DEVELOPMENT AND VALIDATION OF A STABILITY INDICATING RP HPLC METHOD FOR SIMULTANEOUS ESTIMATION OF METFORMIN HCL AND DAPAGLIFLOZIN IN FIXED DOSE COMBINATION TABLET
Main Article Content
Keywords
Metformin HCl, Dapagliflozin, RP‑HPLC, method validation, ICH guidelines, fixed‑dose combination.
Abstract
A fixed‑dose combination of Metformin HCl (MET) and Dapagliflozin (DAPA) is widely used for the management of type 2 diabetes mellitus. A simple, precise, and economical analytical method is required for routine quality control of this combination.
To develop and validate a simple, accurate, and robust reversed‑phase high‑performance liquid chromatography (RP‑HPLC) method for the simultaneous estimation of MET and DAPA in bulk and pharmaceutical tablet formulation.
Chromatographic separation was achieved on an Inertsil ODS‑3V C18 column (250 mm × 4.6 mm, 5 μm particle size) using an isocratic mobile phase consisting of phosphate buffer (pH 3.5) and acetonitrile (50:50 v/v) at a flow rate of 1.0 mL/min. The detection wavelength was set at 233 nm (isobestic point). The method was validated according to ICH Q2(R1) guidelines for system suitability, linearity, accuracy, precision, ruggedness, robustness, LOD, and LOQ.
The retention times of MET and DAPA were 1.893 min and 5.262 min, respectively, with a total run time of 8.0 min. The method was linear over the concentration ranges of 10–20 μg/mL for MET and 32–64 μg/mL for DAPA, with correlation coefficients (r²) of 0.999 for both drugs. Mean recoveries ranged from 99.06% to 101.58%, with %RSD <2%. Intra‑day and inter‑day precision (%RSD) were <1% for both drugs. The LOD and LOQ were 0.57 and 1.72 μg/mL for MET, and 1.22 and 3.72 μg/mL for DAPA, respectively. The method was robust to small changes in flow rate and wavelength, and ruggedness was confirmed by different analysts. Assay results for marketed tablets were 99.70% (MET) and 102.00% (DAPA) of label claim.
A simple, precise, and accurate RP‑HPLC method was successfully developed and validated for the simultaneous estimation of MET and DAPA in bulk and tablet dosage form. The method is suitable for routine quality control analysis in pharmaceutical laboratories.
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Dnyaneshwar Korde
Department of Quality Assurance, Government College of Pharmacy, Amravati, India – 444604
Amol Ghodke
Maharashtra Poly. (D. Pharm) Institute, Nilanga - 413521, India
Dr. K. S. Patil
Department of Quality Assurance, Government College of Pharmacy, Amravati, India – 444604
