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Title: Analysis of non-steroidal anti-inflammatory drugs in milk using QuEChERS and liquid chromatography coupled to mass spectrometry: triple quadrupole versus Q-Orbitrap mass analyzers
Author: Rubies, Antoni
Rúbies Prat, Antoni
Centrich, F.
Granados i Juan, Mercè
Keywords: Cromatografia de líquids
Espectrometria de masses
Antiinflamatoris no esteroïdals
Liquid chromatography
Mass spectrometry
Nonsteroidal anti-inflammatory agents
Issue Date: 20-Jun-2016
Publisher: Springer Verlag
Abstract: We developed a Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) method for the high throughput determination of 10 non-steroidal anti-inflammatory drugs (NSAIDs) in milk samples using high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) with a triple quadrupole (QqQ) instrument and an electrospray ionization (ESI) source. The new extraction procedure is highly efficient, and we obtained absolute recoveries in the range 78.1-97.1 % for the extraction and clean-up steps. Chromatographic separation is performed in the gradient mode with a biphenyl column and acidic mobile phases consisting of water and acetonitrile containing formic acid. The chromatographic run time was about 12 min, and NSAID peaks showed a good symmetry factor. For MS/MS detection, we used multiple reaction monitoring (MRM) mode, using ESI in both positive and negative modes. Our method has been validated in compliance with the European Commission Decision 657/2002/EC, and we obtained very satisfactory results in inter-laboratory testing. Furthermore, we explored the use of a hybrid high resolution mass spectrometer, combining a quadrupole and an Orbitrap mass analyzer, for high resolution (HR) MS/MS detection of NSAIDs. We achieved lower NSAID quantification limits with Q-Orbitrap high resolution mass spectrometry (HRMS/MS) detection than those achieved with the QqQ instrument; however, its main feature is its very high selectivity, which makes HRMS/MS particularly suitable for confirmatory analysis.
Note: Versió postprint del document publicat a:
It is part of: Analytical and Bioanalytical Chemistry, 2016, vol. 408, num. 21, p. 5769-5778
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ISSN: 1618-2642
Appears in Collections:Articles publicats en revistes (Enginyeria Química i Química Analítica)

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