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Simultaneous detection and quantification of parecoxib and valdecoxib in canine plasma by HPLC with spectrofluorimetric detection: development and validation of a new methodology

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Abstract

Parecoxib is the injectable prodrug of valdecoxib, a cicloxygenase-2 selective drug, currently used in human medicine. Recent studies have suggested both its excellent clinical effectiveness and wide safety profile. The aim of the present study was to develop and validate a new high-performance liquid chromatography (HPLC) with spectrofluorimetric detection method to quantify parecoxib and valdecoxib in canine plasma. Several parameters both in the extraction and the detection method were evaluated. The applicability of the method was determined by administering parecoxib to one dog: the protocol provided the expected pharmacokinetic results. The final mobile phase was acetonitrile: AcONH4 (10 mM; pH 5.0) 55:45, v/v, with a flow rate of 0.4 mL min−1, and excitation and emission wavelengths of 265 and 375 nm, respectively. The analytical column was a reverse-phase C18 ODS2 3-μm particle size. Protein precipitation in acidic medium followed by two successive liquid–liquid steps was carried out. The best extraction solvent was cyclohexane:Et2O (3:2, v/v) that gave recoveries ranging from 81.1% to 89.1% and from 94.8% to 103.6% for parecoxib and valdecoxib, respectively. The limits of quantification were 25 and 10 ng mL−1 for parecoxib and valdecoxib, respectively. The chromatographic runs were specific with no interfering peaks at the retention times of the analytes, as confirmed by HPLC–mass spectrometry experiments. The other validation parameters were in agreement with the European Medicines Evaluation Agency and International Conference on Harmonisation guidelines. In conclusion, this method (extraction, separation and applied techniques) is simple and effective. This is the first time that use of a HPLC with spectrofluorimetric detection technique to simultaneously detect parecoxib and valdecoxib in plasma has been reported. This technique may have applications for pharmacokinetic studies.

In vivo metabolism of the prodrug parecoxib in the active ingredient valdecoxib

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Abbreviations

CX:

Celecoxib

DFU:

[5,5-Dimethyl-3-(3-fluorophenyl)-4-(4-methylsulphonyl)phenyl-2(5H)-furanone]

PX:

Parecoxib

RX:

Rofecoxib

VX:

Valdecoxib

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Acknowledgements

None of the authors has any financial or personal relationships that could inappropriately influence or bias the content of the paper. The authors wish to thank Pfizer (Groton, CT, USA) for supplying pure analytical standards of PX and VX. The manufacturer of the agents under review was offered an opportunity to comment on this article. No comment was received concerning the scientific and editorial merit of the manuscript. This work was supported by athenaeum funds (ex 60% University of Pisa). The preparation of manuscript was not supported by any external funding. Authors acknowledged to Dr E. Owen (University of Queensland, Australia) the English editing of the manuscript.

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Authors and Affiliations

  1. Department of Pharmaceutical Science, University of Pisa, via Bonanno 6, 56126, Pisa, Italy

    G. Saccomanni, S. Del Carlo, C. Manera & M. Macchia

  2. Department of Veterinary Clinics, University of Pisa, Via Livornese (lato monte) 1, San Piero a Grado, 56010, Pisa, Italy

    M. Giorgi

  3. Department of Chemistry and Industrial Chemistry, University of Pisa, Via Risorgimento 35, 56126, Pisa, Italy

    A. Saba

Authors
  1. G. Saccomanni
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  2. M. Giorgi
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  3. S. Del Carlo
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  4. C. Manera
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  5. A. Saba
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  6. M. Macchia
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Corresponding author

Correspondence to M. Giorgi.

Additional information

G. Saccomanni and M. Giorgi have equally contributed to the study.

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Saccomanni, G., Giorgi, M., Del Carlo, S. et al. Simultaneous detection and quantification of parecoxib and valdecoxib in canine plasma by HPLC with spectrofluorimetric detection: development and validation of a new methodology. Anal Bioanal Chem 401, 1677–1684 (2011). https://doi.org/10.1007/s00216-011-5244-4

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  • DOI: https://doi.org/10.1007/s00216-011-5244-4

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