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.

Active Publication Date: 2010-12-01
INST OF MATERIA MEDICA AN INST OF THE CHINESE ACAD OF MEDICAL SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0016] After domestic and foreign patent and literature searches, no other

Method used

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  • B-crystal form solid matter of bergenin and preparation method and application thereof
  • B-crystal form solid matter of bergenin and preparation method and application thereof
  • B-crystal form solid matter of bergenin and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

preparation example

[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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Abstract

The invention discloses a B-crystal form of a compound of bergenin shown in a formula (I), a preparation method of a new crystal-form solid matter sample of the bergenin and a pharmaceutical composition containing a new crystal form of the bergenin, and discovers absorption and plasma drug concentration features of a new crystal-form solid matter of the bergenin in an organism after oral solid administration. The new crystal-form solid matter changes the absorption rate of active constituents of the original crystal-form solid drug in the organism, enhances the plasma drug concentration in the organism and strengthens the advantages of the drug in clinical disease treatment.

Description

technical field [0001] The crystal type B of the petracenin compound involved in the present invention belongs to the technical field of medicine. Background technique [0002] Petgenin, named in English as Bergeninum, has the following structural formula: [0003] [0004] In the Chinese patent CN1615846 (publication number), it is recorded that "soft capsule containing petogenin and its preparation method" invented by Li Jie [1] , which involves the preparation method of petracenin soft capsules. [0005] In the Chinese patent CN1615858 (publication number), it is recorded that "compound rock cabbage dropping pills and its preparation method" invented by Guiyang Gaoxin Ruide Technology Development Co., Ltd. [2] , which involves the preparation of compound dropping pills composed of petogenin and other ingredients. [0006] In the Chinese patent CN1634049 (publication number), it is recorded that "Pectin buccal tablet and its preparation process" invented by Yunnan In...

Claims

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Application Information

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IPC IPC(8): C07D493/04A61K31/366A61P13/08A61P35/00A61P11/14A61P11/10A61P11/06
Inventor 吕扬杜冠华杨德智田硕吕丽娟孟凡瑞
Owner INST OF MATERIA MEDICA AN INST OF THE CHINESE ACAD OF MEDICAL SCI
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