文献类型：期刊文献

中文题名：基于QuEChERS前处理技术和弱阳离子交换色谱的牛奶和奶粉中三聚氰胺的快速检测方法

英文题名：Rapid analysis of melamine in milk and milk powder using QuEChERS approach coupled with weak cation exchange chromatography

作者：魏杰[1];郭志谋[2];沈爱金[2];章飞芳[1];梁鑫淼[1,2]

机构：[1]华东理工大学药学院,上海200237;[2]中国科学院大连化学物理研究所,辽宁大连116023

年份：2011

卷号：29

期号：7

起止页码：687

中文期刊名：色谱

外文期刊名：Chinese Journal of Chromatography

收录：CSTPCD;;Scopus;WOS:【ESCI(收录号:WOS:000435249000020)】；北大核心:【北大核心2008】；CSCD:【CSCD2011_2012】；PubMed;

基金：国家科技支撑计划项目(No.2009BADB9B02);上海市科委重点基础研究项目(No.09JC1403900)

语种：中文

中文关键词：QuEChERS方法;弱阳离子交换色谱;快速分析;三聚氰胺;牛奶;奶粉

外文关键词：QuEChERS； weak cation exchange chromatography（WCX）； rapid analysis； melamine； milk； milk powder；

摘要：应用QuEChERS前处理技术,并结合弱阳离子交换色谱,建立了牛奶和奶粉中三聚氰胺的快速检测方法。样品使用医用酒精（乙醇含量75%）和一种新型脂肪吸附（LAS）材料超声振荡处理,在沉淀（吸附）蛋白质和脂肪的同时提取三聚氰胺,然后经8 000r/min离心,上清液过膜直接分析。色谱分析在弱阳离子交换色谱柱（WCX）上进行,采用2mmol/L pH为3.8的磷酸二氢钾水溶液为流动相,在5min内实现分离分析。结果表明,该方法在0.02~20mg/L内线性相关系数大于0.999 9。在1~50mg/kg添加浓度范围内,牛奶的平均回收率为98.9%~105.2%,相对标准偏差（RSD）为0.9%~3.4%;奶粉的平均回收率为86.4%~102.9%,RSD为1.5%~6.7%。本方法的检出限为0.05mg/kg（牛奶）和0.1mg/kg（奶粉）。整个分析检测过程没有使用有毒有害有机溶剂,是一种绿色的分析方法。
A simple,rapid method for the determination of melamine in milk and milk powder was developed using QuEChERS approach coupled with weak cation exchange chromatography（WCX）.The samples were extracted and cleaned-up by medicinal alcohol and lipid adsorbent（LAS） simultaneously,then centrifuged and filtered for high performance liquid chromatographic（HPLC） analysis.The separation was performed on a WCX column（150 mm×4.6 mm,5 μm） with 2 mmol/L KH2PO4（pH 3.8） as mobile phase.The flow rate was 1.5 mL/min and the detection wavelength was 208 nm.The injection volume was 20 μL and the column temperature was 30 ℃.Under the optimized conditions,good linearity was obtained in the range of 0.02-20 mg/L with a correlation coefficient（r2） of 0.999 9.For samples spiked with melamine standard in the range of 1-50 mg/kg,the average recoveries of standard in the milk and milk powder were 98.9%-105.2% and 86.4%-102.9%,respectively.The relative standard deviations were 0.9%-3.4% and 1.5%-6.7%,respectively.The limits of detection（LOD,S/N≥3） were 0.05 mg/kg（milk） and 0.1 mg/kg（milk powder）.The present method is green due to not use of the toxic organic solvents.