Determination of sterols and steroid hormones in surface water and wastewater using liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry

• Published in: Microchemical journal 2017-11, Vol.135, p.39-47
• Main Authors: Jauković, Zorica D., Grujić, Svetlana D., Matić Bujagić, Ivana V., Laušević, Mila D.
• Format: Article
• Language: English
• Subjects: LC-MS/MS; Steroid hormones; Sterols; Surface water; Wastewater
• ISSN: 0026-265X; 1095-9149
• DOI: 10.1016/j.microc.2017.07.011

The development and optimization of an analytical method for simultaneous extraction, determination and reliable confirmation of twenty steroids from different classes (human/animal and plant sterols, and natural and synthetic steroid hormones) in environmental water and wastewater at ngL−1 levels are described. Water samples were prepared using solid-phase extraction and extracts were analyzed by liquid chromatography-linear ion trap-tandem mass spectrometry. Improved instrumental method was developed for complete chromatographic separation of analytes with identical fragmentation reactions, based on the use of a single C8 column and acetonitrile as organic solvent in the mobile phase. The optimized method provided high recoveries (70–114%) for both water matrices with the RSDs generally lower than 20%. Low limits of detection were achieved for both surface water (0.7–15.0ngL−1) and wastewater (1.7–15.0ngL−1). Method displayed good linearity in the tested concentration ranges. As a result of method application to real water samples, cholesterol was detected in all fifteen analyzed river water samples (in the concentration range 176–5162ngL−1) and all seven wastewater samples (1092–4808ngL−1). Also, coprostanol, stigmasterol, campesterol, β-sitosterol and sitostanol were found in the investigated samples. Steroid hormones were not detected in any of the analyzed water samples. [Display omitted] •Novel LC-MS method for analysis of sterols and steroid hormones in surface and wastewater was developed.•Chromatographic separation of steroids with identical fragmentations was achieved.•Optimized SPE method provided high recoveries and low limits of detection.•Six sterols and no hormones were found in 15 surface and 7 wastewater samples.•Cholesterol was the most abundant sterol, detected in all water samples.