衍生-气相色谱-质谱法测定水中痕量雌激素

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。

GC-MS Determination of Trace Amounts of Estrogens in Water with Derivatization

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%.