固相萃取-HPLC法测定水样中雌激素残留  

Determination of Estrogens in Drinking Water by Combining Solid-phase Extraction with High Performance Liquid Chromatography

作　　者：李龙飞[1] 金莹[2] 赵晓磊[1] 何金兴[1] 

机构地区：[1]齐鲁工业大学食品与生物工程学院,山东济南250353 [2]黄岛出入境检验检疫局,山东青岛266555

出　　处：《食品研究与开发》2013年第23期60-64,共5页Food Research and Development

基　　金：山东省优秀中青年科学家科研奖励基金(BS2012SW018)

摘　　要：采用固相萃取与高效液相色谱联用技术,对水中己烯雌酚、己烷雌酚和双烯雌酚残留进行提取、净化、分析,建立了同时测定水样中3种雌激素残留的检测方法。以溶胶凝胶技术合成的聚合物为固相萃取填充材料,探究了不同pH、富集流速、洗脱流速、洗脱溶剂等条件对试验的影响。结果表明,在优化的条件下,该方法对3种雌激素的最低检测限(S/N=3)为0.1μg/L^0.29μg/L,测定样品在3个水平下的加标回收率为70.4%~80.1%,相对标准偏差(RSD)为3.5%~7.8%。方法简便,可靠,适用于日常饮水中雌激素的残留检测。The objective of this research was to establish a method of detecting the residues of diethylstilbestrol , hexestrol and dienestrol which had been affirmed pernicious exceedingly in drinking water by combining solid-phase extraction （SPE） with high performance liquid chromatography （HPLC）. In this work, three estrogens were extracted by the adsorption material compounded on the base of sol-gel technology and filled in extraction small column. Some important parameters, such as sample pH, eluent species, enrichment and elution flow rate, which might influence extraction efficiency were optimized. The experimental results indicated that the detection limit（S/N=3）of the developed method could reach 0.1μg/L-0.29μg/L under the optimized conditions. The recoveries of three estrogens from the water samples at three spiked levels ranged from 70.4%to 80.1%with RSD in the range of 3.5 %-7.8 %. The method was simple, rapid, and reliable for routine analysis of drinking water.

关 键 词：固相萃取 高效液相色谱 雌激素 饮用水 

分 类 号：O657.72[理学—分析化学] R123[理学—化学]