Simultaneous determination of 15 steroidal oral contraceptives in water using solid-phase disk extraction followed by high performance liquid chromatography-tandem mass spectrometry

摘要

A rapid, accurate and sensitive method for simultaneous determination of 15 steroidal hormones including four estrogens (estrone, 17 beta-estradiol, 17 alpha-ethynylestradiol, estriol) and eleven progestogens (17 beta-estradiol-3-benzoate, 19-norethindrone, gestodene. levonorgestrel, medroxyprogesterone, cyproterone acetate, megestrol-17-acetate, progesterone, norethindrone acetate, chlormadinone-17-acetate, and hydroxy progesterone caproate) in environmental waters was developed by coupling solid-phase disk extraction (SPDE) to ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) with electrospray ionization. Among three types of extraction tested (C-8 SPDE, C-18 SPDE and C-18 SPE), the most satisfactory result was achieved using C-18 SPDE for its satisfactory recovery (75.6 to 101.4%) and short extraction time (15 min for 1 L deionised water). The validity of this method was investigated and good analytical performance for all the analytes was obtained, including low limits of method detection (0.5-3.4 ng/L) and excellent linear dynamic range (1.0-50.0 ng/L). The method was applied to determine the steroidal hormones in 10 environmental waters including tap water, river water, lake water and waste water in Beijing. No progestogen was detected in all samples and estrone, estriol, 17 alpha-ethynylestradiol were found in most samples at levels between 1.8 and 127.9 ng/L.