Abstract

Darshit Trivedi, Kavita Desai, Jigar Patel^*

DOI : http://dx.doi.org/10.13005/ojc/380526

A chromatographic method was developed to determine the of assay of Obeticholic Acid with the help of Quality by design approach. QBD is a regulated technique for the process development. In Quality by Design, The method development starts with the specific intentions. A simple method was developed focusing on two critical quality attributes for development of the sturdy and polished method. The implication of self-sufficient factors was resolved using Fisher’s statistical test for Analysis of the Variance (ANOVA) model that was predicted. The aim of the present work is to develop a simple, precise, accurate method for the estimation of obeticholic acid by reverse phase chromatographic technique. Improved chromatographic conditions were observed on Thermo C18 column (150mm x 4.6mm5µm), using the mixture of Orthophosphoric acid (0.1 % OPA) and Acetonitrile (ACN) in the ratio of 55:45% v/v as mobile phase at the flow rate of 1.0mL/min. The column temperature was set at 25°C and wavelength for detection of moiety was 210nm. The system suitability parameters of the instrument used were found within acceptance criteria as per the ICH guidelines. Linearity study was carried out over a range from 100 ppm to 300 ppm and R2 value was found to be 0.9995. The precision study was calculated by injecting six samples of same concentration and the % Relative standard deviation was observed to be 0.3%. The mean percentage recoveries for 50%, 100% and 150% concentration were found to be 100.5%, 99.9% and 100.8% respectively. The percentage purity of the commercial sample assayed using the proposed method was found to be 99.8%. The developed method was validated according to ICH guidelines - Q2 (R1) and all the results were present within the acceptance criteria, Hence the proposed method can be employed for regular quality control analysis of obeticholic acid in bulk and pharmaceutical dosage forms.

Analytical Method development; Antipsychotic Drug; Chromatography; Design Expert; HPLC; Obeticholic Acid; QBD approach

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