CN102432652A - Method for extracting astilbin from china root - Google Patents
Method for extracting astilbin from china root Download PDFInfo
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- CN102432652A CN102432652A CN2010102963354A CN201010296335A CN102432652A CN 102432652 A CN102432652 A CN 102432652A CN 2010102963354 A CN2010102963354 A CN 2010102963354A CN 201010296335 A CN201010296335 A CN 201010296335A CN 102432652 A CN102432652 A CN 102432652A
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Abstract
The invention relates to a method for extracting an astilbin from a china root. The method comprises the following steps: taking the china root as a raw material; extracting in a manner of water backflow; adding salt and acid, and depositing flavonoid glycoside; after degreasing deposition, dissolving in alcohol and adding a macro-porous resin column; utilizing water to remove impurities; utilizing the alcohol to elute in a gradient form; collecting the astilbin stream; and concentrating and re-crystallizing, thereby obtaining a product. The method for producing the astilbin has the advantages of convenience in operation, low cost, environmental friendliness, strong technical specificity, high yield and high purity.
Description
Technical field:
The present invention relates to a kind of method of from Rhizome of Glabrous Greenbrier, extracting astilbin, especially a kind of water carries that acid is heavy, macroporous resin separates, the method for recrystallization purification astilbin.
Background technology:
Rhizome of Glabrous Greenbrier is the not dry rhizome of platymiscium smilacis glabra Smilax glabra Roxb of Liliaceae greenbrier, has dehumidifying, detoxifcation, easing joint movement function.The main effective constituent of Rhizome of Glabrous Greenbrier and its extract is saponin(e and flavonoid compound.It is reported that the Rhizome of Glabrous Greenbrier aqueous extract has tangible anti-inflammatory action, the astilbin of extraction separation has tangible diuresis and analgesic activity from Rhizome of Glabrous Greenbrier.
Astilbin (astilbin) is nineteen fifty from the plant Herba astilbes chinensis, to extract the compound that obtains first by Kozo Hayashi and Kazuhiko Ouchi; According to bibliographical information, astilbin has the number of significant BA, comprises the inhibition CoA-reductase; Suppress aldose reductase; The protection liver, analgesia, Ivy extract etc.In recent years report again that astilbin has significant selectivity immunosuppressive action, and its selectively acting compares with immunosuppressor in the past and have clear superiority, therefore can be used as the treatment that a kind of new immunosuppressor is used for immune correlated disease.It is reported, astilbin in rhizoma smilacis glabrae medicinal material content at 0.08-0.53%.(Li Lei etc. " content of astilbin and trans-resveratrol in the HPLC method mensuration rhizoma smilacis glabrae medicinal material ")
Another name: Taxifolin-3-O-α-L-pyrans rhamnoside
Molecular weight: 450.408
Molecular formula: C
21H
22O
11
Molecular structure:
Compositional classification: flavonoid glycoside
Physico-chemical property: colourless crystallization, 180 ℃ of fusing points are soluble in boiling water, are dissolved in ether hardly.Unstable to photo-thermal, in being exposed to air, purity can decrease for a long time.
The report that extracts astilbin in the relevant plant is less; Most technologies extract as the part of total glycosides; Specificity is not strong; Chinese patent " smilax glabra saponins, flavone extract and preparation method thereof " like publication number CN101524458 is had to flavones saponin(e mixture with the alcohol extracting method of extraction; The Chinese patent of publication number CN101732540A " method of the effective component of total glycoside in the mensuration smilax glabra ethanol water solution extract " has obtained the glycoside material through the method for alcohol extracting, silica gel column chromatography, but astilbin content is lower; Some has only studied the part method of purification, can't constitute complete technology, like " extracting the technical study of total flavones in the Rhizome of Glabrous Greenbrier " such as Wang Jinhuang; Also have many measuring methods that derive from, can't be used for producing, like " the HPLC method is measured the content of astilbin in the Rhizome of Glabrous Greenbrier ", Zhang Xiaoyan etc. such as Chen Xing " content of astilbin in the rhizoma smilacis glabrae medicinal material of the different places of production of high effective liquid chromatography for measuring " etc.
Publication number CN1724552 " a kind of preparation method of astilbin " has set forth macroporous adsorbent resin and the polymeric amide separation method to astilbin; This technological design there is reference; Yet the impurity that wherein carries after the diacolation extraction is more; Consumption of organic solvent in the subsequent step is increased, bring the rising of production cost and increasing the weight of of environmental pressure.After experiment improves repeatedly, design following to the method for purification of astilbin in the Rhizome of Glabrous Greenbrier.
Summary of the invention:
The contriver tests through process optimization, has invented a kind of method of from Rhizome of Glabrous Greenbrier, extracting astilbin.This technology is simple to operation, and the PT is short, and product yield is high, and production cost is low.
The present invention adopts following technical scheme to realize:
A kind of method of from Rhizome of Glabrous Greenbrier, extracting astilbin is characterized in that comprising following steps:
1) water is carried: the arid soil Poria powder is broken to the 20-30 order, and refluxing extraction in the water, united extraction liquid vacuum concentration gets liquid concentrator;
2) acid is heavy: above-mentioned liquid concentrator adds 2-4% sodium-chlor while hot and stirs, and adds acid and is acidified to pH1-2, makes the Flavonoid substances deposition, leaches deposition, and the filtrating thin up filters once more, merges filter cake;
3) degreasing: filter cake is doubly measured ETHYLE ACETATE (V/W) washing with 2-3, the dry nonfatty solid that gets;
4) macroporous resin adsorption: nonfatty solid is dissolved in a small amount of dense ethanol; The saturated absorption of last macroporous resin column, towards post, the ethanol with 10-50% detects astilbin towards post up to effluent again with water; Change the 60-90% ethanol elution; Do not have astilbin up to elute, collect the astilbin elutriant, concentrate medicinal extract;
5) recrystallization: medicinal extract is dissolved in hot water, leaves standstill cooling, crystallization repeats 3-5 time, obtains product.
The consumption of said refluxing extraction water is 5-8 times (V/W) of raw material, extracts each 1-2 hour 2-3 time.
Said extracting solution is concentrated into the 1/4-6 of original volume.
Said acid is hydrochloric acid.
Said macroporous resin filler can be selected a kind of among AB-8 or the HPD-400 for use, and the used alcohol concn of upper prop is 90-95%, and consumption is just clarified with solution and is as the criterion.
The flow velocity of said water and ethanol elution is 2BV/h.
Said recrystallization rearing crystal time 2-3 hour.
In sum, there is following advantage in the present invention:
1, add acid the free astilbin is separated out, with salt can make acid heavy better effects if, this process does not need heat supply, than low-carbon economy;
2, utilize macroporous resin can be efficiently and less energy-consumption play separating effect, and can reuse comparatively environmental protection;
3, astilbin solvability in water is big with temperature variation, so the water recrystallization is effective, and cost is low, can not cause very serious potential safety hazard;
4, this technology is to the purification high-specificity of astilbin, and industry is amplified easily.
To combine embodiment to further specify the present invention below, but the scope that the present invention requires to protect is not limited to following embodiment.
Embodiment:
Embodiment 1:
The Poria cocos 2kg (astilbin content 0.23%) that fetches earth, pulverizing is 20 orders, adds 16L water, refluxing extraction 1 hour is extracted united extraction liquid 3 times.1/4 of extracting solution vacuum concentration to original volume adds 2% sodium-chlor while hot, stir add hcl acidifying to pH be 2, make the Flavonoid substances deposition, filter.Filtrating is continued thin up, filters.Merge twice filter cake and add the degreasing of 2 times of amount ETHYLE ACETATE; The exsiccant nonfatty solid is with the saturated dissolving of 90% ethanol; Mix a kind last AB-8 type macroporous resin, first water is colourless until elute with 2BV/h flow velocity eluting water solubility impurity, is eluted to the 2BV/h flow velocity with 10% ethanol and detects astilbin; Use 60% ethanol with 2BV/h flow velocity wash-out astilbin at last, get the astilbin elutriant.Astilbin is taken off the liquid concentrating under reduced pressure, place crystallization, growing the grain 2 hours repeats 5 times, leaches cryodrying, gets product 3.7g, content 97.2%.
Embodiment 2:
The Poria cocos 2kg (astilbin content 0.28%) that fetches earth, it is 20 orders that powder is pulverized, and adds 12L water, refluxing extraction 2 hours is extracted united extraction liquid 2 times.1/5 of extracting solution vacuum concentration to original volume adds 3% sodium-chlor while hot, stir add hcl acidifying to pH be 2, make the Flavonoid substances deposition, filter.Filtrating is continued thin up, filters.Merge twice filter cake and add the degreasing of 3 times of amount ETHYLE ACETATE; The exsiccant nonfatty solid is with the saturated dissolving of 95% ethanol; Mix kind saturated absorption of last AB-8 type macroporous resin, first water is colourless until elute with 2BV/h flow velocity eluting water solubility impurity, is eluted to the 2BV/h flow velocity with 30% ethanol and detects astilbin; Use 80% ethanol with 2BV/h flow velocity wash-out astilbin at last, get the astilbin elutriant.Astilbin is taken off the liquid concentrating under reduced pressure, place crystallization, growing the grain 2.5 hours repeats 4 times, leaches cryodrying, gets product 3.9g, content 98.5%.
Embodiment 3:
The Poria cocos 2kg (astilbin content 0.3%) that fetches earth, pulverizing is 30 orders, adds 15L water, refluxing extraction 1 hour is extracted united extraction liquid 3 times.1/4 of extracting solution vacuum concentration to original volume adds 2% sodium-chlor while hot, stir add hcl acidifying to pH be 1, make the Flavonoid substances deposition, filter.Filtrating is continued thin up, filters.Merge twice filter cake and add the degreasing of 2 times of amount ETHYLE ACETATE; The exsiccant nonfatty solid is with the saturated dissolving of 90% ethanol; Mix kind saturated absorption of last HPD-400 type macroporous resin, first water is colourless until elute with 2BV/h flow velocity eluting water solubility impurity, is eluted to the 2BV/h flow velocity with 50% ethanol and detects astilbin; Use 90% ethanol with 2BV/h flow velocity wash-out astilbin at last, get the astilbin elutriant.Astilbin is taken off the liquid concentrating under reduced pressure, place crystallization, growing the grain 3 hours repeats 3 times, leaches cryodrying, gets product 4.8g, content 97.4%.
Embodiment 4:
The Poria cocos 2kg (astilbin content 0.26%) that fetches earth, pulverizing is 30 orders, adds 10L water, refluxing extraction 2 hours is extracted united extraction liquid 2 times.1/6 of extracting solution vacuum concentration to original volume adds 4% sodium-chlor while hot, stir add hcl acidifying to pH be 1, make the Flavonoid substances deposition, filter.Filtrating is continued thin up, filters.Merge twice filter cake and add the degreasing of 3 times of amount ETHYLE ACETATE; The exsiccant nonfatty solid is with the saturated dissolving of 90% ethanol; Mix kind saturated absorption of last HPD-400 type macroporous resin, first water is colourless until elute with 2BV/h flow velocity eluting water solubility impurity, is eluted to the 2BV/h flow velocity with 40% ethanol and detects astilbin; Use 70% ethanol with 2BV/h flow velocity wash-out astilbin at last, get the astilbin elutriant.Astilbin is taken off the liquid concentrating under reduced pressure, place crystallization, growing the grain 3 hours repeats 3 times, leaches cryodrying, gets product 4.2g, content 98.8%.
Claims (7)
1. method of from Rhizome of Glabrous Greenbrier, extracting astilbin is characterized in that comprising following steps:
1) water is carried: the arid soil Poria powder is broken to the 20-30 order, and refluxing extraction in the water, united extraction liquid vacuum concentration gets liquid concentrator;
2) acid is heavy: above-mentioned liquid concentrator adds 2-4% sodium-chlor while hot and stirs, and adds acid and is acidified to pH1-2, makes the Flavonoid substances deposition, leaches deposition, and the filtrating thin up filters once more, merges filter cake;
3) degreasing: filter cake is doubly measured ETHYLE ACETATE (V/W) washing with 2-3, the dry nonfatty solid that gets;
4) macroporous resin adsorption: nonfatty solid is dissolved in a small amount of dense ethanol; The saturated absorption of last macroporous resin column, towards post, the ethanol with 10-50% detects astilbin towards post up to effluent again with water; Change the 60-90% ethanol elution; Do not have astilbin up to elute, collect the astilbin elutriant, concentrate medicinal extract;
5) recrystallization: medicinal extract is dissolved in hot water, leaves standstill cooling, crystallization repeats 3-5 time, obtains product.
2. preparation method as claimed in claim 1, the consumption that it is characterized in that step 1) refluxing extraction water is 5-8 times (V/W) of raw material, extracts each 1-2 hour 2-3 time.
3. preparation method as claimed in claim 1 is characterized in that the step 1) extracting solution is concentrated into the 1/4-6 of original volume.
4. preparation method as claimed in claim 1 is characterized in that step 2) acid is for hydrochloric acid.
5. preparation method as claimed in claim 1 is characterized in that step 3) macroporous resin filler can select a kind of among AB-8 or the HPD-400 for use, and the used alcohol concn of upper prop is 90-95%, and consumption is just clarified with solution and is as the criterion.
6. preparation method as claimed in claim 1, the flow velocity that it is characterized in that step 3) water and ethanol elution is 2BV/h.
7. preparation method as claimed in claim 1 is characterized in that step 4) recrystallization rearing crystal time 2-3 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2010102963354A CN102432652A (en) | 2010-09-29 | 2010-09-29 | Method for extracting astilbin from china root |
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| CN2010102963354A CN102432652A (en) | 2010-09-29 | 2010-09-29 | Method for extracting astilbin from china root |
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| CN102432652A true CN102432652A (en) | 2012-05-02 |
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| CN2010102963354A Pending CN102432652A (en) | 2010-09-29 | 2010-09-29 | Method for extracting astilbin from china root |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102964407A (en) * | 2012-12-15 | 2013-03-13 | 广东世信药业有限公司 | Method for extracting astilbin from rhizoma smilacis glabrae and astilbin prepared thereby |
| CN105056027A (en) * | 2015-08-05 | 2015-11-18 | 贵阳中医学院 | Red-section Smilax ocreafa A. DC effective part and use thereof |
| CN108675978A (en) * | 2018-05-28 | 2018-10-19 | 江西农业大学 | A method of preparing high-purity texifolin by raw material of smilax |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020040050A1 (en) * | 1998-09-14 | 2002-04-04 | Qiang Xu | Immunosuppressive agents |
| CN1724552A (en) * | 2005-07-08 | 2006-01-25 | 南京大学 | Preparation method of astilbin |
| CN101804064A (en) * | 2010-04-08 | 2010-08-18 | 成都军区昆明总医院 | Application of dihydroquercetin and glucoside compounds to preparing drug-resistance bacteria medicine |
-
2010
- 2010-09-29 CN CN2010102963354A patent/CN102432652A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020040050A1 (en) * | 1998-09-14 | 2002-04-04 | Qiang Xu | Immunosuppressive agents |
| CN1724552A (en) * | 2005-07-08 | 2006-01-25 | 南京大学 | Preparation method of astilbin |
| CN101804064A (en) * | 2010-04-08 | 2010-08-18 | 成都军区昆明总医院 | Application of dihydroquercetin and glucoside compounds to preparing drug-resistance bacteria medicine |
Non-Patent Citations (1)
| Title |
|---|
| 曾祥腾，等: "大孔吸附树脂富集纯化土茯苓总黄酮的研究", 《今日药学》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102964407A (en) * | 2012-12-15 | 2013-03-13 | 广东世信药业有限公司 | Method for extracting astilbin from rhizoma smilacis glabrae and astilbin prepared thereby |
| CN105056027A (en) * | 2015-08-05 | 2015-11-18 | 贵阳中医学院 | Red-section Smilax ocreafa A. DC effective part and use thereof |
| CN105056027B (en) * | 2015-08-05 | 2019-12-17 | 贵州中医药大学 | Effective part of glabrous greenbrier rhizome with red section and application thereof |
| CN108675978A (en) * | 2018-05-28 | 2018-10-19 | 江西农业大学 | A method of preparing high-purity texifolin by raw material of smilax |
| CN108675978B (en) * | 2018-05-28 | 2021-06-01 | 江西农业大学 | Method for preparing high-purity taxifolin by taking rhizoma smilacis glabrae as raw material |
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Application publication date: 20120502 |