Five different crystalline form substances of dihydromyricelin
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A technology of dihydromyricetin and d-dihydromyricetin, which is applied in the field of medicine and can solve problems such as inability to reveal the crystal structure
Inactive Publication Date: 2015-04-08
TONGJI HOSPITAL ATTACHED TO TONGJI MEDICAL COLLEGE HUAZHONG SCI TECH
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However, due to the presence of more hydrogen bonds in the dihydromyricetin molecule, which can form intramolecular and intermolecular hydrogen bonds, and may also contain crystal water, only from the compound at 3300cm -1 There is a broad peak at , which cannot indicate its crystal structure
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Embodiment 1
[0076] The preparation of embodiment 1 D-dihydromyricetin dihydrate
[0077] Take about 200mg of D-dihydromyricetin raw material, which can be anhydrous or monohydrate, dissolve it in 2ml of 90-100°C aqueous solution, filter with heat preservation, remove the filter residue, and cool the solution naturally to room temperature to precipitate crystals. Get D-dihydromyricetin dihydrate.
Embodiment 2
[0078] The preparation of embodiment 2 D-dihydromyricetin anhydrate
[0079] Take about 200 mg of D-dihydromyricetin raw material, which can be dihydrate or monohydrate, and place it at a temperature of 160 ° C for 1 hour to obtain dihydromyricetin anhydrate.
Embodiment 3
[0080] The preparation of embodiment 3 D-dihydromyricetin monohydrate
[0081] Take about 200 mg of D-dihydromyricetin raw material, which can be dihydrate or anhydrous, dissolve in high-concentration ethanol solution, volatilize slowly until crystallization, and obtain D-dihydromyricetin monohydrate.
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Abstract
The invention discloses five crystalline form substances of dihydromyricelin (of which the chemical name is 3,5,7,3',4',5'-hexahydroxy-2,3-dihydroflavonol and the English name is dihydromyricelin or ampelopsin). The spatial configuration of dihydromyricelin is characterized by virtue of colorimetry-polarimetry and high-performance liquid-phase chiral separation methods. By virtue of solid-state analytical technologies including a powder X-ray diffraction (XRD), differential scanning calorimetry (DSC), thermal gravimetric analysis (TGA), a Karl Fischer titration and Fourier transform-attenuated total reflectance (FT-ATR) infrared spectroscopy, the crystalline forms of dihydromyricelin are characterized. The polymorph screening of dihydromyricelin is of important significance for the development of processes of active pharmaceutical ingredients, the development of dosage forms such as solid preparation, semi-solid preparation and suspension and quality control.
Description
technical field [0001] The present invention relates to the technical field of medicine, and specifically refers to a substance of five different crystal forms of dihydromyricetin Background technique [0002] Dihydromyricelin, also known as Ampelopsin, was first isolated by Kotake and Kubota in 1940 from the leaves of Ampelopsis meliaefolia, a dihydroflavone Alcohol flavonoid compound, the chemical structure is 3,5,7,3',4',5'-hexahydroxy-2,3-dihydroflavonol. Dihydromyricetin is widely found in the genus Vitaceae of the Vitaceae family, and also in the plants of Myriceaceae, Rhododendronaceae, Garciniaceae, Euphorbiaceae, Olives, Fabaceae, Sapotaceae and Salicaceae. [0003] Dihydromyricetin is white or light yellow needle-like crystal, poorly water-soluble (0.2mg / ml, 25℃), easily soluble in hot water, ethanol, methanol, acetone and DMSO. The chemical stability of the aqueous solution is poor in the heated state, but it has good chemical stability in the solid state. [0...
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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/32
CPCC07D311/32
Inventor 方建国王文清施春阳熊微陈婧刘旭王晨光侯小龙
Owner TONGJI HOSPITAL ATTACHED TO TONGJI MEDICAL COLLEGE HUAZHONG SCI TECH
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