QBD APPROACH FOR THE DEVELOPMENT AND VALIDATION OF STABILITY INDICATING RP-HPLC METHOD FOR SIMULTANEOUS ESTIMATION OF FORMOTEROL FUMARATE AND ACLIDINIUM BROMIDE IN PRESSURIZED METER DOSE INHALER

A Quality design approach to method development involves method goal identification, method scouting and evaluation, method selection, and risk assessment. The present study describes the risk-based HPLC method development and validation of Formoterol fumarate and Aclidinium bromide in a pharmaceutical dosage form. The chromatographic conditions were optimized with the Design Expert software 11.0 version i.e., Kromasil C18 (250×4.6 mm, 5 µm) Mobile phase used was 0.01N Kh2po4 (pH :3.0) (52.4%): Acetonitrile (47.6%), flow rate was found to be 1.0ml/min with retention times of formoterol 2.456 min and Aclidinium 3.573min. The developed method was found to be linear in the range of Formoterol 1.5-9μg/ml, aclidinium 50-300μg/ml with a correlation coefficient of 0.999 for both drugs. The % RSD of intraday and inter-day precision for Formoterol 0.3 & 1.0, Aclidinium 0.7 & 0.4. The robustness values were less than 2%.The assay was found to be 99.91%&99.99% for formoterol and aclidinium bromide. The method validation parameters were in the prescribed limit as per ICH guidelines. Stress studies reveal that both drugs were degraded more in acidic conditions than in alkaline, neutral, oxidative, photolytic and thermal conditions. Hence, the proposed method was stability indicating, using QbD approach all the method parameters were better understood that, reduces the time and cost of the analysis.