CN102250164A - Purification method of gastrodin - Google Patents
Purification method of gastrodin Download PDFInfo
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- CN102250164A CN102250164A CN2011102259430A CN201110225943A CN102250164A CN 102250164 A CN102250164 A CN 102250164A CN 2011102259430 A CN2011102259430 A CN 2011102259430A CN 201110225943 A CN201110225943 A CN 201110225943A CN 102250164 A CN102250164 A CN 102250164A
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- gastrodine
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Abstract
The invention relates to a purification method of gastrodin. The method comprises the following specific steps: (1) using an alcohol-containing solution to perform ultrasonic extraction on gastrodin medicinal herb powder, collecting extract, concentrating to ensure that the extract has no alcohol; and (2) purifying a concentrated solution with polyamide resins, adopting ethanol-water (0-60%) to perform gradient elution, collecting the target eluent, concentrating to reach a small volume, adopting the dry method to add the concentrated target eluent with a small volume into an octadecylsilyl (ODS) silica gel column, eluting with an ethanol-water mixed solvent or an acetonitrile-water mixed solvent, recycling the solvent from the eluent, and drying to obtain gastrodin. The method has the advantages of low energy consumption, short preparation period and high product purity.
Description
Technical field
The invention belongs to the Separation of Natural Products field, relate in particular to the method for the refining Gastrodine of a kind of ODS of employing reverse phase silica gel method.
Background technology
Rhizoma Gastrodiae be the orchid rhizoma Gastrodiae (
Gastrodia elataBl.) dry tuber.Rhizoma Gastrodiae has suppressing hyperactive liver for calming endogenous wind, ends the effect of convulsion, is used for the treatment of diseases such as headache is dizzy, numb limbs and tense tendons, infantile convulsion, epilepsy clonus, tetanus.Have and studies show that the main active ingredient of rhizoma Gastrodiae is the Gastrodine compounds, wherein, rhizoma Gastrodiae have analgesia, calmness and cerebral blood flow increasing amount, reduce the cerebral blood flow resistance, particularly can increase the vertebra basilar arterial blood supply, improve labyrinthine artery and inner ear blood is made for usefulness, Chang Zuowei rhizoma Gastrodiae quality of medicinal material controlling index composition.Recent study finds that Gastrodine also has the intelligence of increasing, brain tonic, function in delaying senility, and senile dementia is had certain curative effect.
Gastrodine (Gastrodin), CAS:62499-27-8, molecular formula: C
13H
18O
7, molecular weight: 286.28, chemical name: 4-hydroxybenzene-β-D-glucopyranoside.Physicochemical property: be white, needle-shaped crystals, 154～155 ℃ of fusing points.Soluble in water, methyl alcohol, ethanol are insoluble to chloroform and ether.
The method of extracting Gastrodine in the prior art has enzymolysis process, ultrasonic method etc., as document " technical study of Gastrodine in the Enzymatic Extraction rhizoma Gastrodiae ", the document adopts high performance liquid chromatography to detect the content of Gastrodine, determine the optimum extraction process condition of Gastrodine by single factor and orthogonal test, but do not related to being further purified of Gastrodine; (patent No.: 200710134318.9), this patent adopts alcohol heat reflux to extract to patent " a kind of preparation method of gastrodia tuber dispensing granule ", and the dregs of a decoction add the water refluxing extraction again, concentrate, and spraying drying gets Gastrodine.The employing thermal backflow is extracted, the easy gelatinization of the starch in the rhizoma Gastrodiae, and extracting solution is difficult to handle.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of high-load Gastrodine, this method is easy and simple to handle, and energy consumption is relatively little, and the Gastrodine that makes is purer.
In order to solve the problems of the technologies described above the object of the present invention is achieved like this:
A kind of method of purification of Gastrodine is characterized in that comprising following steps:
1) the rhizoma Gastrodiae medicinal powder is added the alcoholic liquor supersound extraction 2 ~ 4 times of 5 ~ 12 times of amounts, extract 1 ~ 3h at every turn, extracting solution is concentrated into does not have alcohol;
2) above-mentioned concentrated solution is crossed the polyamide resin column purification, use 0-20%, 20-40%, 40-60% aqueous ethanolic solution gradient elution respectively, collecting the target elutriant concentrates, with the ODS silica gel mixed sample, volatilize solvent, last sample is with methanol-water or acetonitrile-water mixed solvent wash-out, collect elutriant, concentrate drying promptly gets product.
Alcoholic liquor in the described step 1) is meant 40 ~ 70% ethanol or methanol solution.
Described step 2) ODS silica gel consumption is 1/2 ~ 1(W/W) of a medicinal material amount in, and eluting solvent is 55 ~ 70% methanol-waters or acetonitrile-water.
Present method positively effect is:
1) adopt the alcoholic liquor supersound extraction, reduce the starch stripping, prevent gelatinization, extracting solution is easy to handle;
1) present method adopts ODS silicagel column purifying, can obtain highly purified Gastrodine, and silica gel can reuse;
2) operation of present method processing step is simpler, easy to operate, products obtained therefrom purity height.
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:
Get rhizoma Gastrodiae medicinal powder 1kg, add the 40% methanol solution refluxing extraction 2 times of 5L, extract 1h at every turn, extracting solution reclaims solvent to there not being the alcohol flavor, crosses the polyamide resin purifying, respectively water, 20%, 60% aqueous ethanolic solution gradient elution, collect 20%, 60% elutriant and merge, concentrate, get 450gODS silica gel dress post again, other gets 50gODS silica gel and concentrated solution is mixed sample, volatilize solvent, upper prop with 60% methanol aqueous solution wash-out, is collected elutriant, concentrate drying promptly gets product 8.3g, content 99.1%.
Embodiment 2:
Get rhizoma Gastrodiae medicinal powder 1kg, add the 70% ethanol liquid refluxing extraction 4 times of 12L, extract 3h at every turn, extracting solution reclaims solvent to there not being the alcohol flavor, crosses the polyamide resin purifying, uses 20%, 40%, 60% aqueous ethanolic solution gradient elution respectively, collect 40%, 60% elutriant and merge, concentrate, get 1000gODS silica gel dress post again, other gets 125gODS silica gel and concentrated solution is mixed sample, volatilize solvent, upper prop with 55% acetonitrile solution wash-out, is collected elutriant, concentrate drying promptly gets product 10.1g, content 99.3%.
Embodiment 3:
Get rhizoma Gastrodiae medicinal powder 5kg, add the 50% ethanol liquid refluxing extraction 3 times of 40L, extract 2h at every turn, extracting solution reclaims solvent to there not being the alcohol flavor, crosses the polyamide resin purifying, uses 10%, 30%, 50% aqueous ethanolic solution gradient elution respectively, collect 20-40%, the merging of 40-60% elutriant, concentrate, get 3kgODS silica gel dress post again, other gets 300gODS silica gel and concentrated solution is mixed sample, volatilize solvent, upper prop with 70% methanol aqueous solution wash-out, is collected elutriant, concentrate drying promptly gets product 45.7g, content 98.7%.
Claims (3)
1. the method for purification of a Gastrodine is characterized in that comprising following steps:
1) the rhizoma Gastrodiae medicinal powder is added the alcoholic liquor supersound extraction 2 ~ 4 times of 5 ~ 12 times of amounts, extract 1 ~ 3h at every turn, extracting solution is concentrated into does not have alcohol;
2) above-mentioned concentrated solution is crossed the polyamide resin column purification, use 0-20%, 20-40%, 40-60% aqueous ethanolic solution gradient elution respectively, collecting the target elutriant concentrates, with the ODS silica gel mixed sample, volatilize solvent, last sample is with methanol-water or acetonitrile-water mixed solvent wash-out, collect elutriant, concentrate drying promptly gets product.
2. the method for purification of a kind of Gastrodine as claimed in claim 1 is characterized in that the alcoholic liquor in the described step 1) is meant 40 ~ 70% ethanol or methanol solution.
3. the method for purification of a kind of Gastrodine as claimed in claim 1 is characterized in that described step 2) in ODS silica gel consumption be 1/2 ~ 1(W/W) of medicinal material amount, eluting solvent is 55 ~ 70% methanol-waters or acetonitrile-water.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011102259430A CN102250164A (en) | 2011-08-09 | 2011-08-09 | Purification method of gastrodin |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011102259430A CN102250164A (en) | 2011-08-09 | 2011-08-09 | Purification method of gastrodin |
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| CN102250164A true CN102250164A (en) | 2011-11-23 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103788148A (en) * | 2014-02-13 | 2014-05-14 | 悦康药业集团有限公司 | Gastrodin compound and preparation thereof |
| CN104262424A (en) * | 2014-10-17 | 2015-01-07 | 神农架绿野食品开发有限责任公司 | Method for extracting gastrodin |
| CN104592324A (en) * | 2015-02-05 | 2015-05-06 | 西安艾克瑞科贸有限公司 | Gastrodin extraction and purification method |
| CN104710484A (en) * | 2015-01-08 | 2015-06-17 | 中国标准化研究院 | Gastrodin extraction and separation method |
| CN106986904A (en) * | 2017-05-08 | 2017-07-28 | 铜仁学院 | A kind of Gastrodin extracted in the anesthesia stem from day and preparation method thereof |
| CN110845553A (en) * | 2019-11-25 | 2020-02-28 | 湖南省博世康中医药有限公司 | Method for extracting gastrodin by ultrasonic water bath heating |
-
2011
- 2011-08-09 CN CN2011102259430A patent/CN102250164A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103788148A (en) * | 2014-02-13 | 2014-05-14 | 悦康药业集团有限公司 | Gastrodin compound and preparation thereof |
| CN103788148B (en) * | 2014-02-13 | 2015-11-04 | 悦康药业集团有限公司 | Gastrodin compound and preparation thereof |
| CN104262424A (en) * | 2014-10-17 | 2015-01-07 | 神农架绿野食品开发有限责任公司 | Method for extracting gastrodin |
| CN104262424B (en) * | 2014-10-17 | 2016-04-13 | 神农架绿野食品开发有限责任公司 | The extracting method of Gastrodine |
| CN104710484A (en) * | 2015-01-08 | 2015-06-17 | 中国标准化研究院 | Gastrodin extraction and separation method |
| CN104592324A (en) * | 2015-02-05 | 2015-05-06 | 西安艾克瑞科贸有限公司 | Gastrodin extraction and purification method |
| CN106986904A (en) * | 2017-05-08 | 2017-07-28 | 铜仁学院 | A kind of Gastrodin extracted in the anesthesia stem from day and preparation method thereof |
| CN110845553A (en) * | 2019-11-25 | 2020-02-28 | 湖南省博世康中医药有限公司 | Method for extracting gastrodin by ultrasonic water bath heating |
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Application publication date: 20111123 |