摘要
建立了固相微萃取（SPME）-高效液相色谱（HPLC）联用测定食品中己烯雌酚（DES）的方法。考察了萃取纤维头、萃取时间、解吸时间和盐的添加对萃取效果的影响。在此基础上,采用正交试验,以解析液组成、萃取液pH和搅拌速度为3因素筛选出了最佳固相微萃取条件。该分析方法的线性范围为0.02~2.0μg/mL,工作曲线线性良好,线性相关系数R=0.9961。方法检出限为0.006μg/mL,测定结果的变异系数小于5%。此方法应用于鸡肉组织和奶粉中己烯雌酚检测,三个加标水平的回收率为81.9%~93.1%。
A novel method of solid-phase microextraction（SPME）coupled with high performance liquid chromatography（HPLC）was developed for the determination of diethylstilbestrol（DES）in food.The experimental conditions of SPME were optimized,including extraction fiber,extraction time,desorption time and ionic strength.An orthogonal test design was used to optimize the desorption solvent,pH value and stirring rate.This method showed a good linear relationship in the range of 0.02～2.0μg/mL,the linear correlation coefficient was 0.9961,the coefficient of variation was less than 5% and the detection limit was 0.006μg/mL.The method was applied to the determinations of DES in chicken as food and milk power.The recoveries of spiked DES in real samples ranged from 81.9%~ 93.1%.
出处
《化学研究与应用》
CAS
CSCD
北大核心
2011年第5期639-643,共5页
Chemical Research and Application
基金
浙江省自然科学基金项目(Y4090258)
宁波市自然科学基金项目(2010A610191)
宁波大学学科基金项目(xk109071)
