title: Development of fast and robust multiresidual LC-MS/MS method for determination of pharmaceuticals in soils.
abstract: The aim of this study was to develop a simple extraction procedure and a multiresidual liquid chromatography-tandem mass spectrometry method for determination of a wide range of pharmaceuticals from various soil types. An extraction procedure for 91 pharmaceuticals from 13 soil types, followed by liquid chromatography-tandem mass spectrometry analysis, was optimized. The extraction efficiencies of three solvent mixtures for ultrasonic extraction were evaluated for 91 pharmaceuticals. The best results were obtained using acetonitrile/water (1/1 v/v with 0.1 % formic acid) followed by acetonitrile/2-propanol/water (3/3/4 v/v/v with 0.1 % formic acid) for extracting 63 pharmaceuticals. The method was validated at three fortification levels (10, 100, and 1000 ng/g) in all types of representative soils; recovery of 44 pharmaceuticals ranged between 55 and 135 % across all tested soils. The method was applied to analyze actual environmental samples of sediments, soils, and sludge, and 24 pharmaceuticals were found above limit of quantification with concentrations ranging between 0.83 ng/g (fexofenadine) and 223 ng/g (citalopram).
authors.affiliation: Faculty of Fisheries and Protection of Waters, South Bohemian Research Center of Aquaculture and Biodiversity of Hydrocenoses, University of South Bohemia in Ceské Budejovice, Zatisi 728/II, 389 25, Vodnany, Czech Republic. ogolovko@frov.jcu.cz.
authors.forename: Oksana
authors.identifier: http://orcid.org/0000-0003-3256-3054
authors.initials: O
authors.lastname: Golovko
authors.affiliation: Faculty of Fisheries and Protection of Waters, South Bohemian Research Center of Aquaculture and Biodiversity of Hydrocenoses, University of South Bohemia in Ceské Budejovice, Zatisi 728/II, 389 25, Vodnany, Czech Republic.
authors.forename: Olga
authors.initials: O
authors.lastname: Koba
authors.affiliation: Department of Soil Science and Soil Protection, Czech University of Life Sciences Prague, Kamycka 129, 16521, Prague 6, Czech Republic.
authors.forename: Radka
authors.initials: R
authors.lastname: Kodesova
authors.affiliation: Faculty of Fisheries and Protection of Waters, South Bohemian Research Center of Aquaculture and Biodiversity of Hydrocenoses, University of South Bohemia in Ceské Budejovice, Zatisi 728/II, 389 25, Vodnany, Czech Republic.
authors.forename: Ganna
authors.initials: G
authors.lastname: Fedorova
authors.affiliation: Faculty of Fisheries and Protection of Waters, South Bohemian Research Center of Aquaculture and Biodiversity of Hydrocenoses, University of South Bohemia in Ceské Budejovice, Zatisi 728/II, 389 25, Vodnany, Czech Republic.
authors.forename: Vimal
authors.initials: V
authors.lastname: Kumar
authors.affiliation: Faculty of Fisheries and Protection of Waters, South Bohemian Research Center of Aquaculture and Biodiversity of Hydrocenoses, University of South Bohemia in Ceské Budejovice, Zatisi 728/II, 389 25, Vodnany, Czech Republic.
authors.forename: Roman
authors.initials: R
authors.lastname: Grabic
mesh_terms: D019840:2-Propanol; D000097:Acetonitriles; D002853:Chromatography, Liquid / Q000379:methods*; D004784:Environmental Monitoring / Q000379:methods*; D004364:Pharmaceutical Preparations / Q000032:analysis*; D012722:Sewage / Q000737:chemistry; D012987:Soil / Q000737:chemistry; D012989:Soil Pollutants / Q000032:analysis*; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D000097:Acetonitriles; D004364:Pharmaceutical Preparations; D012722:Sewage; D012987:Soil; D012989:Soil Pollutants; D019840:2-Propanol; C032159:acetonitrile
keywords: Extraction efficiency; Extraction method; Liquid chromatography-tandem mass spectrometry; Matrix effects; Sediments; Sludge; Validation