QbD Based Analytical Method Development and Validation for the Estimation of Remogliflozin etabonate and Vildagliptin in Bulk and in Their Dosage Form
Main Article Content
Abstract
Introduction: QbD based simple, accurate, precise, sensitive, economic and robust RP-HPLC method was successfully developed and validated for the simultaneous estimation of Remogliflozin etabonate and Vildagliptin in bulk and in tablet dosage forms. Linearity, detection limit, quantitation limit, accuracy, precision, robustness was considered for development and validation of HPLC method for Remogliflozin etabonate (RMO) and Vildagliptin (VLD) in bulk and in tablet dosage form.
Objectives: The objective of present research work is to apply Quality by Design (QbD) approach for developing a simple, economic, accurate, precise and reproducible analytical method and validate the performance methods as per ICH guidelines by using chromatographic technique (RP HPLC).
Methods: Reversed phase chromatography was carried out by using High Performance Liquid Chromatographic System (Analytical Technologies ltd, HPLC 3000 series) equipped with UV detector controlled by HPLC workstation software, using Cosmosil C 18 (250 mm x 4.6 mm; 5µm) HPLC Column. The chromatographic separation was carried out using mobile phase comprised of 10 mM KH2PO4 buffer pH 3 and methanol (10:90 %v/v) with flow rate 0.8 ml/min and response recorded by UV detector at 216 nm. Design expert used as software for evaluation of experimental design study (Stat-Ease Inc., Minneapolis, USA, Version 13.0). Due to high competence with a limited number of runs, Box Behnken Design (BBD) and response surface methodology model is used for present study. Three factors, two levels and five center points are selected for BBD, leads to 17 experimental runs, which were carried out. Standard and sample prepared and injected in to chromatographic system. Retention time, theoretical plates, and peak asymmetry, peak area, resolution were measured as responses. For coefficients and nature of the robustness was evaluated by ANOVA.
Results: Data of ANOVA analysis for selected responses, having P value less than 0.05 and F value more than 2.5 signifies the results of proposed approach. Also, the % RSD values were less than 2.0 for method repeatability and intermediate precision results, indicating high degree of precision of the method. The detection limits and quantitation limits were very low, which is indicate method is sensitive.
Conclusions: Experiments were conducted in HPLC and peak resolution was evaluated. All three variables selected found critical for peak separation. QbD based RP-HPLC methods for simultaneous estimation of Remogliflozin etabonate and Vildagliptin was developed and validated as per ICH guidelines. Experimental results proved that the HPLC methods are linear in the proposed working concentration range as well as specific, sensitive, accurate, precise and robust. The percent recovery results of dosage forms showing that the excipients have no interference in the determination. The proposed method can be applied to the routine analysis of Remogliflozin etabonate and Vildagliptin in quality control department of pharmaceutical industry.