ESTIMATION OF CELECOXIB IN HUMAN PLASMA BY RAPID AND SELECTIVE LC-MS/MS METHOD FOR A BIOEQUIVALENCE STUDY

  • Nirav P. Patel Bio-Analytical Laboratory, Cliantha Research India Ltd., Bodakdev, Ahmedabad-380054, Gujarat, India
  • Mallika Sanyal Kadi Sarva Viswavidyalaya, Sector-15, Ghandhinagar-382715, Gujarat, India
  • Pranav S. Shrivastav Department of Chemistry, School of Sciences, Gujarat University, Navrangpura, Ahmedabad-380009, Gujarat, India
  • Bhavin N. Patel Bio-Analytical Laboratory, Cliantha Research India Ltd., Bodakdev, Ahmedabad-380054, Gujarat, India

Abstract

Objective: A selective, sensitive and rapid liquid chromatography-tandem mass spectrometry (LC-MS/MS) assay has been developed for the determination of celecoxib (CXB) in negative ionization mode.

Methods: Celecoxib and celecoxib-D7 (CXB-D7) as internal standard (IS) were extracted from 300 µl human plasma by solid-phase extraction using strata-X SPE cartridges. Chromatographic separation was achieved on ACE C8-300 (50 × 4.0 mm, 3.0 μm) column using methanol-1.0 mmol ammonium acetate solution in 80:20 (v/v) ratio. The protonated precursor to product ion transitions studied for CXB and CXB-D7 were m/z 380.0 → 315.9 and 387.0 → 323.0, respectively.

Results: The limit of detection (LOD) and lower limit of quantitation of the method were 2.50 and 10.0 ng/ml respectively with a linear dynamic range of 10.0-4000 ng/ml for CXB. The intra-batch and inter-batch precision (% CV) and mean relative recovery across quality control levels is<7.2 % and 85.5 % respectively. Matrix effect in human plasma, expressed as IS-normalized matrix factor ranged from 0.99-1.03.

Conclusion: The method was successfully applied in healthy subjects using a single dose of 400 mg celecoxib capsules under fasting and fed conditions. The reproducibility in the measurement of study data is demonstrated by incurred sample reanalysis.

Keywords: Celecoxib, LC-MS/MS, Solid-phase extraction, Human plasma, Bioequivalence study, Incurred sample reanalysis

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Patel, N. P., M. Sanyal, P. S. Shrivastav, and B. N. Patel. “ESTIMATION OF CELECOXIB IN HUMAN PLASMA BY RAPID AND SELECTIVE LC-MS/MS METHOD FOR A BIOEQUIVALENCE STUDY”. International Journal of Pharmacy and Pharmaceutical Sciences, Vol. 10, no. 10, Oct. 2018, pp. 16-22, doi:10.22159/ijpps.2018v10i10.28289.
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