title: Simultaneous determination of pharmaceuticals and some of their metabolites in wastewaters by high performance liquid chromatography with tandem mass spectrometry.
abstract: The present work describes the development of a sensitive and reliable analytical method based on solid-phase extraction followed by analysis using liquid chromatography with tandem mass spectrometry for the simultaneous determination of pharmaceuticals from antibiotics (fluoroquinolones, sulfonamides, and their N(4)-acetyl metabolites, and trimethoprim as sulfonamides synergist) and anthelmintics groups. SPE was optimized using different cartridges (Strata-X, Oasis HLB, Strata C18 -E, Isolute C18 , SampliQ C8 /Si-SCX). The highest recovery was achieved using Strata X cartridge (>80%) with good reproducibility (RSDs < 5%) despite various physicochemical properties of the compounds. Investigated analytes were identified and quantitatively determined by liquid chromatography with tandem mass spectrometry using multiple reaction monitoring. The method was shown to be linear over the concentration range of 0.05-30 μg/L for febantel and albendazole, and 0.10-60 μg/L for all other pharmaceuticals. Correlation coefficients were >0.99 for all compounds except for sulfamethazine (0.98). In order to demonstrate the applicability of the developed method, wastewater from the veterinary industry was analyzed. Results evidenced the presence of febantel, praziquantel, albendazole, enrofloxacin, sulfamethazine, and sulfadiazine.
authors.affiliation: Department of Analytical Chemistry, Faculty of Chemical Engineering and Technology, University of Zagreb, Zagreb, Croatia.
authors.forename: Martina
authors.initials: M
authors.lastname: Periša
authors.forename: Sandra
authors.initials: S
authors.lastname: Babić
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D015394:Molecular Structure; D004364:Pharmaceutical Preparations / Q000737:chemistry* / Q000302:isolation & purification / Q000378:metabolism; D052616:Solid Phase Extraction; D053719:Tandem Mass Spectrometry / Q000379:methods*; D062065:Wastewater / Q000737:chemistry*; D014874:Water Pollutants, Chemical / Q000737:chemistry* / Q000302:isolation & purification / Q000378:metabolism
chemical_list: D004364:Pharmaceutical Preparations; D062065:Wastewater; D014874:Water Pollutants, Chemical
keywords: Anthelmintics; Fluoroquinolones; Sulfonamide metabolites; Wastewater analysis; solid-phase extraction