Characterization of Edoxaban Tosylate drug substance by different Instrumental Analysis

Abstract

Differential scanning calorimetry (DSC) is one of the thermal analysis techniques. In the case of DSC, differences in heat flow between a specimen and reference are measured against the temperature or time while the specimen is continuously heated under controlled conditions. The function of the calorimeter is to measure the heat content which comes in and out of the sample. TGA (Thermo Gravimetric Analysis) is an important characterization technique which measures the change in mass of a material with variations in temperature. It operates in two modes: 1) change in mass is measured with increasing temperature (called scanning mode having constant heating rate); and 2) change in mass is measured with time (called the isothermal mode with constant temperature or constant mass loss). This change of mass is due to both physical and chemical phenomena like absorption, sublimation, vaporization, oxidation, reduction and decomposition likewise. The impurities ranging in Edoxaban tosylate were detected by a simple gradient reverse-phase high-performance liquid chromatography (HPLC). LC–MS was performed to identify the mass of the impurities. These Impurities in the Edoxaban tosylate crude sample have been isolated by using a column. The Characters were elucidated by various techniques 2D NMR (1H, 2D NMR, COSY and NOESY) and reported in this paper.