COMPLEX-FORMATION BETWEEN DEOXYCHOLIC-ACID AND MENADIONE BY GRINDING AND SEALED HEATING METHODS

Complex formation between deoxycholic acid (DCA) and menadione (MND) b y grinding and sealed heating was investigated. The complex between DC A and MND was prepared by coprecipitation and showed a stoichiometry o f 2:1 (DCA:MND), The IR spectrum of the complex suggested that MND mol ecules were located in the channel formed by DCA molecules. The 10 min ground mixture of DCA-MND gave the same X-ray diffraction pattern as the DCA-MND coprecipitate, Differential scanning calorimetry (DSC) and IR spectroscopy also demonstrated the identical results between the g round mixture and the complex, confirming the complex formation betwee n DCA and MND by grinding, The DSC data suggested that the complex for mation was expected during heating process of the DCA-MND physical mix ture, The sealed heated samples were prepared and compared with the co mplex prepared by coprecipitation, After heating in a sealed ampoule a t 110 degrees C for 10 min or at 80 degrees C for 24 h, samples demons trated the same X-ray diffraction patterns, DSC curves and IR spectra as the complex, These results indicated that the complex formation too k place between DCA and MND by sealed heating as well as by grinding.