摘要
建立了三种天然雌激素和三种人工合成雌激素在水体和沉积物中的HPLC-MS/MS分析方法。该方法运用固相萃取技术进行富集及净化,有效降低了基质的干扰,六种雌激素在水体中的回收率为76.4%-110.3%,沉积物中的回收率为63.7%-88.5%,相对标准偏差在1.04%-9.23%间。质谱采用负离子扫描模式,定量的碎片离子分别是：雌酮：269.02/144.99;雌二醇：271.04/182.96;雌三醇：287.03/170.94;己烯雌酚：267.20/251.12;己烷雌酚：269.15/119.06;17α-乙炔基雌二醇：295.20/145.07。雌酮、雌二醇、雌三醇在水样和沉积物中的方法检出限分别为0.3ng/L和0.075×10-9;己烯雌酚、己烷雌酚、17α-乙炔基雌二醇在水样和沉积物中的方法检出限分别为0.135ng/L和0.037×10-9。研究表明,所建立的方法适用于水体和沉积物中该类雌激素的分析和检测。
A method for detecting three types of natural estrogen and synthetic estrogen in water and sediment was established by HPLC-MS/MS.This method is to use the solid-phase extraction technology for the enrichment and purification to reduce the matrix interference.The recovery of six estrogens was 76.4%~110.3% in water,63.7%~88.5% in sediment,with the relative standard deviations of 1.04%～9.23%.The scan mode of mass spectrometry with negative ions is used,The fragment ions used for quantitative analysis were estrone,269.02/144.99,Estradiol,271.04/182.96,estriol,287.03/170.94,diethylstilbestrol,267.20/251.12,hexestrol,269.15/119.06,17α-Ethinylestradiol,and 295.20/145.07.The method detection was 0.3 ng/L and 0.075×10-9 in water and sediment for estrone,estradiol and estriol,0.135 ng/L and 0.037×10-9 for diethylstilbestrol,hexestrol and 17α-Ethinylestradiol.The result showed that the method could be applicable for the estrogens monitoring in water and sediment.
出处
《海洋环境科学》
CAS
CSCD
北大核心
2011年第3期424-427,共4页
Marine Environmental Science
基金
国家海洋局青年海洋科学基金(20090507)
