高效液相色谱法测定鸡蛋中的三聚氰胺  

Determination of Melamine in Chicken Eggs by High Performance Liquid Chromatography

作　　者：吴彩梅[1] 白洁[1] 贾刚[1] 张克英[1] 丁雪梅[1] 白世平[1] 陈代文[1] 吴秀群[1] 

机构地区：[1]四川农业大学动物营养研究所,教育部抗病营养重点实验室,四川雅安625014

出　　处：《食品科学》2011年第8期212-218,共7页Food Science

基　　金：农业部饲料中三聚氰胺限量制定专项

摘　　要：建立采用固相萃取净化,高效液相色谱法测定鸡蛋中三聚氰胺含量的方法。样品采用三氯乙酸和乙酸铅溶液提取,优化样品提取时间、色谱柱及固相萃取柱,最终确定为样品提取20min、采用TC-C18(4.6mm×150mm,5μm)色谱柱和PCX固相萃取柱。采用紫外检测器,检测波长为240nm,流动相为乙腈:辛烷磺酸钠-柠檬酸缓冲液(10:90,V/V),流速1.0mL/min,进样量20μL,外标法定量。三聚氰胺在1～50μg/mL范围内,具有良好的线性关系(R2=1),在添加质量浓度为5～20mg/kg范围内,三聚氰胺添加回收率在72.8%～87.6%,RSD(n=6)为1.5%～4.0%,最低检测限为0.54mg/kg。A high performance liquid chromatography method was developed for the quantitative analysis of melamine in chicken eggs based on solid phase extraction.Samples were extracted with mixed trichloroacetic acid/ead acetate solution for 20 min,followed by clean up on a PCX solid phase extraction column.The chromatographic separation was achieved on a TC-C18 column（4.6 mm×150 mm,5μm）using a mobile phase composed of perfluorooctane sulfonate and citric acid buffer（10：90,V/V）at a flow rate of 1.0 mL/min.Melamine was detected at 240 nm and quantitatively determined using an external calibration method.The injection volume was 20μL.The linear range of the developed method was between 5 mg/kg and 20 mg/kg（R2=1）.The average recoveries for melamine were ranged from 72.8%to 87.6%with a relative standard deviation between 1.5%and 4.0%（n=6）at the spiked levels of 5,10 mg/kg and 20 mg/kg.The limit of detection for melamine was 0.54 mg/kg.

关 键 词：三聚氰胺 高效液相色谱 固相萃取 鸡蛋 

分 类 号：TS207.5[轻工技术与工程—食品科学]