title: Development and optimization of the determination of pharmaceuticals in water samples by SPE and HPLC with diode-array detection.
abstract: This paper describes the development, optimization, and validation of a method for the determination of five pharmaceuticals from different therapeutic classes (antibiotics, anthelmintics, glucocorticoides) in water samples. Water samples were prepared using SPE and extracts were analyzed by HPLC with diode-array detection. The efficiency of 11 different SPE cartridges to extract the investigated compounds from water was tested in preliminary experiments. Then, the pH of the water sample, elution solvent, and sorbent mass were optimized. Except for optimization of the SPE procedure, selection of the optimal HPLC column with different stationary phases from different manufacturers has been performed. The developed method was validated using spring water samples spiked with appropriate concentrations of pharmaceuticals. Good linearity was obtained in the range of 2.4-200 μg/L, depending on the pharmaceutical with the correlation coefficients >0.9930 in all cases, except for ciprofloxacin (0.9866). Also, the method has revealed that low LODs (0.7-3.9 μg/L), good precision (intra- and interday) with RSD below 17% and recoveries above 98% for all pharmaceuticals. The method has been successfully applied to the analysis of production wastewater samples from the pharmaceutical industry.
authors.affiliation: Department of Analytical Chemistry, Faculty of Chemical Engineering and Technology, University of Zagreb, Zagreb, Croatia.
authors.forename: Dragana Mutavdžić
authors.initials: DM
authors.lastname: Pavlović
authors.forename: Danijela
authors.initials: D
authors.lastname: Ašperger
authors.forename: Dijana
authors.initials: D
authors.lastname: Tolić
authors.forename: Sandra
authors.initials: S
authors.lastname: Babić
mesh_terms: D002851:Chromatography, High Pressure Liquid; D004364:Pharmaceutical Preparations / Q000032:analysis*; D052616:Solid Phase Extraction; D014874:Water Pollutants, Chemical / Q000737:chemistry*
chemical_list: D004364:Pharmaceutical Preparations; D014874:Water Pollutants, Chemical
keywords: HPLC; Optimization; Pharmaceuticals; Production wastewater; SPE