高效液相色谱-串联质谱法检测生物样品中6种雌激素

Determination of six estrogens in biological samples by HPLC-MS/MS

建立了雌酮、雌二醇、雌三醇、己烯雌酚、己烷雌酚和炔雌醇6种雌激素在生物体中的HPLC-MS/MS分析方法。采用加速溶剂萃取、固相萃取技术进行提取、富集及净化,有效降低了基质的干扰。以甲醇-0.1%氨水溶液为流动相,以C18色谱柱进行分离,质谱采用电喷雾负离子扫描模式,6种雌激素的回收率为88%～104%,相对标准偏差在1.3%～8.3%之间。雌酮、雌二醇、雌三醇在生物体中的方法检出限0.35ng/g;己烯雌酚、己烷雌酚、17α-乙炔基雌二醇在生物体中的方法检出限为0.13ng/g。方法适用于生物体内雌激素的分析和检测。

A liquid chromatography-tandem mass spectrometry method has been established for the simultaneous determination of 6 estrogens,including Estrone,17β-estradiol,estriol,diethylstilbestrol,hexestrol,17α-ethinylestradiol in biological samples.This method used accelerated solvent extraction and solid-phase extraction technology were employed for extract and purification to reduce the matrix interference.The separation was performed on a C18 column with methonal-0.1 % ammonia,and the scan mode of mass spectrometry was negative ions.The recoveries of six estrogens were 88%～104% in biological samples,with relative standard deviations of 1.3%～8.3%.The method detection limits were 0.35ng/g in aquatic products for estrone、estradiol and estriol,0.13ng/g for diethylstilbestrol、hexestrol and 17α-Ethinylestradiol.The result showed that this method was applicable to estrogens monitoring in aquatic products.