title: Development of a SPE-HPLC-MS/MS method for the determination of most prescribed pharmaceuticals and related metabolites in urban sewage samples.
abstract: Based on regional prescription data several pharmaceuticals with variable amounts of prescription and corresponding metabolites were selected and analyzed in influent and effluent samples of the sewage treatment plant (STP) in Dresden, Germany. Pharmaceuticals of the following most prescribed therapeutic groups were chosen: antibiotics, antifungals, anticonvulsants, antipsychotics, antidepressants, and cardiovascular active compounds like beta blockers and angiotensin-converting enzyme inhibitors. To analyze the selected compounds, a multi-target method was developed and applied to 24-h composite wastewater samples for three single days in May and June 2014. The method was based on a cleanup of a sample with a volume of 1mL using solid phase extraction followed by a high performance liquid chromatography coupled to a tandem mass spectrometer. Analytes were separated in a 15min chromatographic separation and quantified using 23 Internal Standards and a calibration curve in 40-fold diluted blank urine. The limit of quantification varied between 50 and 200ng/L and for all analytes good accuracy and precision as well as linearity for the calibration curve with the correlation coefficient R(2) higher than 0.99 was reached. A total of 41 and 40 of the selected 55 analytes were detected and quantified in the influent and effluent samples of the studied STP, respectively. Valsartan was the compound with the highest maximum concentration in influent (27.1μg/L) and effluent (15.7μg/L). Furthermore, analytes like bezafibrate, candesartan, carbamazepine, gabapentin, metoprolol, levetiracetam, pregabalin and telmisartan as well as the metabolite O-desmethyl venlafaxine were detectable in influent and effluent samples, respectively, with a concentration higher than 1μg/L.
authors.affiliation: Institute of Clinical Pharmacology, Faculty of Medicine Carl Gustav Carus, Technische Universität Dresden, Fiedlerstraße 27, D-01307 Dresden, Germany; Research Association Public Health Saxony and Saxony Anhalt, Faculty of Medicine Carl Gustav Carus, Technische Universität Dresden, Fiedlerstraße 33, D-01307 Dresden, Germany. Electronic address: robert.gurke@tu-dresden.de.
authors.forename: Robert
authors.initials: R
authors.lastname: Gurke
authors.affiliation: Institute of Clinical Pharmacology, Faculty of Medicine Carl Gustav Carus, Technische Universität Dresden, Fiedlerstraße 27, D-01307 Dresden, Germany; Research Association Public Health Saxony and Saxony Anhalt, Faculty of Medicine Carl Gustav Carus, Technische Universität Dresden, Fiedlerstraße 33, D-01307 Dresden, Germany.
authors.forename: Julia
authors.initials: J
authors.lastname: Rossmann
authors.affiliation: Institute of Clinical Pharmacology, Faculty of Medicine Carl Gustav Carus, Technische Universität Dresden, Fiedlerstraße 27, D-01307 Dresden, Germany.
authors.forename: Sara
authors.initials: S
authors.lastname: Schubert
authors.affiliation: Research Association Public Health Saxony and Saxony Anhalt, Faculty of Medicine Carl Gustav Carus, Technische Universität Dresden, Fiedlerstraße 33, D-01307 Dresden, Germany.
authors.forename: Tobias
authors.initials: T
authors.lastname: Sandmann
authors.affiliation: Research Association Public Health Saxony and Saxony Anhalt, Faculty of Medicine Carl Gustav Carus, Technische Universität Dresden, Fiedlerstraße 33, D-01307 Dresden, Germany.
authors.forename: Martin
authors.initials: M
authors.lastname: Rößler
authors.affiliation: Institute of Clinical Pharmacology, Faculty of Medicine Carl Gustav Carus, Technische Universität Dresden, Fiedlerstraße 27, D-01307 Dresden, Germany.
authors.forename: Reinhard
authors.initials: R
authors.lastname: Oertel
authors.affiliation: Institute of Clinical Pharmacology, Faculty of Medicine Carl Gustav Carus, Technische Universität Dresden, Fiedlerstraße 27, D-01307 Dresden, Germany.
authors.forename: Joachim
authors.initials: J
authors.lastname: Fauler
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D002947:Cities; D016014:Linear Models; D004364:Pharmaceutical Preparations / Q000032:analysis*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D012722:Sewage / Q000737:chemistry*; D052616:Solid Phase Extraction / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods; D014874:Water Pollutants, Chemical / Q000032:analysis*
chemical_list: D004364:Pharmaceutical Preparations; D012722:Sewage; D014874:Water Pollutants, Chemical
keywords: Metabolites; Multi-target; Pharmaceutical; Regional prescription data; SPE-HPLC–MS/MS; Sewage