engleski

Development of multirezidual LC-MS/MS method for the assessment of trace levels of pharmaceuticals in aquatic environment

Pharmaceuticals or active pharmaceutical ingredients (APIs) are chemical compounds designed to help regulate the specific metabolic pathways in living organisms. Due to the high biological activity, exposure to these highly biologically active compounds in the aquatic environment could lead to adverse effects on non-target species. Consequently, having in mind a continuous increase in their production and consumption, APIs represent one of the most prominent categories of so-called emerging pollutants. The aim of this work was to develop and validate a novel multiresidue method for the quantitative determination of trace levels of 44 APIs and their metabolites in aqueous matrices, using liquid chromatography tandem mass spectrometry (LC- MS/MS). To develop a robust and reliable analytical protocol, a careful optimization of the key steps included in the sample preparation and instrumental analysis was performed. The optimized method involved solid-phase extraction using Oasis HLB cartridges and LC-MS/MS analysis employing positive electrospray ionization and highly specific MRM detection, based on two selected precursor/product ion transitions for each analyte. The chromatographic separation of selected analytes was achieved using a Synergi Polar column with water and methanol, both containing 0.1% (v/v) formic acid, as eluting solvents. Accurate quantification of ng/L levels of target APIs was achieved using isotopically labeled surrogate standards. Validation parameters included determination of the method linearity range, extraction and evaporation recoveries, matrix effect, method precision and accuracy. The developed analytical method was applied to assess the API concentrations in wastewaters of the city of Zagreb and the Sava River.

biota ; pharmaceuticals ; bioaccumulation

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