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Stability Indicating HPTLC Method for Estimation of Dabigatran Etexilate Mesylate in its Pharmaceutical Dosage Form


Pintu B. Prajapati, Arti J. Rakholiya, Kunjan B. Bodiwala, Bhavin P. Marolia, Shailesh A. Shah

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Keywords

High-performance thin-layer chromatography (HPTLC), dabigatran etexilate mesylate (DEM), stress degradation, method validation

Abstract

Dabigatran etexilate mesylate is an anticoagulant drug. Dabigatran demonstrated its efficacy for prophylaxis and treatment of thromboembolic event during orthopaedic surgery and curative treatment of hypercoagulability in atrial fibrillation. The present study deals with the development and validation of a stability-indicating high performance thin-layer chromatography (HPTLC) method for the estimation of Dabigatran etexilate mesylate using TLC plates precoated with silica gel 60 F254 as stationary phase and toluene: ethyl acetate: methanol: formic acid (3:4:3:0.2, v/v/v/v) as the mobile phase. The drug was subjected to stress conditions such as hydrolysis, oxidation, photolysis, neutral and dry heat. Degradation products produced as a result of the stress conditions did not interfere with the detection of DEM, therefore the proposed method can be considered stability-indicating. DEM showed degradation under hydrolytic, oxidative, photolytic and dry heat conditions. DEM (Rf 0.47 ± 0.02) and its degradation products were well resolved. The wavelength selected for quantitation was 314 nm. The method was linear in the concentration range 50-250 ng/spot with a correlation coefficient of 0.9955. The %RSD for repeatability of peak area measurement was found to be 0.62 and %RSD for repeatability of sample application was found to be 0.75. The % RSD of intraday and interday precisions were 0.91- 1.5 and 1.21- 1.7 respectively. The accuracy (recovery) was found to be in the range of 99.45-100.37 %. The developed method was applied for assay of marketed formulations and the results were found to be good agreement with labelled claim of formulations.