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Simultaneous determination of ten nonsteroidal anti-inflammatory drugs from drinking water, surface water and wastewater using micro UHPLC-MS/MS with on-line SPE system.
Journal article

Simultaneous determination of ten nonsteroidal anti-inflammatory drugs from drinking water, surface water and wastewater using micro UHPLC-MS/MS with on-line SPE system.

  • Márta Z MS Metabolomics Laboratory, Instrumentation Center, Research Centre for Natural Sciences, Hungarian Academy of Sciences, Magyar tudósok krt.2, H-1117 Budapest, Hungary; Department of Inorganic and Analytical Chemistry, Faculty of Chemical Technology and Biotechnology, Budapest University of Technology and Economics, Szent Gellért tér 4, H-1111, Budapest, Hungary.
  • Bobály B School of Pharmaceutical Sciences, University of Geneva, University of Lausanne, Centre Médical Universitaire (CMU), Rue Michel-Servet 1, 1206, Geneva, Switzerland.
  • Fekete J Department of Inorganic and Analytical Chemistry, Faculty of Chemical Technology and Biotechnology, Budapest University of Technology and Economics, Szent Gellért tér 4, H-1111, Budapest, Hungary.
  • Magda B MS Metabolomics Laboratory, Instrumentation Center, Research Centre for Natural Sciences, Hungarian Academy of Sciences, Magyar tudósok krt.2, H-1117 Budapest, Hungary.
  • Imre T MS Metabolomics Laboratory, Instrumentation Center, Research Centre for Natural Sciences, Hungarian Academy of Sciences, Magyar tudósok krt.2, H-1117 Budapest, Hungary.
  • Szabó PT MS Metabolomics Laboratory, Instrumentation Center, Research Centre for Natural Sciences, Hungarian Academy of Sciences, Magyar tudósok krt.2, H-1117 Budapest, Hungary. Electronic address: szabo.pal@ttk.mta.hu.
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  • 2018-08-04
Published in:
  • Journal of pharmaceutical and biomedical analysis. - 2018
Analytical method development
LC–MS/MS
Micro LC
Nonsteroidal anti-inflammatory drugs
On-line SPE
Anti-Inflammatory Agents, Non-Steroidal
Chromatography, High Pressure Liquid
Drinking Water
Limit of Detection
Solid Phase Extraction
Tandem Mass Spectrometry
Waste Water
Water Pollutants, Chemical
English A simple, accurate and sensitive micro UHPLC-MS/MS method was developed and validated for the simultaneous determination of 10 nonsteroidal anti-inflammatory drugs (NSAIDs) from different environmental matrices. The micro LC ‒ on-line SPE method described in this study allowed to determine the selected drugs at ultra-trace levels without the most commonly used complex off-line SPE sample preparation procedures. The presented method is capable of reaching satisfactory low LOQ values with analysing the sample directly after being diluted with water. In order to attain high sensitivity, mass spectrometry was carefully optimized for the analysis of the drugs. Fenoprofen, flurbiprofen and naproxen were found to produce CO2 loss during ionization, forming intense [M-H-CO2]- ions instead of [M-H]-. All the other compounds were analyzed through their [M+H]+ and [M-H]- ions. Effect of mobile phase pH on ionization was also studied. Lower pH resulted in higher ion intensities. For this reason, a reversed phase chromatographic separation was applied at pH 3.1 with formic acid at concentration of 0.01%. Matrix effects have been evaluated during validation and sample dilution was optimized focusing on the lowest achievable LOQ values. Analytes were determined from drinking water directly, from surface water and wastewater following dilution with purified water by 2 : 8 (v/v) and 1 : 9 (v/v), respectively. Finally, the method was applied to real sample analysis.
Language
  • English
Open access status
closed
Identifiers
Persistent URL
https://sonar.rero.ch/global/documents/169576
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