Simple and quick determination of analgesics and other contaminants of emerging concern in environmental waters by on-line solid phase extraction coupled to liquid chromatography-tandem mass spectrometry

J Chromatogr A. 2016 May 13:1446:27-33. doi: 10.1016/j.chroma.2016.04.009. Epub 2016 Apr 4.

Abstract

A simple and quick analytical method has been developed for the determination of pharmaceutical compounds in water. An on-line solid-phase extraction (SPE) coupled to liquid chromatography-tandem mass spectrometry (LC-MS/MS) method has been optimized to determine 7 contaminants of emerging concern in environmental waters at ngL(-1) levels. This procedure requires minimal sample handling and small sample volume (900μL) with a total running time of 18min. Several SPE parameters were evaluated and optimized in order to achieve a high sample throughput. Therefore sample volume, carryover and reusability of the cartridges were evaluated. Performance characteristics were evaluated and good linearity was obtained (R(2)>0.98). Recoveries were evaluated in spiked samples at three concentrations and the values ranged from 71 to 104%. Intra and inter-day precision was lower than 10 and 13% respectively. Limits of quantification were equal to or lower than 10ngL(-1), except for 1,7-dimethylxanthine (20ngL(-1)) and ibuprofen (50ngL(-1)). The method was applied to 20 environmental water samples, and ibuprofen was the compound most widely detected at concentrations up to 42.06μgL(-1), whereas the other compounds were detected in fewer samples at lower concentrations (up to 15.99μgL(-1)).

Keywords: Environmental water; LC–MS/MS; On-line SPE; Pharmaceutical compounds.

MeSH terms

  • Analgesics / analysis*
  • Chromatography, High Pressure Liquid / methods
  • Fresh Water / chemistry
  • Ibuprofen / analysis
  • Solid Phase Extraction / methods
  • Tandem Mass Spectrometry / methods
  • Water Pollutants, Chemical / analysis*

Substances

  • Analgesics
  • Water Pollutants, Chemical
  • Ibuprofen