State Key Laboratory of Organic Geochemistry, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, 511 Kehua Street, Tianhe, Guangzhou 510640, China.
J Chromatogr A. 2011 Mar 11;1218(10):1367-78. doi: 10.1016/j.chroma.2011.01.014. Epub 2011 Jan 12.
A sensitive rapid resolution liquid chromatography-tandem mass spectrometry (RRLC-MS/MS) method, combined with solid-phase extraction, ultrasonic extraction and silica gel cartridge cleanup, was developed for 28 steroids including 4 estrogens (estrone (E1), 17β-estradiol (E2), 17α-ethynyl estradiol (EE2), diethylstilbestrol (DES)), 14 androgens (androsta-1,4-diene-3,17-dione (ADD), 17α-trenbolone, 17β-trenbolone, 4-androstene-3,17-dione, 19-nortestoserone, 17β-boldenone, 17α-boldenone, testosterone (T), epi-androsterone (EADR), methyltestosterone (MT), 4-hydroxy-androst-4-ene-17-dione (4-OHA), 5α-dihydrotestosterone (5α-DHT), androsterone (ADR), stanozolol (S)), 5 progestagens (progesterone (P), ethynyl testosterone (ET), 19-norethindrone, norgestrel, medroxyprogesterone (MP)), and 5 glucocorticoids (cortisol, cortisone, prednisone, prednisolone, dexamethasone) in surface water, wastewater and sludge samples. The recoveries of surface water, influents, effluents and sludge samples were 90.6-119.0% (except 5α-DHT was 143%), 44.0-200%, 60.7-123% and 62.6-138%, respectively. The method detection limits for the 28 analytes in surface water, influents, effluents and freeze-dried sludge samples were 0.01-0.24 ng/L, 0.02-1.44 ng/L, 0.01-0.49 ng/L and 0.08-2.06 ng/g, respectively. This method was applied in the determination of the residual steroidal hormones in two surface water of Danshui River, 12 wastewater and 8 sludge samples from two wastewater treatment plants (Meihu and Huiyang WWTPs) in Guangdong (China). Ten analytes were detected in surface water samples with concentrations ranging between 0.4 ng/L (17β-boldenone) and 55.3 ng/L (5α-DHT); twenty analytes in the wastewater samples with concentrations ranging between 0.3 ng/L (P) and 621 ng/L (5α-DHT); and 12 analytes in the sludge samples with concentrations ranging between 1.6 ng/g (E1) and 372 ng/g (EADR).
建立了一种灵敏的快速分辨液相色谱-串联质谱法（RRLC-MS/MS），结合固相萃取、超声提取和硅胶柱净化，用于检测包括 4 种雌激素（雌酮（E1）、17β-雌二醇（E2）、17α-乙炔基雌二醇（EE2）、己烯雌酚（DES））、14 种雄激素（雄甾-1,4-二烯-3,17-二酮（ADD）、17α- trenbolone、17β-trenbolone、4-雄烯-3,17-二酮、19-去甲睾酮、17β-boldenone、17α-boldenone、睾酮（T）、表雄酮（EADR）、甲基睾酮（MT）、4-羟基-雄甾-4-烯-17-二酮（4-OHA）、5α-二氢睾酮（5α-DHT）、雄酮（ADR）、司坦唑醇（S））、5 种孕激素（孕酮（P）、乙炔睾酮（ET）、19-去甲炔诺酮、去氧孕烯、甲羟孕酮（MP））和 5 种糖皮质激素（皮质醇、皮质酮、泼尼松、泼尼松龙、地塞米松）在地表水、废水和污泥样品中的残留情况。地表水、进水、出水和污泥样品的回收率分别为 90.6-119.0%（5α-DHT 除外，为 143%）、44.0-200%、60.7-123%和 62.6-138%。该方法在地表水、进水、出水和冻干污泥样品中 28 种分析物的方法检出限分别为 0.01-0.24ng/L、0.02-1.44ng/L、0.01-0.49ng/L 和 0.08-2.06ng/g。该方法应用于检测中国广东省淡水河两个地表水、两个污水处理厂（美湖和惠阳污水处理厂）的 12 个废水和 8 个污泥样品中残留的甾体激素。在地表水样品中检测到 10 种分析物，浓度范围为 0.4ng/L（17β-boldenone）至 55.3ng/L（5α-DHT）；在废水样品中检测到 20 种分析物，浓度范围为 0.3ng/L（P）至 621ng/L（5α-DHT）；在污泥样品中检测到 12 种分析物，浓度范围为 1.6ng/g（E1）至 372ng/g（EADR）。
