Simplified solid-phase extraction procedure combined with liquid chromatography tandem-mass spectrometry for multiresidue assessment of pharmaceutical compounds in environmental liquid samples

Abstract

To follow the twelve "green analytical chemistry" (GAC) principles, it is necessary to continuously develop analytical extraction and determination methodologies to assess the presence of micropollutants, such as pharmaceuticals, in environmental samples. A reduction in the analysis time and solvent quantity, which is one of the GAC principles, has been achieved through a simplified solid-phase extraction (SPE) procedure combined with high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the determination of twenty-three pharmaceuticals in liquid environmental samples using N-vinylpyrrolidone-divinylbenzene copolymer (OASIS HLB) cartridges. The optimal SPE conditions were studied. In these optimized conditions, 82.6% of the data have a median recovery above 70% for all compounds in each sample. The relative standard deviations (RSDs) were below 14.4% and 22.0% for intra- and inter-day repeatability, respectively. Method detection limits (MDLs) and method quantification limits (MQLs) ranged from 0.011 to 188ngL^-1 and from 0.033 to 628ngL^-1, respectively. The applicability of the method was evaluated in real samples from natural and conventional wastewater treatment plants (WWTPs), and results were obtained in concentration ranges from 0.013 to 91.5μgL^-1 and from 0.004 to 49.1μgL^-1, respectively.

Keywords: High-performance liquid chromatography–tandem mass spectrometry; Pharmaceuticals; Simplified solid-phase extraction; Wastewater.