Ginsenoside C-K monohydrate crystal and preparation method thereof

A technology of ginsenoside and monohydrate, which is applied in the field of ginsenoside C-K monohydrate crystal and preparation to achieve the effects of improving crystallization yield, avoiding explosive nucleation and uniform particle size distribution

Active Publication Date: 2013-05-08
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] At present, there is no literature report about the monohydrate of ginsenoside C-K. We have obtained the single crystal structure of ginsenoside C-K monohydrate, and also prepared the monohydrate of ginsenoside C-K in the solution at the same time. Its X-ray The powder diffraction characteristic peaks are obviously different from other solvent compounds, no coalescence occurs, and the preparation method is relatively simple

Method used

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

Examples

Experimental program
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Effect test

Embodiment 1

[0027] The method that this example produces ginsenoside C-K monohydrate crystal specifically comprises the following steps:

[0028] 1) Add 18.0126g of crude ginsenoside C-K into 260ml of acetonitrile and water mixed solvent with a mass ratio of 1.5:1, dissolve it completely at 60°C, then raise the temperature to 63°C to ensure that ginsenoside C-K is completely dissolved, and add Condensation reflux device to avoid solvent volatilization;

[0029] 2) Cool down the saturated solution obtained above at a rate of 0.15°C / min, add 1% seed crystals when the temperature drops to 43°C, and maintain the temperature of seed crystals for 30 minutes to consume the supersaturation in the solution;

[0030] 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 monohydrate, the yield is m...

Embodiment 2

[0034] The method that this example produces ginsenoside C-K monohydrate crystal specifically comprises the following steps:

[0035] 1) Add 8.1265g of crude ginsenoside C-K into 300ml of acetonitrile and water mixed solvent with a mass ratio of 1:1, dissolve it completely at 60°C, and then raise the temperature to 63°C to ensure that ginsenoside C-K is completely dissolved, and add Condensation reflux device to avoid solvent volatilization;

[0036] 2) Cool down the saturated solution obtained above at a rate of 0.1°C / min, add 0.5% seed crystals when the temperature drops to 45°C, and maintain the seeding temperature for 60 minutes to consume the supersaturation in the solution;

[0037] 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 monohydrate, the yield is more tha...

Embodiment 3

[0041] The method that this example produces ginsenoside C-K monohydrate crystal specifically comprises the following steps:

[0042] 1) Add 9.6338g of crude ginsenoside C-K into 310ml of acetonitrile and water mixed solvent with a mass ratio of 2:1, dissolve it completely at 60°C, then raise the temperature to 63°C to ensure that ginsenoside C-K is completely dissolved, and add Condensation reflux device to avoid solvent volatilization;

[0043] 2) Cool down the saturated solution obtained above at 0.2°C / min, add 3% seed crystals when the temperature drops to 40°C, and maintain the seeding temperature for 60 minutes to consume the supersaturation in the solution;

[0044] 3) After constant temperature stirring, continue to drop the temperature to 4°C at a cooling rate of 0.4°C / min, grow crystals at 4°C for 1 hour, filter and wash, and dry at 55°C for 1 hour under a vacuum of 0.08Mp-0.1Mp to obtain the product Ginsenoside C-K monohydrate, the yield is more than 90%.

[0045]...

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Abstract

The invention relates to a ginsenoside C-K monohydrate crystal and a preparation method thereof. One molecule of ginsenoside C-K monohydrate contains one molecule of ginsenoside C-K and molecule of water. The preparation method comprises the following steps of: adding ginsenoside C-K raw material in a mixed solvent of acetonitrile and water, adding seed crystal in a supersaturated solution of ginsenoside C-K in a cooling process, inducing the seed crystal to separate out crystals, and promoting the growth of the crystals. The 2 theta value of the obtained crystal product of ginsenoside C-K monohydrate crystal is 6.3+ / -0.2, 11.2+ / -0.2, 12.7+ / -0.2, 13.3+ / -0.2, 15.8+ / -0.2, 16.2+ / -0.2, 17.4+ / -0.2, 20.0+ / -0.2, 20.8+ / -0.2, 22.6+ / -0.2, 23.6+ / -0.2, 24.3+ / -0.2 and 25.6+ / -0.2. By the preparation method, the crystallization yield of C-K is improved and the stability of the product is improved.

Description

technical field [0001] The invention relates to a ginsenoside C-K monohydrate crystal and a preparation method thereof, in particular to a single crystal structure of the ginsenoside C-K monohydrate. The preparation method is specifically a method for producing ginsenoside C-K monohydrate by cooling crystallization. The ginsenoside C-K monohydrate obtained by the method is a flaky crystal with uniform particle size distribution, no agglomeration, and high yield. 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 ol...

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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