A simple, sensitive, precise, accurate and robust high performance liquid chromatographic method has been developed for simultaneous estimation of saxagliptin (SAXA) and dapagliflozin (DAPA) in pharmaceutical formulation. Design of experiments (DoE) was applied for multivariate optimization of the experimental conditions of RP-HPLC method. Risk assessment was performed to identify the critical method parameters. Three independent factors; mobile phase composition, flow rate and column temperature were used to design mathematical models. Central composite design (CCD) was used to study the response surface methodology and to study in depth the effects of these independent factors. Desirability function was used to simultaneously optimize the retention time and resolution of SAXA and DAPA. The optimized and predicted data from contour diagram consisted of acetonitrile and ortho phosphoric acid (0.1%) in the ratio of 50:50 respectively, at a flow rate of 0.98 ml/min and column temperature 31.4 °C. Using these optimum conditions baseline separation of both drugs with good resolution and run time of less than 6 min were achieved. The optimized assay conditions were validated according to ICH guidelines. Hence, the results clearly showed that Quality by design approach could be successfully applied to optimize RP-HPLC method for simultaneous estimation of SAXA and DAPA.
Objective: A combination of hydrocortisone and tetracycline as topical ophthalmic ointment is used for skin irritations, eye infections, inflammation, skin infections, acne, and rashes. The objective of the current work is to a simple, rapid, accurate, and precise, stability-indicating reverse-phase liquid chromatographic method was developed for the simultaneous estimation of hydrocortisone and tetracycline in bulk and pharmaceutical dosage form. Methods: The separation was carried out in Discovery C18 column (250 × 4.6 mm, 5 μm) using mobile phase ratio of water (pH 2.2 adjusted with orthophosphoric acid):acetonitrile (40:60 v/v) in an isocratic elution mode with a flow rate of 1.0 ml/min at detection wavelength of 244 nm. The injection volume was 10 μl and the column temperature was set at 30°C. Results: The retention time for hydrocortisone and tetracycline was found to be 2.214 ± 0.001 min and 3.497 ± 0.001 min, respectively. Calibration curves were linear (r2=0.999) at a concentration range of 2.5–15 mg/ml for both hydrocortisone and tetracycline. The percentage recoveries were found to be 99.13–99.67% for hydrocortisone and 99.39–99.61% for tetracycline. Relative standard deviation was found to be 0.3% for both the drugs. Limit of detection and limit of quantification values of hydrocortisone and tetracycline were found to be 0.09 μg/ml and 0.27 μg/ml and 0.17 μg/ml and 0.52 μg/ml, respectively. The drugs were subjected to various stress conditions and found no interference of degraded products peak at the retention times of analyte peaks. Conclusion: A rapid and accurate reverse-phase high-performance liquid chromatographic method was developed for simultaneous estimation of hydrocortisone and tetracycline, and the method was validated as per the International Council for Harmonization guidelines. Hence, the developed method can be successfully applied for the simultaneous estimation of hydrocortisone and tetracycline in bulk and ointment formulation.
A high performance liquid chromatographic assay method was developed for the simultaneous estimation of Levodropropizine and Chlorpheniramine maleate in syrup dosage form. Chromatogram was run through Discovery C18 (4.6 x 150mm, 5µm) column. Mobile phase containing 0.01N KH2PO4 buffer (p H 2.8): acetonitrile (50:50) pumped through the column at a flow rate of 1.0 ml/min. The column temperature was maintained at 30°C and the detector was monitored at a wavelength of 215 nm. The injection volume was 10 µl with a total run time of 7 min. Retention time of Levodropropizine and Chlorpheniramine maleate were found to be 2.451 min and 3.595 min. The calibration curves were linear in the concentration range of 15-90 µg/ml and 1-6 µg/ml of Levodropropizine and Chlorpheniramine maleate respectively (r 2 = 0.999). The percentage recoveries were found to be 99.26 % for Levodropropizine and 99.43 % for Chlorpheniramine maleate. The limit of detection was found to be 0.33 μg/ml & 0.03 μg/ml and limit of quantitation was found to be 1.00 μg/ml & 0.09 μg/ml for Levodropropizine and Chlorpheniramine maleate respectively. The most effective RP-HPLC method was developed for the estimation of syrup dosage form containing Levodropropizine and Chlorpheniramine maleate. The developed method was validated for system suitability, specificity, accuracy, precision, linearity, limit of detection, limit of quantitation and robustness according to International Conference on Harmonization (ICH) guidelines.
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