摘要
提出了气相色谱-质谱法测定水中雌二醇、雌酮、雌三醇、戊酸雌二醇、己烯雌酚、乙炔雌二醇、双酚A和壬基酚等8种雌激素含量的方法。样品经乙酸乙酯提取和HLB小柱净化后,所得净化液中的雌激素与三甲基硅基化剂(TMS)或七氟丁酸酐(HFBA)进行衍生化反应产物用正己烷定容。在气相色谱分离中用DB-5MS毛细管柱为固定相,在质谱分析中采用全扫描和选择离子监测模式。8种雌激素的峰面积与质量浓度在20.0～1 000μg.L-1范围内呈线性关系,检出限(3S/N)在0.1～0.5μg.L-1之间。方法用于水中雌激素的测定,回收率在71%～103%之间,相对标准偏差(n=6)在4.2%～15%之间。
A method of GC-MS for simultaneous determination of 8 estrogens, i. e. , estradiol, estrone, estriol, estradiol valerate, diethylstilbestrol, ethynyl estradiot, bisphenol A and 4-nonylphenol in water was proposed. Sample was extracted with ethyl acetate and purified on the HLB column, then derivatized with TMS or HFBA. The derivatized product was dissolved with n-hexane. The DB-SMS capillary column was used for GC separation and the full-scanning mode and selected ion monitoring mode were adopted in MS determination. Linear relationship between values of peak area and mass concentration of 8 estrogens were obtained in the same range of 20. 0--1 000μg .L ^-1, with detection limits （3S/N） in the range of 0.1-0. 5/μg .L^-1. The proposed method was applied to the analysis of water sample, giving values of recovery in the range of 71%--103% and RSD＇s （n=6） in the range of 4. 2%-15%.
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2012年第7期797-799,802,共4页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
江苏省2009年环保科研计划项目(2009035)
作者简介
王荟（1976-），女，江苏宿迁人，工程师，主要从事有机污染物分析。E-mail：wh_nju@163．com
