ESTIMATION OF CELECOXIB IN HUMAN PLASMA BY RAPID AND SELECTIVE LC-MS/MS METHOD FOR A BIOEQUIVALENCE STUDY
Keywords:Celecoxib, LC-MSMS, Solid-phase extraction, Human plasma, Bioequivalence study, Incurred sample reanalysis
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 Âµl human plasma by solid-phase extraction using strata-X SPE cartridges. Chromatographic separation was achieved on ACE C8-300 (50 Ã— 4.0 mm, 3.0 Î¼m) 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 â†’ 315.9 and 387.0 â†’ 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.
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