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A kind of dissolving solution, recrystallization method and refining purification method of 6-gingerol

A technology of recrystallization and dissolving solution, applied in the separation/purification of carbonyl compounds, organic chemistry and other directions, can solve the problems of unstable chemical properties of 6-gingerol, waste of solvent and time, and low yield of 6-gingerol , to prevent waste, increase purity, and facilitate manipulation.

Active Publication Date: 2020-12-25
INST OF GEOCHEM CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the existing refining and purification methods are very difficult for the preparation of high-purity (6-gingerol content greater than or equal to 98%) 6-gingerol samples. At the same time, column chromatography and chromatographic separation are limited by the amount of each preparation Small and will consume a lot of solvent and time
And because the chemical properties of 6-gingerol are unstable, it is easy to decompose when exposed to light and heat, and its content in ginger is low, so the yield of 6-gingerol in the existing method is also low

Method used

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  • A kind of dissolving solution, recrystallization method and refining purification method of 6-gingerol
  • A kind of dissolving solution, recrystallization method and refining purification method of 6-gingerol
  • A kind of dissolving solution, recrystallization method and refining purification method of 6-gingerol

Examples

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Embodiment 1

[0071] A dissolving solution of 6-gingerol, which is a mixed solution of n-hexane, petroleum ether and ethyl acetate; the density of the dissolving solution is 0.706±0.03g / ml.

Embodiment 2

[0073] A dissolving solution of 6-gingerol, which is a mixed solution of n-hexane and ethyl acetate; the density of the dissolving solution is 0.707±0.03g / ml.

Embodiment 3

[0075] A kind of recrystallization method of 6-gingerol, it comprises:

[0076] After separation by column chromatography, the crude product 6-gingerol was obtained, which was ultrasonically dissolved in the first dissolving solution at 33°C, and the obtained ultrasonic dissolving solution was filtered while hot to remove the yellow insoluble matter at the bottom.

[0077] Cool down to -32°C and let stand for 2 hours, remove the supernatant, separate and recrystallize,

[0078] Wherein, the addition ratio of the first solution and the 6-gingerol crude product is: v / m=30, the first solution is a mixed solution of petroleum ether, n-hexane and ethyl acetate, and the density of the first solution is 0.705 ±0.03g / ml.

[0079] in, figure 1 The HPLC chromatogram of the product obtained after separation by column chromatography used in this example, that is, the crude product of 6-gingerol, the abscissa is time, and the ordinate is the absorbance value. according to figure 1 , it...

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Abstract

The invention discloses a dissolving solution, a recrystallization method and a refined purification method of 6-gingerol, and relaters to the field of pharmaceutical processing. The refined purification method comprises the steps of dissolving a crude 6-glycolol (the mass fraction of 6-gingol is 75% to 90%) mainly comprising 6-gingerol, 8-gingerol and 10-gingerol in the dissolving solution, recrystallizing with the recrystallization method, and refining to obtain the 6-gingerol, wherein the yield of 6-gingerol is up to 84% or more than 84% in the recrystallization process, the mass fraction of 6-gingerol in 6-gingerol crystals obtained by recrystallization is increased to 92%-95%, the content of 6-gingerol can reach up to 98% or be more than 98% after purification, at the same time, the yield of 6-gingerol can reach up to 68% or be more than 68%, the purity and the yield of 6-gingerol are effectively improved, and the methods are easy to manipulate.

Description

technical field [0001] The invention relates to the field of pharmaceutical processing, and in particular to a solution of 6-gingerol, a recrystallization method and a refining and purification method. Background technique [0002] 6-gingerol is the main component of gingerol in ginger, which has a variety of biological activities, such as anti-oxidation, anti-mutagenesis, anti-inflammation, anti-rheumatism, anti-tumor, cold-dispelling, liver-protecting and gallbladder-protecting effects. 6-gingerol can also be used in the production of medicines and health food for the treatment of cardiovascular and cerebrovascular diseases, rheumatoid arthritis, gastric ulcer and other diseases. [0003] At present, the initial extraction of 6-gingerol has solvent extraction, supercritical CO 2 Extraction, etc., further refining and purification can be carried out by column chromatography, high-speed countercurrent chromatography purification and the like. However, the existing refining...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/81C07C49/255
CPCC07C45/81C07C49/255
Inventor 余德顺陈可可马龙利叶菲菲李岗范文垒雷登凤
Owner INST OF GEOCHEM CHINESE ACADEMY OF SCI