title: Trace analysis of selected hormones and sterols in river sediments by liquid chromatography-atmospheric pressure chemical ionization-tandem mass spectrometry.
abstract: In this paper, development and optimization of new LC-MS method for determination of twenty selected hormones, human/animal and plant sterols in river sediments were described. Sediment samples were prepared using ultrasonic extraction and clean up with silica gel/anhydrous sodium sulphate cartridge. Extracts were analyzed by liquid chromatography-linear ion trap-tandem mass spectrometry, with atmospheric pressure chemical ionization. The optimized extraction parameters were extraction solvent (methanol), weight of the sediment (2 g) and time of ultrasonic extraction (3× 10 min). Successful chromatographic separation of hormones (estriol and estrone, 17α- and 17β-estradiol) and four human/animal sterols (epicoprostanol, coprostanol, α-cholestanol and β-cholestanol) that have identical fragmentation reactions was achieved. The developed and optimized method provided high recoveries (73-118%), low limits of detection (0.8-18 ng g(-1)) and quantification (2.5-60 ng g(-1)) with the RSDs generally lower than 20%. Applicability of the developed method was confirmed by analysis of six river sediment samples. A widespread occurrence of human/animal and plant sterols was found. The only detected hormone was mestranol in just one sediment sample.
authors.affiliation: Faculty of Technology and Metallurgy, University of Belgrade, Karnegijeva 4, 11000 Belgrade, Serbia. Electronic address: imatic@tmf.bg.ac.rs.
authors.forename: Ivana
authors.initials: I
authors.lastname: Matić
authors.affiliation: Faculty of Technology and Metallurgy, University of Belgrade, Karnegijeva 4, 11000 Belgrade, Serbia.
authors.forename: Svetlana
authors.initials: S
authors.lastname: Grujić
authors.affiliation: Faculty of Technology and Metallurgy, University of Belgrade, Karnegijeva 4, 11000 Belgrade, Serbia.
authors.forename: Zorica
authors.initials: Z
authors.lastname: Jauković
authors.affiliation: Faculty of Technology and Metallurgy, University of Belgrade, Karnegijeva 4, 11000 Belgrade, Serbia.
authors.forename: Mila
authors.initials: M
authors.lastname: Laušević
mesh_terms: D002853:Chromatography, Liquid / Q000379:methods; D019015:Geologic Sediments / Q000032:analysis*; D006728:Hormones / Q000032:analysis*; D045483:Rivers / Q000737:chemistry; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods; D013261:Sterols / Q000032:analysis*; D053719:Tandem Mass Spectrometry / Q000379:methods; D014874:Water Pollutants, Chemical / Q000032:analysis*
chemical_list: D006728:Hormones; D013261:Sterols; D014874:Water Pollutants, Chemical
keywords: Hormones; LC–MS; Sediments; Steroids; Sterols