A RAPID RP-HPLC METHOD DEVELOPMENT AND VALIDATION FOR THE QUANTITATIVE ESTIMATION OF DABIGATRAN ETEXILATE MESYLATE IN CAPSULES
Objective: To develop a rapid, sensitive, accurate, precise and linear Reverse Phase High Performance Liquid Chromatographic (RP-HPLC) method and validate as per ICH guidelines for the quantitative estimation of Dabigatran etexilate mesylate in capsules.
Methods: The optimized method uses a reverse phase column, Waters Symmetry C18 (250 X 4.6 mm; 5Î¼), a mobile phase of tri ethylammonium phosphate buffer (pH 2.5):acetonitrile in the proportion of 40:60 v/v, flow rate of 1.0 ml/min and a detection wavelength of 313 nm using a UV detector.
Results: The developed method resulted in Dabigatran etexilate mesylate eluting at 2.44 min. It exhibited linearity in the range 15-45Î¼g/ml. The precision is exemplified by relative standard deviation of 0.05%. Percentage mean recovery was found to be in the range of 98â€102, during accuracy studies. The limit of detection (LOD) and limit of quantitation (LOQ) was found to be 39.19Î¼g/ml and 118.88Î¼g/ml respectively.
Conclusion: A sensitive, rapid, accurate, precise and linear RP-HPLC method was developed and validated for the quantitative estimation of Dabigatran etexilate mesylate in capsules as per ICH guidelines and hence it can be used for the routine analysis in various pharmaceutical industries.
2. Eerenberg ES, Kamphuisen PW, Sijpkens MK, Meijers JC, Buller HR, Levi M. Reversal of Rivaroxaban and Dabigatran by prothrombin complex concentrate: a randomized, placebo-controlled, crossover study in healthy subjects. Circulation 2011;124:1573-9.
3. Ankit P, Sharad K, Ashim KS, Aarti Z, Seth AK. Spectro-photometric method for estimation of Dabigatran etexilate in bulk and its pharmaceutical dosage form. Pharm Sci Mon 2014;5:31-9.
4. Zhe-Yi Hu, Robert BP, Vanessa LH, Casey L. Conventional liquid chromatography/triple quadrupole mass spectrometry based metabolite identification and semi-quantitative estimation approach in the investigation of invitro Dabigatran etexilate metabolism. Anal Bioanal Chem 2013;405:1695-704.
5. Xavier D, Julie M, Laporte S, Patrick M, Thierry B. UPLC MS/MS assay for routine quantification of Dabigatran-a direct thrombin inhibitor in human plasma. J Pharm Biomed Anal 2012;25:152-6.
6. Mrinalini CD, Rupesh AB. Development and validation of stability-indicating RP-HPLC method for estimation of Dabigatran etexilate. J Adv Sci Res 2014;5:39-44.
7. Bernardi RM, Froehlich PE, Bergold AM. Development and validation of a stability indicating liquid chromatography method for the determination of Dabigatran etexilate in capsules. J AOAC Int 2013;96:37-41.
8. Sekhar reddy BRC, Vijaya bhaskar rao N. A stability indicating RP-HPLC method for estimation of Dabigatran in pure and pharmaceutical dosage forms. South Pacific J Pharma Bio Sci 2014;2:80-92.
9. International Conference on Harmonization of Technical Requirements for Registration of Pharmaceuticals for Human use. Validation of Analytical Procedures: Text and Methodology ICH Q2 (R1); 2005.