Method for extracting 6-gingerol with content greater than or equal to 98%

A technology of gingerol and content, applied in chemical instruments and methods, preparation of organic compounds, separation/purification of carbonyl compounds, etc., can solve the problem that the quality cannot reach high quality, the key production points are not well controlled, and the large-scale production products are not available. and other problems, to achieve the effect of shortening the purification cycle, no pesticide residues, and low production costs

Active Publication Date: 2021-06-08
GUILIN NATURAL INGREDIENTS CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, domestic large-scale production of 6-gingerol with a high content of ≥98% is rare, mainly due to the complexity of the process, the difficulty of operation, and the poor control of key production points, and the quality has not reached high quality.
It is reported that although there is a patent for gingerol production, there are almost no products that can be mass-produced

Method used

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  • Method for extracting 6-gingerol with content greater than or equal to 98%

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 1) Get 2kg of dried ginger (the content of 6-gingerol detected by HPLC is 0.4%), be pulverized to 100 orders, and the material is put into a flash extractor, and extracted with 75vt% ethanol (vt% is percent volume concentration) Solvent, adding 18 times the weight of ginger, extracting at room temperature for 3 minutes at a motor speed of 5000r / min, and extracting 3 times, each time for one minute. Rest for 2 minutes between extractions. The filtrate was separated, and the filtrates extracted 3 times were combined to obtain the total filtrate;

[0030] 2) Concentrate the total filtrate membrane to 2000ML, adjust the ethanol concentration of the concentrate to 50vt% with 96vt% ethanol, stir evenly, enter the alumina column chromatography, the alumina and ginger mass ratio contained in the chromatography column is 2 : 1, the alumina is neutral alumina, the number of meshes is 100 meshes, and the flow rate of the concentrated solution into the column is 1BV / h. After the c...

Embodiment 2

[0038] 1) Get 2kg of dried ginger (the content of 6-gingerol detected by HPLC is 0.4%), pulverize to 150 orders, put the material into a flash extractor, use 78vt% ethanol as the extraction solvent, add 19 times the solvent of ginger weight , under the condition of motor speed 5500r / min, extract at room temperature for 3 minutes, extract 3 times, each time for one minute. Rest for 2 minutes between extractions. The filtrate was separated, and the filtrates extracted 3 times were combined to obtain the total filtrate;

[0039]2) Concentrate the total filtrate through membrane to 2000ML, adjust the ethanol concentration of the concentrated solution to 55vt% with 98vt% ethanol, stir evenly, enter the alumina column chromatography, the mass ratio of alumina and ginger contained in the chromatography column is 2.5 : 1, the alumina is neutral alumina, the number of meshes is 150 meshes, and the flow rate of the concentrated solution into the column is 1.2BV / h. After the column is c...

Embodiment 3

[0047] 1) Get 2kg of dried ginger (the content of 6-gingerol detected by HPLC is 0.4%), be pulverized to 200 orders, and the material is put into a flash extractor, and 80vt% ethanol (vt% is volume percentage concentration) is used as extraction Solvent, add 20 times the weight of ginger, extract at normal temperature for 4 minutes under the condition of motor speed 6000r / min, extract 4 times, each time for one minute. Rest for 2 minutes between extractions. Separating the filtrate, merging the filtrates extracted for 3-4 times to obtain the total filtrate;

[0048] 2) Concentrate the total filtrate membrane to 2000ML, adjust the ethanol concentration of the concentrate to 60vt% with 97vt% ethanol, stir evenly, enter the alumina column chromatography, the mass ratio of alumina and ginger contained in the chromatography column is 3 : 1, the alumina is neutral alumina, the number of meshes is 200 meshes, the flow rate of the concentrated solution into the column is 1.5BV / h, aft...

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Abstract

The invention belongs to the field of 6-gingerol extraction, and particularly relates to a method for extracting 6-gingerol with the content larger than or equal to 98%. The method for extracting 6-gingerol with the content larger than or equal to 98% comprises the following steps: crushing fresh ginger, adding ethyl alcohol for flash extraction, and separating out a filtrate; concentrating the obtained filtrate, carrying out alumina column chromatography, and collecting an alumina column chromatography eluent; adsorbing the alumina column chromatography eluent through a macroporous resin column, eluting with alkali-containing ethanol, acid-containing ethanol and 50-60 vt% ethanol in sequence, collecting 50-60 vt% ethanol eluent, and concentrating to prepare a concentrated solution with the baume degree of 10-15; mixing the obtained concentrated solution with an organic solvent, adjusting the alcohol concentration to 55-60 vt%, adding activated carbon, and filtering with an organic membrane; and performing gradient elution separation on the obtained filtrate by using macroporous resin through 50-60 vt% ethanol and 65-70 vt% ethanol in sequence, respectively collecting each gradient eluent, concentrating and drying to obtain the required 6-gingerol. The original extraction method is replaced by flash extraction, so that the production efficiency is greatly improved, and various data of series macroporous resin purification are optimized to achieve the maximum efficiency.

Description

technical field [0001] The invention belongs to the field of 6-gingerol extraction, in particular to a method for extracting 6-gingerol with a content of ≥98%. Background technique [0002] Gingerol, a phenolic substance mainly present in the spice ginger (Latin name Zingiber officinale Roscoe), has a variety of different pharmacological effects, including antioxidant, anti-apoptotic, and anti-inflammatory effects. Gingerol is composed of a series of similar compounds, these compounds are 4-gingerol, 6-gingerol, 8-gingerol, 10-gingerol, 12-gingerol, among which 6-gingerol has the highest content. There is evidence that gingerol has anticancer and chemopreventive properties, and a possible mechanism of action has been proposed to inhibit cyclooxygenase-2 expression by blocking the p38 mitogen-activated protein kinase nuclear transcription factor signaling pathway. [0003] At present, there are very few manufacturers of large-scale production of 6-gingerol with a high conten...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/78C07C45/79C07C49/255
CPCC07C45/78C07C45/786C07C45/79C07C49/255
Inventor 赵军杨美英陆宝屹李杰
Owner GUILIN NATURAL INGREDIENTS CORP
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