Cycloastragenol-6-O-beta-D glucoside monohydrate and crystal thereof

A technology of cycloastragenol and glucoside, which is applied in the field of medicine and can solve the problems of easy moisture absorption, difficult storage, poor stability, etc.

Inactive Publication Date: 2011-04-27
天津天诚新药评价有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Therefore, the object of the present invention is to provide cycloastragenol-6-O-β-D glucoside in a stable form, to overcome the di

Method used

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  • Cycloastragenol-6-O-beta-D glucoside monohydrate and crystal thereof
  • Cycloastragenol-6-O-beta-D glucoside monohydrate and crystal thereof
  • Cycloastragenol-6-O-beta-D glucoside monohydrate and crystal thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] CMG 5g, heated and dissolved with 50ml 70% (volume) ethanol aqueous solution, filtered while hot, added ethyl acetate to the filtrate under stirring until the volume ratio of ethyl acetate to ethanol in the solution was 10:1, left at room temperature for 24 hours, and white needles were precipitated. crystallized, filtered. Vacuum dry at 105°C for 24 hours, and dry in an infrared dryer for 1 hour to obtain a CMG monohydrate type I single crystal, whose diffraction three-dimensional structure projection diagram is shown in figure 1 ,

[0040] The projection diagram of the molecules in the single crystal diffraction unit cell along the α-axis direction is shown in figure 2 . The single crystal is ground into powder, and the powder diffraction of CMG monohydrate type I crystal is carried out. The X-ray powder diffraction pattern represented by 2θ angle is shown in image 3 , Table 1 shows the X-ray single crystal diffraction atomic coordinate parameters and equivalent ...

Embodiment 2

[0057] CMG 5g, heated and dissolved with 100ml 80% (volume) ethanol aqueous solution, filtered while it was hot, added ethyl acetate to the filtrate under stirring until the volume ratio of ethyl acetate to ethanol in the solution was 8:1, left at room temperature for 36 hours, and precipitated white Needle crystal, filtered. Vacuum drying at 60°C for 12 hours gave type I CMG monohydrate crystals. Thermogravimetric analysis showed a weight loss of 3.1% at 70-120°C.

Embodiment 3

[0059] CMG 5g, heated and dissolved with 60ml 90% (volume) ethanol aqueous solution, filtered while hot, added ethyl acetate to the filtrate under stirring until the volume ratio of ethyl acetate to ethanol in the solution was 6:1, left at room temperature for 48 hours, and precipitated white Needle crystal, filtered. Dry at room temperature for 48 hours to obtain type I CMG monohydrate crystals. Thermogravimetric analysis showed a weight loss of 2.7% at 70-120°C.

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Abstract

The invention provides cycloastragenol-6-O-beta-D glucoside monohydrate and a crystal thereof and preparation methods of the cycloastragenol-6-O-beta-D glucoside monohydrate and the crystal thereof and a drug composition. Studies show that the prepared cycloastragenol-6-O-beta-D-glucoside hydrate containing crystal water is white crystalline powder, can exist stably and is convenient to store and transport and to prepare drug preparations. The cycloastragenol-6-O-beta-D-glucoside containing crystal water is easier to dissolve in water and alcohols solvents, has good room temperature storage stability and lower moisture absorption and is convenient for preparing the directly dissolved and absorbed preparations.

Description

technical field [0001] The invention belongs to the technical field of medicine, and relates to cycloastragenol-6-O-β-D glucoside monohydrate and crystals thereof, and the preparation of cycloastragenol-6-O-β-D glucoside monohydrate and crystals thereof Methods and pharmaceutical compositions. Background technique [0002] Cycloastragenol triterpene saponins are the main biologically active ingredients in the commonly used traditional Chinese medicine Astragalus membranaceus Beg. Kidney, pancreatic islet damage and many other pharmacological effects. Isao Kitagawa et al. reported for the first time in 1983 (Chem.Pharm.Bull.319 (2), 698-708, 1983) the structure of cycloastragenol 6-O-β-D-glucoside (abbreviated as CMG in English) (see the following structural formula ), which is a by-product obtained during the study of the structure of astragaloside IV. International invention patent application PCT / US2004 / 020277 and Chinese invention patent application CN1809364A disclose...

Claims

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Application Information

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IPC IPC(8): C07J53/00A61K31/7048A61P37/00A61P9/00A61P9/10A61P1/16A61P29/00A61P31/12A61P13/12
Inventor 韩英梅夏广萍刘鹏付晓丽赵娜夏
Owner 天津天诚新药评价有限公司
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