European Journal of Biomedical and Pharmaceutical Sciences

QBD BASED NOVEL ANALYTICAL METHOD DEVELOPMENT AND VALIDATION FOR THE ESTIMATION OF CLOPIDOGREL AND ROSUVASTATIN IN BULK AND PHARMACEUTICAL DOSAGE FORMS BY RP-HPLC

Husna Kanwal Qureshi and Muneeza Fatima*

ABSTRACT

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 Clopidogrel and Rosuvastatin in bulk form and marketed pharmaceutical dosage form. The chromatographic conditions were optimized with the Design Expert software 11.0 version i.e., Phenomenex Gemini (250mm x 4.6mm) 5μm Particle size and Mobile phase used was Methanol and KH2PO4 buffer with pH 4.2 in the proportion of 20:80 % v/v, flow rate was found to be 1.0 ml/min with retention times of Clopidogrel and Rosuvastatin was found to be 2.474 min and 4.356 min respectively. The developed method was found to be linear in the range of Clopidogrel is 20-100 μg/ml and Rosuvastatin is 40-120 μg/ml with a correlation coefficient of 0.999 for both drugs. The % RSD of intraday and inter-day precision for Clopidogrel is 0.086 & 0.231 and Rosuvastatin is 0.59 & 0.274%. The robustness values were less than 2%. The assay was found to be 99.98% & 99.56% for Clopidogrel and Rosuvastatin respectively. The method validation parameters were in the prescribed limit as per ICH guidelines. Stress studies reveal that both drugs were degraded more in alkaline, thermal conditions than in acidic, oxidative and photolytic 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.

Keywords: Clopidogrel and Rosuvastatin, RP-HPLC, Quality by Design, Accuracy.