DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD FOR SIMULTANEOUS ESTIMATION OF AZILSARTAN MEDOXIMIL AND CHLORTHALIDONE IN BULK FORM AND FORMULATION USING QUALITY BY DESIGN
Abstract
Objective: Development of an accurate, precise, robust, sensitive, economical and rapid isocratic reversed-phase high-performance liquid chromatography (RP-HPLC) method complying quality by design (QbD) trends for simultaneous estimation of azilsartan medoximil and chlorthalidone in bulk and formulation form and validation of the method as per ICH guidelines.
Methods: The simultaneous estimation of the drugs-azilsartan and chlorthalidone was performed using C8 column having dimensions 150×4.6 mm×5 µm, injection volume 10 µl, flow rate 0.8 ml/min., runtime 10 min., column temperature 20 oC, sampler temperature 5 °C and ultraviolet detection using a photodiode array detector at 220 nm as constant. The optimized method was validated as per ICH guidelines.
Results: The retention times for chlorthalidone and azilsartan medoxomil were 2.4 min. and 5.1 min. respectively with resolution 17. The method was validated as per the ICH guidelines. The linearity of chlortalidone and azilsartan medoxomil was in the range of 6.3 to 15 µg/ml and 20 to 48 µg/ml respectively. The potency of the formulation was found to be 108.12 % and 98.20 % respectively, which are within acceptable limits as per IP.
Conclusion: Method validation results have proven the method to be selective, precise, accurate, and robust, as well as stability indicating. The C8 column used for analysis gave encouraging results with better resolution and less retention time. This method can be successfully applied for the routine analysis involving the determination of content uniformity and dissolution profiling as well as stability study by the industry.
Keywords: RP-HPLC, QbD, ICH, Azilsartan medoximil, Chlorthalidone.
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References
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