STABILITY-INDICATING VALIDATED REVERSED PHASE-HIGH PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR SIMULTANEOUS DETERMINATION OF COBICISTAT AND ATAZANAVIR SULFATE IN BULK AND PHARMACEUTICAL DOSAGE FORM
Abstract
ABSTRACT
Objective: A simple, rapid, precise, accurate, and economical stability-indicating reversed phase-high performance liquid assay method was developed
and validated for simultaneous estimation of cobicistat (COB) and atazanavir (ATV) sulfate in bulk drugs and their combined commercial tablets.
Methods: The method has shown adequate separation of COB and ATV from their degradation products. Separation was achieved on a Luna
CN (250 mm × 4.6 mm, 5 μm column at a detection wavelength of 239 nm) using a mobile phase consists of o-phthaldialdeyde (Ph2.5) IX buffer,
acetonitrile, and methanol in the ratio of 40:40:20 in an isocratic elution mode at a flow rate of 1 ml/min.
Results: The retention times for COB and ATV sulfate were found to be 3.606 and 6.113 min, respectively. COB and ATV sulfate, their combination
drug product was subjected to acid, base, neutral hydrolysis, thermal, and photolytic stress conditions. Thus, stressed samples were analyzed by the
proposed analytical method. Validation of the proposed analytical method was carried out as per ICH guidelines Q2R1. Quantitation was achieved
with UV detection at 239 nm based on peak area with linear calibration curves at concentration ranges 50-600 μg/ml for COB and 100-1200 μg/ml for
ATV sulfate (R2 = 0.999 for both drugs). The limits of detection were 0.25 μg/ml and 0.5 μg/ml for COB and ATV sulfate, respectively.
Conclusion: The method was found to be specific and stability indicating as no interfering peaks of degradants and excipients were observed. The
proposed method is hence suitable for application in quality-control laboratories for quantitative analysis of both the drugs individually and in
combination dosage forms since it is simple and rapid with good accuracy and precision.
Keywords: Stability-indicating assay, Reversed phase-high performance liquid, Cobicistat, Atazanavir sulfate, Forced degradation studies.
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References
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