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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

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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.

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Acknowledgments

The authors thank Jojo Tibon for his contribution to the HRMS experiments.

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Authors and Affiliations

  1. Laboratori de l’Agència de Salut Pública de Barcelona, Avinguda Drassanes 13-15, 08001, Barcelona, Spain

    Antoni Rúbies, Lili Guo & Francesc Centrich

  2. Department de Química Analítica, Universitat de Barcelona, Martí Franquès 1-11, 08028, Barcelona, Spain

    Lili Guo & Mercè Granados

  3. CIBER of Epidemiology and Public Health (CIBERESP), 28029, Madrid, Spain

    Francesc Centrich

Authors
  1. Antoni Rúbies
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  2. Lili Guo
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  3. Francesc Centrich
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  4. Mercè Granados
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Correspondence to Antoni Rúbies.

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Rúbies, A., Guo, L., Centrich, F. et al. 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. Anal Bioanal Chem 408, 5769–5778 (2016). https://doi.org/10.1007/s00216-016-9679-5

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  • DOI: https://doi.org/10.1007/s00216-016-9679-5

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