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

Zoltán Márta, Balázs Bobály, J. Fekete, Balázs Magda, T. Imre, P. Szabó

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4 Citations (Scopus)

Abstract

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.

Original languageEnglish
Pages (from-to)99-108
Number of pages10
JournalJournal of Pharmaceutical and Biomedical Analysis
Volume160
DOIs
Publication statusPublished - Oct 25 2018

Fingerprint

Online Systems
Online systems
Waste Water
Surface waters
Drinking Water
formic acid
Wastewater
Anti-Inflammatory Agents
Ions
Dilution
Ionization
Water
Fenoprofen
Pharmaceutical Preparations
Flurbiprofen
Naproxen
Mass spectrometry
Mass Spectrometry

Keywords

  • Analytical method development
  • LC–MS/MS
  • Micro LC
  • Nonsteroidal anti-inflammatory drugs
  • On-line SPE

ASJC Scopus subject areas

  • Analytical Chemistry
  • Pharmaceutical Science
  • Drug Discovery
  • Spectroscopy
  • Clinical Biochemistry

Cite this

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title = "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",
abstract = "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.",
keywords = "Analytical method development, LC–MS/MS, Micro LC, Nonsteroidal anti-inflammatory drugs, On-line SPE",
author = "Zolt{\'a}n M{\'a}rta and Bal{\'a}zs Bob{\'a}ly and J. Fekete and Bal{\'a}zs Magda and T. Imre and P. Szab{\'o}",
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T1 - 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

AU - Márta, Zoltán

AU - Bobály, Balázs

AU - Fekete, J.

AU - Magda, Balázs

AU - Imre, T.

AU - Szabó, P.

PY - 2018/10/25

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N2 - 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.

AB - 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.

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