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20.0~1 000 μg·L-1范围内呈线性关系,检出限(3S/N)在0.1~0.5 μg·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 estradiol, 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-5MS 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 20.0-1 000 μg·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%.