气相色谱质谱法测定尿及河底泥中的环境雌激素

Determination of Environmental Estrogens in Urine and Bed Mud by Gas Chromatography-Mass Spectrometry

报道了尿及河底泥中环境雌激素(壬基酚、双酚A、己烯雌酚、17α 乙炔基雌二醇)和内源性雌激素(17α 雌二醇、17β 雌二醇、雌三醇、雌酮)的气相色谱 质谱(GC MS)测定法。尿样经盐酸溶液水解后用固相萃取(SPE)柱浓缩净化,底泥样品用甲醇 乙酸乙酯萃取。被测组分经五氟丙酸酐(PFPA)衍生化后用GC MS进行定性定量检测。该法测定的峰面积的日内相对标准偏差为1 22%～5 55%,检出限为0 05～1 27μg/L(或μg/kg)。被测组分的加标回收率除尿样中17α 乙炔基雌二醇和己烯雌酚分别为25 4%和71 0%外,其余为86 7%～111 2%。

A gas chromatographicmass spectrometric method (GCMS) for the simultaneous determination of environmental estrogens (including 4nonylphenol, bisphenol A, diethylstilbestrol and 17αethinylestradiol) and endogenous estrogens (including 17αestradiol, 17βestradiol, estriol and estrone) in urine and bed mud is reported. Urine samples were hydrolyzed with HCl and cleaned up by reversedphase C18 cartridge. Bed mud samples were extracted using a mixture of methanolethyl acetate (3∶7, v/v). After derivatization with pentafluoropropionic anhydride (PFPA), the derivatives were determined by GCMS. The intraday relative standard deviations of the peak area were 122%-555% and the detection limits ranged from 005 to 127 μg/L (or μg/kg) and the recoveries ranged from 867% to 1112% except for the diethylstilbestrol and 17αethinylestradiol in urine samples, whose recoveries were 710% and 254%, respectively.