B-crystal form solid matter of bergenin and preparation method and application thereof
A technology of petracenin and solid substances, which is applied in the field of medicine and can solve the problems of undiscovered petracenin crystal form patents or literature reports, etc.
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[0066] Preparation example The preparation of petrogin crystal type C sample
[0067] Take 5g of petracenin sample, completely dissolve the petracenin sample with absolute ethanol at a normal temperature of 20°C, heat to a temperature of 40°C, and quickly evaporate the solvent under vacuum conditions to prepare the obtained petracenin 4.20g of plain crystal solid substance. HPLC purity 98.9%, recovery 84%.
[0068] The petracenin crystal C-type solid substance obtained by one embodiment of the present invention, the chemical purity and crystal form purity of its sample are both greater than 90%. When using powder X-ray diffraction analysis and using CuKα radiation experimental conditions, the diffraction peak position: 2-Theta value (°) or d value and diffraction peak relative intensity: peak height (Height%) or peak area (Area%) has the following characteristic peaks (see Figure 4 ).
[0069]For the petracenin crystal C-type solid material obtained in one embodiment of ...
Embodiment 1
[0074] Preparation method 1 of petracenin crystal type B sample
[0075] Take 5g of petracenin sample, completely dissolve the petracenin sample with tetrahydrofuran solvent at room temperature of 20°C, heat it to a temperature of 40°C, evaporate the solvent quickly under vacuum conditions, and prepare the obtained petracenin 4.40 g of crystalline solid substance. HPLC purity 98.7%, recovery 88%.
[0076] The chemical purity and crystalline purity of the sample of the B-type solid substance of petogenin obtained by one embodiment of the present invention are both greater than 90%. When powder X-ray diffraction is used to analyze and adopt CuKα radiation experimental conditions, the diffraction peak position is: 2-Theta value (°) or d value and diffraction peak relative intensity: peak height value (Height%) or peak area value (Area%) have following characteristic peak (see table 1 and figure 1 ).
[0077] For the petracenin crystal B-type solid material obtained in one em...
Embodiment 2 to 9
[0081] Preparation method 2 to 9 of petracenin crystal type B sample
[0082] Referring to the preparation method of Example 1, DMF, dioxane, n-butanol, isopropanol, dichloromethane, ethyl acetate, chloroform or pyridine were used as solvents to obtain petracenin solids. The experimental results are shown in Table 2 below. Powder X-ray diffraction, IR, melting point determination and DSC analysis were carried out on the obtained crystals, which showed that the crystal form obtained was the B-type petogenin crystal.
[0083] The preparation result of table 2 petogenin crystal type B sample 1
[0084] Example
[0085] 3
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