Trace analysis of 28 steroids in surface water, wastewater and sludge samples by rapid resolution liquid chromatography–electrospray ionization tandem mass spectrometry

• Published in: Journal of Chromatography A Vol. 1218; no. 10; pp. 1367 - 1378
• Main Authors: Liu, Shan, Ying, Guang-Guo, Zhao, Jian-Liang, Chen, Feng, Yang, Bin, Zhou, Li-Jun, Lai, Hua-jie
• Format: Journal Article
• Language: English
• Published: Amsterdam Elsevier B.V 11.03.2011; Amsterdam; New York: Elsevier; Elsevier
• Subjects: Analysis methods; Analytical chemistry; Applied sciences; Chemistry; Chromatographic methods and physical methods associated with chromatography; Chromatography, Liquid - methods; Exact sciences and technology; Other chromatographic methods; Other industrial wastes. Sewage sludge; Other wastewaters; Pollution; Reproducibility of Results; Rivers - chemistry; RRLC–MS/MS; Sensitivity and Specificity; Sewage - chemistry; Sludge; Solid Phase Extraction; Spectrometry, Mass, Electrospray Ionization; Steroids; Steroids - analysis; Steroids - chemistry; Surface water; Tandem Mass Spectrometry - methods; Waste Disposal, Fluid - methods; Wastes; Wastewater; Wastewaters; Water Pollutants, Chemical - analysis; Water Pollutants, Chemical - chemistry; Water treatment and pollution; China, People's Rep; RRLC–MS/MS; Wastewater; Sludge; Surface water; Steroids; Trace analysis; Steroid; Validation; Solid phase extraction; Tandem mass spectrometry; Chemical analysis; Coupled method; HPLC chromatography; RRLC―MS/MS; Solvent extraction; Sewage sludge; Electrospray; Waste water; Chemical enrichment; Ultrasound assisted extraction; Sample preparation; Water pollution; Mass spectrometry; Ultrasound; Quantitative analysis
• ISSN: 0021-9673; 1873-3778
• DOI: 10.1016/j.chroma.2011.01.014

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).