Stability-indicating HPLC method development and validation for simultaneous estimation of metformin, dapagliflozin, and saxagliptin in bulk drug and pharmaceutical dosage form.

A simple, precise, and rapid stability-indicating reversed-phase-HPLC method was developed and validated for the estimation of metformin (MET), dapagliflozin (DAP), and saxagliptin (SAX) combination in bulk and tablet dosage forms. The proposed method uses a Kromasil C18 column (150 × 4.6 mm, 5 µm) with column oven temperature of 30°C and mobile phase containing a mixture of 60% phosphate buffer (pH = 3) and 40% acetonitrile. The flow rate was set at 1.0 mL/min, and the injection volume was 10 µL. The detection was carried out at 230 nm using a photodiode array detector, and the total run time was 4 min. The proposed method was validated according to International Council for Harmonisation (ICH) guidelines for specificity, linearity, precision, accuracy, robustness, and solution stability. The method is linear over the range of 125-750 µg/mL for MET, 1.25-7.5 µg/mL for DAP, and 0.625-3.75 µg/mL for SAX. The observed correlation coefficients (R2 ) for MET, DAP, and SAX are >0.999. The proposed method is precise, and the percentage relative standard deviation was found to be between 0.4 and 0.8. The observed percentage recoveries were between 98.51 and 100.80 for all three compounds. The product was subjected to stress conditions of acid, base, oxidative, thermal, and photolytic degradation. The product was found to degrade significantly in oxidative, acid, and base hydrolysis degradation conditions, and the degradation products were well determined from the active peaks, thus proving the stability-indicating power of the method. The developed and validated stability-indicating reversed-phase-HPLC method was appropriate for quantitative determination of these drugs in pharmaceutical preparations and also for quality control in bulk manufacturing.

A rapid RP-HPLC stability-indicating method development and validation of moxifloxacin hydrochloride-related substances in finished dosage forms.

A reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed and validated for the identification and quantification of moxifloxacin hydrochloride-related substances in finished dosage forms. Chromatographic separation was achieved on an Agilent C18 column (150 × 4.6 mm, 5 µm) with the mobile phase (0.01 M potassium dihydrogen orthophosphate as buffer and methanol in the ratio of 70:30) eluted in isocratic mode. The HPLC flow rate was 1.0 mL min-1 , and peaks were monitored at 230 nm using a photodiode array (PDA) detector. The column temperature was kept constant at 30°C, and the injection volume was 10 µL. The run time of the method was 16 min. The method was validated as per the International Conference on Harmonization (ICH) guidelines. Linearity was recorded at various concentrations ranging from 0.25 to 1.5 µg mL-1 for all the moxifloxacin impurities. Linearity, regression value, recovery, %relative standard deviation (RSD) of method precision values were found within the acceptance limits. The method for related substances (RS) in moxifloxacin was found to be specific, linear, accurate, precise, rugged, and robust. The validated method was suitable for the quantification of the RSs in moxifloxacin drug products. The method was applied in quality control lab for the analysis of moxifloxacin impurities in stability analysis.

Stability-indicating ultra performance liquid chromatography method development and validation for simultaneous estimation of metformin, linagliptin, and empagliflozin in bulk and pharmaceutical dosage form.

A rapid stability-indicating reversed phase-ultrapure liquid chromatography (RP-UPLC) was developed and validated for the estimation of metformin (MET), linagliptin (LIN), and empagliflozin (EMP) combination in bulk and tablet dosage form using Kromasil C18 column (2.1 × 50 mm, 1.8 µm) as a stationary phase and a mixture solution of 40% phosphate buffer (pH = 3) and 60% acetonitrile as mobile phase at a flow rate of 0.6 mL/min. The detection was performed at 248 nm using a photodiode array detector. The linearity, sensitivity, selectivity, robustness, specificity, precision, and accuracy were determined. The peak area response-concentration curve was rectilinear over the range of 50-150 (MET), 5-15 (LIN), and 10-30 µg/mL (EMP) with quantitation limits of 0.042 (MET), 0.023 (LIN), and 0.059 µg/mL (EMP). The proposed method was successfully validated for the determination of MET, LIN, and EMP simultaneously in combined tablet dosage form. The performance of the proposed method was compared with reported RP-UPLC methods and found to be rapid and economical. The developed and validated stability-indicating RP-UPLC method was appropriate for the quality control and drug analysis.