CN101967504A - Method for extracting isofraxidin - Google Patents
Method for extracting isofraxidin Download PDFInfo
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- CN101967504A CN101967504A CN2010102107024A CN201010210702A CN101967504A CN 101967504 A CN101967504 A CN 101967504A CN 2010102107024 A CN2010102107024 A CN 2010102107024A CN 201010210702 A CN201010210702 A CN 201010210702A CN 101967504 A CN101967504 A CN 101967504A
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- isofraxidin
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Abstract
The invention relates to a method for extracting isofraxidin, which comprises the following steps of: pulverizing acanthopanax root serving as a raw material, and adding 10 to 20 percent water for wetting; adding biological enzyme for enzymolysis in the normal state for 3 to 10 days, and after the enzymolysis, extracting through the reflux in 80 to 90 percent methyl alcohol; and concentrating extracting solution under reduced pressure, adding ethyl acetate for dissolving to remove aqueous layer, decolorizing through an activated carbon alumina mixed column to remove impurities, concentrating and crystallizing, recrystallizing through the reflux of chloroform and acetone, and drying crystals at the low temperature to obtain the isofraxidin. In the method for extracting the isofraxidin, the product yield is high, the operation is simple, the repeatability is good, and the enlargement production is easy to perform.
Description
Technical field:
The present invention relates to a kind of extracting method of Isofraxidin, especially a kind of biological enzymolysis and recrystallization extract the method for Isofraxidin.
Background technology:
Isofraxidin is isofraxidin, isofraxidin, coumarin kind compound again.
Molecular formula: C
11H
10O
5
Molecular structural formula::
Isofraxidin Radix Et Caulis Acanthopanacis Senticosi glucoside B
1
Be dissolved in methyl alcohol, ethanol, acetone, chloroform, boiling water, alkaline aqueous solution, be slightly soluble in ether, be insoluble in sherwood oil, cold water.Isofraxidin has the sedative effect of calming the nerves, and can shorten time for falling asleep, improves sleep quality, also has anti-inflammatory, antitumor action.
The Isofraxidin content of free state is not high in the Radix Et Caulis Acanthopanacis Senticosi only has about 0.3%, and some is that the Isofraxidin of chemical combination attitude is a Radix Et Caulis Acanthopanacis Senticosi glucoside, extracts the more Isofraxidin of volume from Radix Et Caulis Acanthopanacis Senticosi, be the Radix Et Caulis Acanthopanacis Senticosi glucoside hydrolysis.
The existing technology of extracting Isofraxidin has:
" optimal conditions of the Isofraxidin glucoside hydrolysis research in the Radix Et Caulis Acanthopanacis Senticosi " that Sun Huafang etc. deliver, the document adopts and adds 100 ℃ of hydrolysis of 5% sulfuric acid 5 hours.
" the hydrolysis original position extracting and separating Radix Et Caulis Acanthopanacis Senticosi isofraxidin " that Yang Lei etc. deliver, the document adopt and add 85 ℃ of hydrolysis of hydrochloric acid dichloromethane extraction method simultaneously.
" research of sarcandra glaber chemical ingredients and finger printing " that Wang Binglan delivers, the document is extraction using alcohol from sarcandra glaber, and ethyl acetate extraction, silicagel column separate the high-content Isofraxidin of system repeatedly, also adopt high speed adverse current chromatogram to prepare the high-content Isofraxidin.
Patent (application number 02109475) " is produced the method for Isofraxidin, eleutheroside, Radix Et Caulis Acanthopanacis Senticosi polysaccharide " with Radix Et Caulis Acanthopanacis Senticosi, the disclosed method of this patent be the Radix Et Caulis Acanthopanacis Senticosi rhizome pulverize oven dry → supercritical carbon dioxide extraction → waste residue behind Isofraxidin → alcohol at normal temperature lixiviate supercritical carbon dioxide extraction → concentrate vat liquor → macroporous resin column chromatography → wash-out → concentrate eluant freeze-drying handle the concentrated vat liquor crossed of eleutheroside → resin absorption through decolouring, concentrated, freeze-drying handle Radix Et Caulis Acanthopanacis Senticosi polysaccharide.
As above-mentioned institute, existing technology exists that extract yield is low, the operating process reaction is violent, turnout is little and the problem of poor reproducibility.
Summary of the invention:
The technical problem to be solved in the present invention provides a kind of extracting method of Isofraxidin, and this method can improve the Isofraxidin yield, reduces production costs.
In order to solve the problems of the technologies described above, extractive technique scheme of the present invention is as follows:
A kind of extracting method of Isofraxidin is characterized in that comprising following steps:
1) pulverizes enzymolysis: with Radix Et Caulis Acanthopanacis Senticosi pulverizing medicinal materials 40-80 order, add 10-20% water, mix thoroughly and add biological enzyme again, natural enzymolysis 3-10 days;
2) extract: get above-mentioned enzymolysis raw material and add the 6-15BV80-90%% methanol eddy and extracted 1-3 hour, extract 1-3 time, merge extracting solution;
3) decolouring removal of impurities: methyl alcohol is reclaimed in the pressurization of said extracted liquid, add 4-9BV ethyl acetate heating for dissolving in the concentrated solution and remove water layer, add the decolouring of gac aluminum oxide mixing column, fluid injection reclaim under reduced pressure ethyl acetate is to original volume 1/3-1/8 under collecting, adding a small amount of petroleum ether and stirring has precipitation only to separate out, and places crystallization;
4) recrystallization: leach the coarse crystallization thing, use chloroform, acetone crystallization successively, vacuum low-pressure is drying to obtain Isofraxidin.
Described step 1) is pulverized enzymatic hydrolysis condition: the optional cellulase of enzyme, beta-glucanase or naringinase one or more, enzyme addition 1-5 ‰.Preferred beta-glucanase.
5. in the described step 3) in the gac aluminum oxide mixing column activated carbon alumina ration be 1: 3-6.Aluminum oxide is a 100-200 order neutral alumina, and gac is a grain active carbon.Preferred proportion 1: 4.
Described step 4) recrystallization is the dissolving refrigeration crystallization that refluxes, refrigerating temperature 0-4 ℃.
There is following advantage in the present invention:
1) product yield height, technology is simple to operation, is easy to industrialization.
2) biological enzymolysis process gentleness, pollution level is far smaller than acid hydrolysis.
3) aluminium oxide active charcoal mixing column decolouring good impurity removing effect.
Further specify the present invention below in conjunction with embodiment, but the scope of protection of present invention is not limited to following embodiment.
Embodiment:
Embodiment 1:
40 orders are pulverized in the Radix Et Caulis Acanthopanacis Senticosi impurity elimination, get 1kg, add 200ml water, mix thoroughly and add the 5g cellulase again, natural enzymolysis 5 days, taking-up drops into and adds 6L80% methanol eddy extraction extraction in 1 hour 3 times in the flask, and extracting solution Rotary Evaporators recovery methyl alcohol adds 4BV ethyl acetate heating for dissolving and removes water layer in the concentrated solution, add the decolouring of gac aluminum oxide (1: 4) post, fluid injection reclaim under reduced pressure ethyl acetate is to original volume 1/8 under collecting, and adding a small amount of petroleum ether and stirring has precipitation only to separate out, and places crystallization; Leach coarse crystallization, refluxing to dissolve with chloroform, acetone successively refrigerates crystallization in 0-4 ℃ of environment, and vacuum low-pressure is drying to obtain Isofraxidin 3.4g, content 95%.
Embodiment 2:
80 orders are pulverized in the Radix Et Caulis Acanthopanacis Senticosi impurity elimination, get 5kg, add 800ml water, mix thoroughly and add the 5g beta-glucanase again, natural enzymolysis 10 days, taking-up drops into and adds 50L90% methanol eddy extraction extraction in 2 hours 2 times in the multi-function extractor, and united extraction liquid recovery methyl alcohol adds 9BV ethyl acetate heating for dissolving and removes water layer in the concentrated solution, add the decolouring of gac aluminum oxide (1: 6) post, fluid injection reclaim under reduced pressure ethyl acetate is to original volume 1/3 under collecting, and adding a small amount of petroleum ether and stirring has precipitation only to separate out, and places crystallization; Leach coarse crystallization, refluxing to dissolve with chloroform, acetone successively refrigerates crystallization in 0-4 ℃ of environment, and vacuum low-pressure is drying to obtain Isofraxidin 20g, content 98%.
Embodiment 3:
60 orders are pulverized in the Radix Et Caulis Acanthopanacis Senticosi impurity elimination, get 5kg, add 1000ml water, mix thoroughly and add the 15g naringinase again, natural enzymolysis 7 days, taking-up drops into and adds 75L85% methanol eddy extraction extraction in 3 hours 1 time in the multi-function extractor, and united extraction liquid recovery methyl alcohol adds 6BV ethyl acetate heating for dissolving and removes water layer in the concentrated solution, add the decolouring of gac aluminum oxide (1: 3) post, fluid injection reclaim under reduced pressure ethyl acetate is to original volume 1/5 under collecting, and adding a small amount of petroleum ether and stirring has precipitation only to separate out, and places crystallization; Leach coarse crystallization, refluxing to dissolve with chloroform, acetone successively refrigerates crystallization in 0-4 ℃ of environment, and vacuum low-pressure is drying to obtain Isofraxidin 14g, content 97%.
Embodiment 4:
40 orders are pulverized in the Radix Et Caulis Acanthopanacis Senticosi impurity elimination, get 10kg, add 2L water, mix thoroughly and add the 15g beta-glucanase again, natural enzymolysis 5 days, taking-up drops into and adds 60L90% methanol eddy extraction extraction in 1 hour 3 times in the multi-function extractor, and united extraction liquid recovery methyl alcohol adds 8BV ethyl acetate heating for dissolving and removes water layer in the concentrated solution, add the decolouring of gac aluminum oxide (1: 64) post, fluid injection reclaim under reduced pressure ethyl acetate is to original volume 1/6 under collecting, and adding a small amount of petroleum ether and stirring has precipitation only to separate out, and places crystallization; Leach coarse crystallization, refluxing to dissolve with chloroform, acetone successively refrigerates crystallization in 0-4 ℃ of environment, and vacuum low-pressure is drying to obtain Isofraxidin 38g, content 99%.
Claims (4)
1. the extracting method of an Isofraxidin is characterized in that comprising following steps:
1) pulverizes enzymolysis: with Radix Et Caulis Acanthopanacis Senticosi pulverizing medicinal materials 40-80 order, add 10-20% water, mix thoroughly and add biological enzyme again, natural enzymolysis 3-10 days;
2) extract: get above-mentioned enzymolysis raw material and add the 6-15BV80-90% methanol eddy and extracted 1-3 hour, extract 1-3 time, merge extracting solution;
3) decolouring removal of impurities: methyl alcohol is reclaimed in the pressurization of said extracted liquid, add its volume 4-9BV ethyl acetate heating for dissolving in the concentrated solution and remove water layer, add the decolouring of gac aluminum oxide mixing column, fluid injection reclaim under reduced pressure ethyl acetate is to original volume 1/3-1/8 under collecting, adding a small amount of petroleum ether and stirring has precipitation only to separate out, and places crystallization;
4) recrystallization: leach the coarse crystallization thing, use chloroform, acetone crystallization successively, vacuum low-pressure is drying to obtain Isofraxidin.
Such as claim 1 the extracting method of Isofraxidin, it is characterized in that described step 1) pulverizes enzymatic hydrolysis condition and be: the optional cellulase of enzyme, beta-glucanase or naringinase one or more, enzyme addition 1-5 ‰.
3. the extracting method of Isofraxidin according to claim 1 is characterized in that in the described step 3) that the activated carbon alumina ration is 1 in the gac aluminum oxide mixing column: 3-6, and aluminum oxide is a 100-200 order neutral alumina, gac is a grain active carbon.
4. the extracting method of Isofraxidin according to claim 1 is characterized in that described step 4) recrystallization is the cold good crystallization of dissolving that refluxes, cold good temperature 0-4 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102107024A CN101967504A (en) | 2010-06-28 | 2010-06-28 | Method for extracting isofraxidin |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102107024A CN101967504A (en) | 2010-06-28 | 2010-06-28 | Method for extracting isofraxidin |
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| CN101967504A true CN101967504A (en) | 2011-02-09 |
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| CN2010102107024A Pending CN101967504A (en) | 2010-06-28 | 2010-06-28 | Method for extracting isofraxidin |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103720733A (en) * | 2014-01-23 | 2014-04-16 | 程钰翔 | Preparation method of manyprickle acanthopanax root extract |
| CN108484557A (en) * | 2018-06-15 | 2018-09-04 | 东北林业大学 | A method of extracting isofraxidin from wilsonii |
-
2010
- 2010-06-28 CN CN2010102107024A patent/CN101967504A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103720733A (en) * | 2014-01-23 | 2014-04-16 | 程钰翔 | Preparation method of manyprickle acanthopanax root extract |
| CN108484557A (en) * | 2018-06-15 | 2018-09-04 | 东北林业大学 | A method of extracting isofraxidin from wilsonii |
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Application publication date: 20110209 |