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Analysis of ecologically relevant pharmaceuticals in wastewater and surface water using selective solid phase extraction and UPLC/MS/MS
Citation:
BATT, A., M. KOSTICH, AND J. M. LAZORCHAK. Analysis of ecologically relevant pharmaceuticals in wastewater and surface water using selective solid phase extraction and UPLC/MS/MS. Analytical Chemistry. American Chemical Society, Washington, DC, 80(13):5021-5030, (2008).
Impact/Purpose:
This work describes the development and limited application of a rapid, sensitive analytical method utilizing a single extraction and multiple injection ultra performance liquid chromatography/tandem mass spectrometry (UPLC/MS/MS) needed to accurately identify and quantify trace levels of over fifty selected active pharmaceutical ingredients (APIs) and metabolites of interest in wastewater effluent and surface water. This method will also be used in future studies to assess the exposure of ecosystems to APIs present in wastewater treatment plants.
Description:
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 ultra performance 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 minutes and SPE-LC/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.