Abstract
Objective: The present study was conducted to develop a simple and precise analytical method for the estimation of ticagrelor in tablet formulation.Methods: Reverse Phase HPLC was used for method development and validation studies of ticagrelor. The optimum chromatographic conditions comprised of C18 column (Kromasil, 250×4.6 mm, 5 µ) as the stationary phase and aqueous buffer (containing 0.5 ml formic acid and triethylamine each in water) and acetonitrile in the ratio of 50:50 v/v as the mobile phase. The flow rate was 1.3 ml/min with detection at 256 nm and a run time of 6 min. Forced degradation studies were conducted and the isocratic mode was modified to a gradient mode to make the method stability indicating in nature.Results: The retention time of ticagrelor was 3.372 min. The linearity studies indicated that the range of the developed method was 20-90 ppm with a correlation coefficient of 0.9956. The method was specific with a percent mean recovery was found to be 99.93%.. The % RSD in the precision studies was 0.069. The validated method was applied to conduct the assay of ticagrelor in tablets and the with a percent mean recovery of 99.82%. The modified method was capable of resolving 13 related substances from the ticagrelor peak in the forced degradation studies.Conclusion: The developed and validated RP-HPLC isocratic method was simple, accurate and precise as per the ICH guidelines. It was suitable for the analysis of ticagrelor in bulk and tablet formulation. The modified gradient method can be used to resolve the in-process impurities and related substances and can be directly applied to liquid chromatography hyphenated with mass spectroscopy (LC/MS) studies with minor modifications for identification of related substances.
Highlights
Chromatography is a powerful separation method that finds application in all branches of science which is used for method development
High Performance Liquid Chromatography or High Pressure Liquid Chromatography (HPLC) is mainly a chromatography technique that can separate a mixture of compounds and is used in biochemistry and analytical chemistry to identify, quantify and purify the individual components of a mixture of analytes by distributing between the mobile phase and a stationary phase
Whatman Nylon w/GMF membrane filter pore size of 0.45μ was selected after comparing the peak area and concentration of centrifuged drug solution to other drug samples. Based on these observations acetonitrile: water; 90: 10 v/v was selected as the diluent for further studies
Summary
Chromatography is a powerful separation method that finds application in all branches of science which is used for method development. Ticagrelor is newly introduced into the market, the data on the qualitative and quantitative estimation of this drug is limited It is marketed as a tablet for the treatment of thrombosis. It reduces the rate of thrombotic cardiovascular events in patients with the acute coronary syndrome. Ticagrelor and its major metabolite reversibly interact with the platelet P2Y12 ADP-receptor to prevent signal transduction and platelet activation It is a white crystalline powder with an aqueous solubility of approximately 10μg/ml at room temperature. The marketed formulation of ticagrelor replaced clopidogrelcontaining formulations due to higher efficacy and lower side effects It was approved for use in the European Union by the European Commission on December 3, 2010, by the US Food and Drug Administration on July 20, 2011. The aim of this study was to develop a simple, accurate and precise RP-HPLC analytical method for the estimation of ticagrelor in tablet formulation
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