Studies on Methods of Particle Size Reduction of Medicinal Compounds. VI. Solvate Formation of Griseofulvin with Benzene and Dioxane

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Solvate formation of griseofulvin with benzene and dioxane was confirmed by differential scanning calorimetry (DSC), thermogravimetric analysis (TG), and X-ray diffractometry. Combining ratios of the two solvates were determined by TG to be 1 : 2 and 2 : 1 with respect to griseofulvin and benzene, and griseofulvin and dioxane, respectively. From data by solubility measurements and by various thermal methods of analysis such as DSC, freezing point determination by cooling curve method, the phase diagrams of the systems between benzene and griseofulvin, and between dioxane and griseofulvin were constructed. Also, thermodynamic properties of these solvates were investigated. It was found that the transition temperatures and the overall heats of desolvation were 35°and 6.3±0.2 kcal/mole of solvent for the benzene solvate, and 80-85°and 6.0±0.5 kcal/mole for the dioxane solvate, respectively. Moreover, the possibilities of these solvates for applying to particle size reduction of griseofulvin were examined. As for the benzene solvate, the free griseofulvin obtained by desolvation has a specific surface area of 7 m^2/g, and a mean particle size of 0.58μ. In the case of the dioxane solvate, the specific surface area after desolvation was reached to 4.8 m^2/g ; however, the desolvated particles retained their original shapes. Surface structures of the two kinds of desolvated products were examined by scanning electron microscopy. As the results, it became clear that the desolvated particles from the dioxane solvate has a stout and very porous structure, though those from the benzene solvate are the laminar aggregates composed of very easily separable primary particles.
公益社団法人日本薬学会の論文
1976-07-25

Studies on Methods of Particle Size Reduction of Medicinal Compounds. VI. Solvate Formation of Griseofulvin with Benzene and Dioxane

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