ACHIEVING ANALYTICAL EXCELLENCE: QBD-DRIVEN DEVELOPMENT AND VALIDATION OF REVERSED PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY-BASED SIMULTANEOUS ESTIMATION METHOD FOR AZILSARTAN MEDOXOMIL AND CILNIDIPINE
DOI:
https://doi.org/10.22159/ajpcr.2025v18i11.56812Keywords:
Azilsartan, Cilnidipine, Quality by design, Box–Behnken design, Antihypertensive agents, Simultaneous estimation, Method development, Validation, Design Expert 13Abstract
Objectives: This article aimed to develop a method for the simultaneous estimation of Azilsartan medoxomil (AZT) and cilnidipine (CIL) by incorporating a quality-by-design approach, which is used to develop the most accurate and precise analytical method in comparison with traditional method development.
Methods: At the initial phase, researchers conducted high-performance liquid chromatography (HPLC) trials as per the traditional method development protocol, and factors such as mobile phase, flow rate, and column temperature were taken into consideration for finalizing the most suitable trial. Quality-by-Design approach is then implemented for further study. As per the Box–Behnken design (BBD) system, the method was optimized. The most suitable optimized solution is used for validation.
Results: Based on traditional method development, methanol and 0.1% v/v ortho phosphoric acid selected as a mobile phase in an 82:18 ratio, the flow rate was selected as 1 mL/min, and column temperature was selected at 40°C. Based on these factors, 17 HPLC runs were performed as per BBD protocol the p-values for quadratic model for all factors was found <0.0500, which shows the quadratic model is best for proposed study by which method get optimized, and the validation was carried out on the most appropriate optimized solution. The R2 for AZT and CIL was found to be 0.9998 and 0.9999, respectively. The method was linear for both the drugs, and accuracy was found to be 100.45% for AZT and 99.49% for CIL. Other validation parameters were also found within limits.
Conclusion: At the end of the study, it was found that the developed method was accurate, precise, linear, specific, and reproducible. Method is cost-effective and can be able to used for routine analysis in laboratories as well as in industries.
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