Use of surface free energy for differential evaluation of crystal, crystal evaluated on basis of surface free energy as index, and pharmaceutical composition prepared by containing the crystal
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example 1
[0072]Luliconazole was recrystallized under various conditions to obtain crystals in different states. The powder X-ray diffraction measurement was performed for these crystals (machine type of apparatus: XRD-DSCII, manufacturer: Rigaku Corporation, Condition: X-ray source: CuKα, measurement temperature: room temperature, tube voltage: 40 kV, tube current: 40 mA, 2θ: 5 to 35°, step angle: 0.05°). As a result, the positions of the diffraction angle 2θ of the diffraction peaks were identical in relation to all of them (see FIG. 1). Further, the peak was also single in DSC (machine type of apparatus: DSC7, manufacturer: PerkinElmer), and the melting point was observed in the vicinity of 149° C. (see FIG. 2, crystal recrystallized with water-containing ethanol (25%), crystal recrystallized with water-containing ethanol (50%), crystal recrystallized with water-containing ethanol (75%), and crystal recrystallized with ethyl acetate / n-hexane are shown from the top). According to these resu...
production example 1
[0079]Luliconazole was dissolved in ethanol while being heated, to which water in an amount of ⅓ of that of ethanol was gradually added, followed by being gently cooled to obtain Crystal 1 (ethanol / water (75:25) not pulverized).
production example 2
[0080]Crystal 1 was ground or pulverized with an agate mortar for 3 minutes to obtain Crystal 2 (ethanol / water (75:25) pulverized for 3 minutes).
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