Dissolution Method Development and Validation of Dabigatran Etexilate Mesylate Capsules by RP-HPLC

摘要

ABSTRACT The article aims at developing simple, fast and effective dissolution method for Dabigatran etexilate mesylate capsules by RP-HPLC and validate as per ICH guidelines. The optimized RP-HPLC method for dissolution studies uses a reverse phase column, Phenomenex Luna C18 (250 X 4.6 mm;5μ), a mobile phase of triethylammonium phosphate buffer (pH 3.0):acetonitrile in the proportion of 40:60 v/v, diluent as 0.01N HCl, flow rate of 1.0ml/min, injection volume as 20µl. and a detection wavelength of 341nm using a UV detector. The optimized dissolution conditions include, 0.01N HCl as dissolution media, apparatus as USP Type 1 Basket, rpm as 100, dissolution media temperature as 37±0.5ºC, dissolution volume as 500ml, dissolution time point as 30mts, working concentration of standard and sample as 5µg/ml and a detection wavelength of 341 nm. The developed method resulted in Dabigatran etexilate exhibiting linearity in the range 1.25-10μg/ml. System precision and intra-day precision is exemplified by relative standard deviation of 1.59% and 2.21% respectively. Method was found to be rugged/inter day precise as %RSD was found to be 3.25. Percentage Mean recovery was found to be greater than 80% at all the three levels by absolute method during accuracy studies. LOD and LOQ for Dabigatran etexilate were found to be 0.05ng/ml and 5ng/ml respectively. Hence it can be concluded that effective dissolution method by RP-HPLC is developed and validated as per ICH guidelines which can be applicable in various pharmaceutical industries. Keywords: Dabigatran etexilate, Dissolution, RP-HPLC, ICH guidelines, Validation