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建立了固相萃取-超高效液相色谱串联质谱法(SPE-UPLC-MS/MS)同时测定环境水体中12种类固醇激素(雌酮、17α-雌二醇、17β-雌二醇、雌三醇、乙炔基雌二醇、睾酮、雄烯二酮、甲基睾酮、孕酮、炔诺酮、孕二烯酮、左炔诺孕酮)的分析方法。样品经C_(18)固相萃取柱净化和浓缩,采用多反应监测模式(MRM)进行分析。12种类固醇激素在1.0~200.0μg/L质量浓度范围内呈良好线性,相关系数r~2均不低于0.992,方法检出限(S/N=3)为1.22~87.5 ng/L。在5.0,50.0和200.0μg/L 3个添加水平下回收率为72.6~111.9%,相对标准偏差(RSD)均不高于12%。方法适用于不同水体中多种类固醇激素的痕量分析。
A solid-phase extraction coupled with ultra performance liquid chromatography-tandem mass spectrometry (SPE-UPLC-MS / MS) was developed for the simultaneous determination of 12 steroid hormones (estrone, 17α-estradiol, 17β-estradiol, Alcohol, ethinyl estradiol, testosterone, androstenedione, methyltestosterone, progesterone, norethindrone, gestodene, levonorgestrel). Samples were purified and concentrated on a C_ (18) solid phase extraction cartridge and analyzed using multiple reaction monitoring (MRM). The linearity of 12 steroid hormones was in the range of 1.0 ~ 200.0μg / L, the correlation coefficient was no less than 0.992, and the detection limit (S / N = 3) was 1.22 ~ 87.5 ng / L. The recoveries were 72.6 ~ 111.9% at 5.0, 5.0 and 200.0 μg / L, respectively, and the relative standard deviations (RSDs) were no higher than 12%. The method is suitable for the trace analysis of multiple steroid hormones in different water bodies.