Ginsenoside C-K semihydrate crystal and preparation method thereof

A technology of ginsenoside and hemihydrate, applied in the direction of steroids, organic chemistry, etc., to achieve the effect of controlling crystal nucleation, uniform particle size distribution, and improving crystallization yield

Active Publication Date: 2013-05-01
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Now there is no report about the crystallization of ginsenoside C-K hydrate in solution, we have obtained a hemihydrate of ginsenoside C-K in solution, and its X-ray powder diffraction characteristic peak is obviously different from other solvents compound, will not coalesce, and the preparation method is relatively simple

Method used

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  • Ginsenoside C-K semihydrate crystal and preparation method thereof
  • Ginsenoside C-K semihydrate crystal and preparation method thereof
  • Ginsenoside C-K semihydrate crystal and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0029] The method that this example produces ginsenoside C-K hemihydrate crystal specifically comprises the following steps:

[0030] 1) Add 22.3950g of crude ginsenoside C-K to 290ml of acetone and water mixed solvent with a mass ratio of 4:1, dissolve it completely at 50°C, then raise the temperature to 53°C to ensure that ginsenoside C-K is completely dissolved, and add Condensation reflux device to avoid solvent volatilization;

[0031] 2) Cool down the saturated solution obtained above at a rate of 0.1°C / min, add 1% seed crystals when the temperature drops to 40°C, and maintain the seeding temperature for 60 minutes to consume the supersaturation in the solution;

[0032] 3) After constant temperature stirring, continue to drop the temperature to 4°C at a cooling rate of 0.2°C / min, grow crystals at 4°C for 1 hour, filter and wash, and dry at 50°C for 1 hour under a vacuum of 0.08Mp-0.1Mp to obtain the product Ginsenoside C-K hemihydrate, the yield is more than 92%.

[0...

Embodiment 2

[0037] The method that this example produces ginsenoside C-K hemihydrate crystal specifically comprises the following steps:

[0038] 1) Add 15.0205g of crude ginsenoside C-K to 320ml of acetone and water mixed solvent with a mass ratio of 10:1, dissolve it completely at 50°C, then raise the temperature to 53°C to ensure that ginsenoside C-K is completely dissolved, and add Condensation reflux device to avoid solvent volatilization;

[0039] 2) Cool down the saturated solution obtained above at a rate of 0.05°C / min, add 0.5% seed crystals when the temperature drops to 42°C, and maintain the seeding temperature for 60 minutes to consume the supersaturation in the solution;

[0040] 3) After constant temperature stirring, continue to drop the temperature to 4°C at a cooling rate of 0.1°C / min, grow crystals at 4°C for 1 hour, filter and wash, and dry at 45°C for 1 hour under a vacuum of 0.08Mp-0.1Mp to obtain the product Ginsenoside C-K hemihydrate, the yield is greater than 91%...

Embodiment 3

[0045] The method that this example produces ginsenoside C-K hemihydrate crystal specifically comprises the following steps:

[0046] 1) Add 18.1238g of crude ginsenoside C-K to 300ml of acetone and water mixed solvent with a mass ratio of 8:1, dissolve it completely at 50°C, then raise the temperature to 53°C to ensure that ginsenoside C-K is completely dissolved, and add Condensation reflux device to avoid solvent volatilization;

[0047] 2) Cool down the saturated solution obtained above at a rate of 0.2°C / min, add 3% seed crystals when the temperature drops to 38°C, and maintain the seeding temperature for 60 minutes to consume the supersaturation in the solution;

[0048] 3) After constant temperature stirring, continue to drop the temperature to 4°C at a cooling rate of 0.3°C / min, grow crystals at 4°C for 1 hour, filter and wash, and dry at 60°C for 1 hour under a vacuum of 0.08Mp-0.1Mp to obtain the product Ginsenoside C-K hemihydrate, the yield is more than 90%.

[0...

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Abstract

The invention relates to a ginsenoside C-K semihydrate crystal and a preparation method thereof. The raw material of ginsenoside C-K is added into a mixed solvent of acetone and water, a cooling crystallization method is adopted, seed crystals are added into the supersaturated solution of the ginsenoside C-K during cooling and induced to form crystals, the core formation of the crystals is controlled, and the growth of the crystals is promoted. The 2 theta values corresponding to the powder diffraction characteristic peaks of the obtained ginsenoside C-K semihydrate crystal are 5.4+/-0.2, 6.6+/-0.2, 11.0+/-0.2, 12.6+/-0.2, 13.2+/-0.2, 14.5+/-0.2, 15.5+/-0.2, 15.9+/-0.2, 17.1+/-0.2 and 20.6+/-0.2. According to the invention, the ginsenoside C-K semihydrate crystal is prepared via the cooling crystallization method, and the crystallization yield of C-K is improved; and the core formation generated during crystallization is avoided, and a product with uniformly distributed granularity and stability is obtained.

Description

technical field [0001] The invention relates to a ginsenoside C-K hemihydrate crystal and a preparation method thereof, in particular to a method for producing ginsenoside C-K hemihydrate by cooling crystallization. The ginsenoside C-K hemihydrate obtained by the method is a long columnar crystal, the particle size distribution is uniform, no coalescence occurs, and the yield is high. Background technique [0002] Ginseng is a traditional Chinese medicine that is widely used for health care and treatment. It has a certain therapeutic effect on the enemy of human health, cancer, which is related to its effects on secretion, immunity and metabolism. Ginsenoside is one of the main active ingredients of ginseng, which has the functions of inhibiting the proliferation of tumor cells and anti-metastasis. Also have anti-aging effect, it is divided into protopanaxadiols, protopanaxatriol saponins and oleanolic acid saponins (Yang Na etc., the antitumor of ginseng and the inhibitory...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J17/00
Inventor 龚俊波李润妍代常亮董伟兵王静康尹秋响张美景王永莉侯宝红郝红勋鲍颖陈巍
Owner TIANJIN UNIV
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