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New crystalline type 3,4',5-trihydroxy stilbene-3-beta-D-glucocide

A technology of glucoside and trihydroxystilbene is applied in the field of 3,4',5-trihydroxystilbene-3-β-D-glucoside of new crystal form, which can solve the problems of double melting point and long melting range, and achieve Good compressibility, reduced raw material cost and easy quality control

Active Publication Date: 2007-01-31
SHENZHEN NEPTUNUS PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, the measured melting range is generally longer, and even double melting point phenomenon occurs.

Method used

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  • New crystalline type 3,4',5-trihydroxy stilbene-3-beta-D-glucocide
  • New crystalline type 3,4',5-trihydroxy stilbene-3-beta-D-glucocide
  • New crystalline type 3,4',5-trihydroxy stilbene-3-beta-D-glucocide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] [Example 1] Preparation of type II crystal form 3,4',5-trihydroxystilbene-3-β-D-glucoside

[0034] 3,4',5-trihydroxystilbene-3-β-D-glucoside (polydatin) raw material compound can be prepared by the method described in Chinese patent application 03117246; solvent ethanol and acetone are respectively re-distilled to obtain refined ethanol and refined acetone . Add 300g of polydatin to about 1L of refined ethanol solvent, dissolve and filter, concentrate the filtrate under reduced pressure (0.1Mpa, 55°C) to about 0.5L, add about 1L of refined acetone while it is hot, and place the mixed solution in a refrigerator at 4°C to precipitate a solid The product was vacuum-dried (0.1Mpa, room temperature) after suction filtration to obtain about 226g of type II polydatin.

[0035] Its XRD spectrum is as figure 1 As shown, the DSC spectrum is as figure 2 shown.

Embodiment 2

[0036] [Example 2] Preparation of Type III crystal form 3,4',5-trihydroxystilbene-3-β-D-glucoside

[0037] 3,4', 5-trihydroxystilbene-3-β-D-glucoside (polydatin) raw material compound can be prepared by the method described in Chinese patent application 03117246; solvent acetone, ethyl acetate, n-hexane are refined respectively to obtain refined Acetone, ethyl acetate and refined n-ethane. Add 100g of polydatin into about 1.5L of refined acetone solvent, dissolve and filter, concentrate the filtrate under reduced pressure (0.1Mpa, 55°C) to about 0.8L, add about 0.3L of refined ethyl acetate while it is hot, mix well, add Refined about 1 L of n-hexane, and placed the mixed solution in a refrigerator at 4°C. The precipitated solid was suction filtered and then vacuum-dried (0.1 Mpa, room temperature) to obtain about 69 g of type III polydatin.

[0038] Its XRD spectrum is as image 3 As shown, the DSC spectrum is as Figure 4 shown.

[0039] 0.5g of 3,4',5-trihydroxystilbene...

Embodiment 3

[0040] [embodiment 3] the preparation of solid pharmaceutical preparation

[0041] Element

[0042] Preparation method: The above prescription ingredients are mixed according to conventional preparation methods, and directly compressed into tablets.

[0043] Element

[0044] Preparation method: Type II crystal polydatin (Example 1) is mixed evenly with starch, lactose, and dextrin according to the method of equal multiplication, and the pre-prepared HPMC solution is added to make a soft material, granulated with a 20-mesh sieve, and dried at 60°C for about After 30 minutes, sieve with 18 meshes, add micropowder silica gel, mix evenly, and fill with 2# capsules.

[0045] Element

[0046] Preparation method: The above prescription ingredients are mixed, granulated and compressed into tablets according to conventional preparation methods.

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Abstract

The present invention relates to two kinds of new crystal types of 3,4,5-resveratrol-3-beta-D-glucoside and their preparation method and medicine composition containing them.

Description

technical field [0001] The present invention relates to 3,4',5-trihydroxystilbene-3-β-D-glucoside (3,4',5-trihydroxy-stilbene-3-β-D-glucoside; polydatin) with a defined crystal form, As well as the preparation method of the crystal form and its application in pharmaceutical preparations. Background technique [0002] literature Melting point (°C) crystallization solvent 1. Chinese patent (application number) 03117246 2. Fulvia Orsini. Isolation, Synthesis, and Antiplatelet Aggregation Activity of Resveratrol 3-O-β-D- Glucopyranoside and Related Compounds.J.Nat.Prod. 1997, 60, 1082~1087. (The reference cited in this article is Hillis WE, Ishikura K, J Chromatogr, 32, 323 (1968) has a melting point of 228-230 °C) 3. Gamini S. Jayatilake. Kinase Inhibitors From Polygonum Cuspidtum. Journal of Nature Products. 1993, 56(10), 1805-110. (References cited in this article M.Antoni, D.M.X. Donnelly, Phyto...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/20A61K31/7032A61K9/20A61K9/48A61K9/16A61K9/02A61K9/06A61K47/38A61P9/10A61P3/06C07H1/08
CPCC07H15/20C07H1/06A61P9/00A61P9/10
Inventor 赵金华康晖曾伟珍李靖于琳
Owner SHENZHEN NEPTUNUS PHARM CO LTD
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