the target analyte from the sample matrix.The extracted solution was cleaned-up with Oasis MCX SPE column using an automated solid phase extractin system.The HPLC separation was carried out on a Atlantis Hilic Silica column（4.6 mm×150 mm,3 μm） with acetonitrile-20 mmol/L ammonium acetate（90：10,v/v） as mobile phase at flow rate of 1.00 ml/min,and detected at UV 210 nm,then quantified by external standard calibration.Results：The limit of quantification（s/n=10） for melamine was 0.2 mg/kg.The recoveries were 87%～96% with the relative standard deviation of 0.8%～3.4%（n=5）.Conclusion：This method is accurate and precise to detect melamine in raw milk and dairy products.
出处
《中国卫生检验杂志》
CAS
2009年第3期537-538,551,共3页
Chinese Journal of Health Laboratory Technology
关键词
三聚氰胺
乳及乳制品
高效液相亲水色谱法
Melamine
Raw milk and dairy products
Hydrophilic interaction liquid chromatography
