加压毛细管电色谱测定乳及乳制品中三聚氰胺  

Determination of Melamine in Milk and Dairy Product by Pressurized Capillary Electro-Chromatography

作　　者：郭启雷[1] 史海良[1] 赵丽[1] 杨红梅[1] 王浩[1] 

机构地区：[1]国家食品质量安全监督检验中心,北京100094

出　　处：《食品研究与开发》2015年第8期77-80,共4页Food Research and Development

基　　金：北京市科技计划项目(Z111100056811006)

摘　　要：研究建立利用加压毛细管电色谱(p CEC)测定乳及乳制品中三聚氰胺的分析方法。样品采用2%三氯乙酸水溶液超声提取,阳离子固相萃取柱(MCX)净化,提取液经C18反相毛细管电色谱柱分离,流动相乙腈-10 mmol/L辛烷磺酸钠溶液(p H 3.0)=15+85,泵流速0.05 m L/min,分离电压-2 k V,紫外检测器240 nm检测。该方法在1.0 mg/kg^100 mg/kg质量浓度范围内线性关系良好(R2=0.999),在牛奶和酸奶中的定量限为2.5 mg/kg,在奶粉中的定量限为10 mg/kg,加标回收率为78.9%~93.5%,相对标准偏差小于5%。An effective and convenient method for determination of melamine in milk and dairy product was developed. Pressurized capillary electro-chromatography （pCEC） was used as separation technology. The samples were extracted by ultrasonic with 2 % trichloroacetic acid solution, cleaned up by mixed cation exchange solid phase extraction （MCX SPE）. The separation was performed on a reversed phase C18 column with 240 nm as the UV detection wavelength. The mobile phase was composed of acetonitrile and sodium octanesulfonate solution （15 ： 85, v/v, pH3.0）, at a pump flow rate of 0.05 mL/min and separation voltage of -2 kV. Under the optimal conditions, the linear range of melamine was 1.0 mg/kg-100 mg/kg with correlation coefficient higher than 0.999. The LOQ was 2.5 mg/kg in milk and yoghurt, and 10 mg/kg in milk powder. Therecoveries were 78.9 %-93.5 % and the relative standard deviations （RSD） were less than 5 %.

关 键 词：加压毛细管电色谱 乳及乳制品 三聚氰胺 

分 类 号：O657.7[理学—分析化学] TS252.7[理学—化学]