CN1616461A - Method for producing glabridin product - Google Patents
Method for producing glabridin product Download PDFInfo
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- CN1616461A CN1616461A CN 200410079233 CN200410079233A CN1616461A CN 1616461 A CN1616461 A CN 1616461A CN 200410079233 CN200410079233 CN 200410079233 CN 200410079233 A CN200410079233 A CN 200410079233A CN 1616461 A CN1616461 A CN 1616461A
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Abstract
The present invention relates to the production process of extracting active component glabridin from common licorice as a kind of medicinal plant. The production process includes the following steps: drying and crushing common licorice, organic solvent reflux extraction or diacolation extraction, concentrating the extract liquid and decompresson drying to obtain coarse product; dissolving the coarse product in chloroform, gradient elution with mixed chloroform-acetone solvent in silica gel column, silica gel thin layer chromatography until dilute sulfuric acid development, collecting target solution, decompression concentration, vacuum drying, dissolving in ethanol, filtering, decompression concentrating the filtrate and vacuum drying to obtain the product. The product is yellow brown powder and has active component content up to 44.64 %.
Description
Technical field
The present invention relates to the biological extraction technology, particularly relate to a kind of its activeconstituents---production method of glabridin product of from natural biology, extracting.
Background technology
Glabridin (Glabridin) is a kind of natural antioxidants, it is the flavanone compound of separation and Extraction from medicinal plant glycyrrhiza glabra (Glycyrrhiza Glabra), has very strong anti-oxidant and estrogen activity, can the human activin sod gene, as cosmetic applications, can anti aging effect, " factor of whitening " is otherwise known as.Glabridin (Glabridin) safety non-toxic is even life-time service is also harmless, at industrial cosmetics additive and the medical material of being used as usually.
Glabridin
(Glabridin)
At present, yet there are no both at home and abroad report on the open source literature about glabridin production technology aspect.
Summary of the invention
Purpose of the present invention just provides the production method of glabridin product.
Purpose of the present invention realizes by following scheme:
A kind of production method of glabridin product, its processing step is: at first with the glycyrrhiza glabra drying and crushing, extract with organic solvent refluxing extraction or diacolation then, the gained extracting solution is through concentrating, and drying under reduced pressure gets crude product; With above-mentioned gained crude product with the dissolving of an amount of chloroform after, last silicagel column, with chloroform, acetone mixed solvent gradient elution, check effluent liquid with the silica gel thin-layer chromatography detection method, collect target solution, through concentrating under reduced pressure, after the vacuum-drying, use the dissolve with ethanol after-filtration, filtrate is again through concentrating under reduced pressure, vacuum-drying;
The consumption of above-mentioned organic solvent is 5-10 a times of glycyrrhiza glabra;
Described organic solvent is ethyl acetate or methylene dichloride;
Described reflux extracting time is 5-8 hour;
Described diacolation is extracted into effluent liquid to be ended when colourless.
The inventive method technology is simple, and products obtained therefrom is the yellowish brown powder, and wherein activeconstituents (glabridin) content is greater than 40%, and all the other indexs all meet international standard.
Specific embodiment
Embodiment 1
With the glycyrrhiza glabra drying and crushing, according to 1: 10 ratio glycyrrhiza glabra pulverizing material and ethyl acetate are put in the reflux device then earlier, reflux is 8 hours together, filters, washs.Repeat twice, merging filtrate and washing lotion concentrate, and reclaim solvent, and drying under reduced pressure gets residue, is crude product.
Above-mentioned crude product is ground, be dissolved in minimum of chloroform, again solution is carefully added to (silica gel is that Haiyang Chemical Plant, Qingdao produces) on the silicagel column that anticipate, filling gel.With chloroform, acetone gradient elution.Check effluent liquid (dilute sulphuric acid colour developing) with the silica gel thin-layer chromatography detection method.Collect the target feed liquid, concentrating under reduced pressure, vacuum-drying.Add small amount of ethanol, dissolution residual substance filters, and filtrate is again through concentrating under reduced pressure, and vacuum-drying gets product.After testing, glabridin in the product (Glabridin) content is greater than 40%, and identification reaction is positive, and all the other indexs meet international standard.
Embodiment 2
With the glycyrrhiza glabra drying and crushing, according to 1: 5 ratio glycyrrhiza glabra pulverizing material and methylene dichloride are put in the percolator together then earlier, diacolation when waiting to flow out colourless liquid (about 10 hours), reclaims solvent, and residue gets crude product again through vacuum-drying.
Above-mentioned crude product is dissolved in minimum of chloroform, again solution is carefully added to (silica gel is that Haiyang Chemical Plant, Qingdao produces) on the silicagel column that anticipate, filling gel.With chloroform, acetone gradient elution.Check effluent liquid (dilute sulphuric acid colour developing) with the silica gel thin-layer chromatography detection method.Collect the target feed liquid, concentrating under reduced pressure, vacuum-drying.Add small amount of ethanol, dissolution residual substance filters, and filtrate is again through concentrating under reduced pressure, and vacuum-drying gets product.After testing, glabridin in the product (Glabridin) content 44.64%, identification reaction is positive, and all the other indexs meet international standard.
Embodiment 3
With the glycyrrhiza glabra drying and crushing, according to 1: 7 ratio glycyrrhiza glabra pulverizing material and methylene dichloride are put in the reflux device then earlier, reflux is 6 hours together, filters, washs.Repeat twice, merging filtrate and washing lotion concentrate, and reclaim solvent, and drying under reduced pressure gets residue, is crude product I.
Or glycyrrhiza glabra is pulverized material and ethyl acetate is put in the percolator together according to 1: 7 ratio, and diacolation when waiting to flow out colourless liquid (about 10 hours), reclaims solvent, and residue must crude product II again through vacuum-drying.
Above-mentioned gained crude product I and crude product II are ground, be dissolved in minimum of chloroform, again solution is carefully added to (silica gel is that Haiyang Chemical Plant, Qingdao produces) on the silicagel column that anticipate, filling gel.With chloroform, acetone gradient elution.Check effluent liquid (dilute sulphuric acid colour developing) with the silica gel thin-layer chromatography detection method.Collect the target feed liquid, concentrating under reduced pressure, vacuum-drying.Add small amount of ethanol, dissolution residual substance filters, and filtrate is again through concentrating under reduced pressure, and vacuum-drying gets product.After testing, glabridin in the product (Glabridin) content 44.64%, identification reaction is positive, and all the other indexs meet international standard.
Claims (5)
1. the production method of a glabridin product, its processing step is: at first with the glycyrrhiza glabra drying and crushing, extract with organic solvent refluxing extraction or diacolation then, the gained extracting solution is through concentrating, and drying under reduced pressure gets crude product; With above-mentioned gained crude product with the dissolving of an amount of chloroform after, last silicagel column, with chloroform, acetone mixed solvent gradient elution, check effluent liquid with the silica gel thin-layer chromatography detection method, collect target solution, through concentrating under reduced pressure, after the vacuum-drying, use the dissolve with ethanol after-filtration, filtrate is again through concentrating under reduced pressure, vacuum-drying.
2, the production method of glabridin product as claimed in claim 1, the consumption that it is characterized in that above-mentioned organic solvent are 5-10 times of glycyrrhiza glabra.
3, the production method of glabridin product as claimed in claim 1 or 2 is characterized in that described organic solvent is ethyl acetate or methylene dichloride.
4, the production method of glabridin product as claimed in claim 1 is characterized in that described reflux extracting time is 5-8 hour.
5, the production method of glabridin product as claimed in claim 1 is characterized in that described diacolation is extracted into effluent liquid and ends when colourless.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410079233 CN1273471C (en) | 2004-09-15 | 2004-09-15 | Method for producing glabridin product |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410079233 CN1273471C (en) | 2004-09-15 | 2004-09-15 | Method for producing glabridin product |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1616461A true CN1616461A (en) | 2005-05-18 |
| CN1273471C CN1273471C (en) | 2006-09-06 |
Family
ID=34765530
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200410079233 Expired - Fee Related CN1273471C (en) | 2004-09-15 | 2004-09-15 | Method for producing glabridin product |
Country Status (1)
| Country | Link |
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| CN (1) | CN1273471C (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101735233B (en) * | 2009-12-11 | 2011-11-16 | 暨南大学 | Method for producing high-purity glabridin |
| CN101830906B (en) * | 2009-12-13 | 2012-06-27 | 成都普思生物科技有限公司 | Separation and purification method of high-purity glabridin |
| CN101519408B (en) * | 2008-02-27 | 2012-08-29 | 新疆富沃药业有限公司 | Method for producing glabridin from glycyrrhiza residue |
| CN103848841A (en) * | 2012-11-29 | 2014-06-11 | 陕西华泰生物精细化工有限公司 | Method of extracting high-purity glabridin from licorice waste residue by adoption of new technology |
| CN104072512A (en) * | 2014-07-21 | 2014-10-01 | 江苏天晟药业有限公司 | Method for preparing glabridin |
| CN104277048A (en) * | 2013-07-10 | 2015-01-14 | 岳普湖天瑞生物工程有限公司 | Preparation method for glycyrrhiza glabra total flavonoids |
| CN104800206A (en) * | 2015-04-15 | 2015-07-29 | 江苏天晟药业有限公司 | Application of glabridin |
| CN105777771A (en) * | 2016-05-06 | 2016-07-20 | 青海省青海湖药业有限公司 | Method for extracting and purifying glabridin from glycyrrhiza glabra residues |
| CN106798654A (en) * | 2015-11-26 | 2017-06-06 | 无限极（中国）有限公司 | The application of glabridin |
-
2004
- 2004-09-15 CN CN 200410079233 patent/CN1273471C/en not_active Expired - Fee Related
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101519408B (en) * | 2008-02-27 | 2012-08-29 | 新疆富沃药业有限公司 | Method for producing glabridin from glycyrrhiza residue |
| CN101735233B (en) * | 2009-12-11 | 2011-11-16 | 暨南大学 | Method for producing high-purity glabridin |
| CN101830906B (en) * | 2009-12-13 | 2012-06-27 | 成都普思生物科技有限公司 | Separation and purification method of high-purity glabridin |
| CN103848841A (en) * | 2012-11-29 | 2014-06-11 | 陕西华泰生物精细化工有限公司 | Method of extracting high-purity glabridin from licorice waste residue by adoption of new technology |
| CN103848841B (en) * | 2012-11-29 | 2016-01-20 | 陕西华泰生物精细化工有限公司 | Employ new technology from licorice slag, extract the method for high-purity glabrene |
| CN104277048A (en) * | 2013-07-10 | 2015-01-14 | 岳普湖天瑞生物工程有限公司 | Preparation method for glycyrrhiza glabra total flavonoids |
| CN104277048B (en) * | 2013-07-10 | 2016-09-21 | 岳普湖天瑞生物工程有限公司 | A kind of preparation method of Glycyrrhiza glabra L. total flavones |
| CN104072512A (en) * | 2014-07-21 | 2014-10-01 | 江苏天晟药业有限公司 | Method for preparing glabridin |
| CN104800206A (en) * | 2015-04-15 | 2015-07-29 | 江苏天晟药业有限公司 | Application of glabridin |
| CN106798654A (en) * | 2015-11-26 | 2017-06-06 | 无限极（中国）有限公司 | The application of glabridin |
| CN105777771A (en) * | 2016-05-06 | 2016-07-20 | 青海省青海湖药业有限公司 | Method for extracting and purifying glabridin from glycyrrhiza glabra residues |
| CN105777771B (en) * | 2016-05-06 | 2018-06-08 | 青岛新昆仑生物科技有限公司 | A kind of method of extraction purification glabridin in slag from glycyrrhiza glabra |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1273471C (en) | 2006-09-06 |
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