title: Analysis of ecologically relevant pharmaceuticals in wastewater and surface water using selective solid-phase extraction and UPLC-MS/MS.
abstract: A rapid and sensitive method has been developed for the analysis of 48 human prescription active pharmaceutical ingredients (APIs) and 6 metabolites of interest, utilizing selective solid-phase extraction (SPE) and ultraperformance liquid chromatography in combination with triple quadrupole mass spectrometry (UPLC-MS/MS). The single-cartridge extraction step was developed using a mixed mode reversed-phase/cation-exchange cartridge (Oasis MCX) and validated in both wastewater effluent and surface water. Recoveries for the majority of compounds ranged from 80% to 125%, with relative standard deviations generally below 15%. Analytes were quantified using a multiple injection analysis with four chromatographic runs, with a combined run time of 48 min and SPE-UPLC-MS/MS method detection limits ranging from 1.0 to 51 ng/L. The analysis of seven wastewater effluents and one surface water sample revealed at least one detection for 38 of the 54 compounds, with effluent concentrations ranging from 7 to 2950 ng/L and surface water concentrations ranging from 10 to 140 ng/L. This initial data demonstrates that a significant number of the selected target analytes are present in wastewater treatment plant discharges.
authors.affiliation: U.S. Environmental Protection Agency, Office of Research and Development, National Exposure Research Laboratories, 26 West Martin Luther King Drive, MS 642, Cincinnati, Ohio 45268, USA. batt.angela@epa.gov
authors.forename: Angela L
authors.initials: AL
authors.lastname: Batt
authors.forename: Mitch S
authors.initials: MS
authors.lastname: Kostich
authors.forename: James M
authors.initials: JM
authors.lastname: Lazorchak
mesh_terms: D002853:Chromatography, Liquid / Q000379:methods*; D004364:Pharmaceutical Preparations / Q000032:analysis*; D015203:Reproducibility of Results; D053719:Tandem Mass Spectrometry / Q000379:methods*; D014867:Water / Q000032:analysis*; D014874:Water Pollutants, Chemical / Q000032:analysis*
chemical_list: D004364:Pharmaceutical Preparations; D014874:Water Pollutants, Chemical; D014867:Water