CN103479856A - Rhizoma anemarrhenae chemical component cluster extracts and preparation process thereof - Google Patents
Rhizoma anemarrhenae chemical component cluster extracts and preparation process thereof Download PDFInfo
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- CN103479856A CN103479856A CN201310430996.5A CN201310430996A CN103479856A CN 103479856 A CN103479856 A CN 103479856A CN 201310430996 A CN201310430996 A CN 201310430996A CN 103479856 A CN103479856 A CN 103479856A
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Abstract
The invention belongs to the technical field of medicine, and discloses three kinds of rhizoma anemarrhenae chemical component cluster extracts and a preparation process thereof. According to the three kinds of extracts disclosed by the invention, the rhizoma anemarrhenae medicine material source is comprehensively utilized, so that the medicinal material is reduced, and water soluble and fat soluble ingredients are fully utilized. The three kinds of extracts are the rhizoma anemarrhenae total saponin extract, the rhizoma anemarrhenae total sapogenin extract and the rhizoma anemarrhenae polysaccharide extract respectively, wherein the weight contents of both the total saponins and total sapogenin of the extracts are greater than 50%, and the weight content of the total polysaccharides of the extracts is 50-95%. The preparation method and process are simple, and the content is stable.
Description
Technical field
The invention belongs to medical technical field, relate to three kinds of chemical composition group extracts of the Rhizoma Anemarrhenae and preparation technology thereof, according to three kinds of extracts of this preparation technology's gained, its chemical composition total content can reach more than 50%.
Background technology
The main chemical compositions of the Rhizoma Anemarrhenae is steroidal saponin and polysaccharide, and the amount of steroidal saponin in rhizome is about 6%, and the sapogenin after these two kinds of chemical composition groups and saponin hydrolysis all has clear and definite pharmacological action.Anemaran have regulate immunologic function, resisting fatigue, protect the liver, antioxidation, defying age and antineoplastic action; Extraced total timosaponin has the control senile dementia, improves the pharmacological actions such as memory, anticoagulant, antioxidation and blood sugar lowering; The Sarsasapogenin Cholinergic low to senile dementia has some improvement and therapeutical effect, can promote osteoblastic propagation and the differentiation and maturation of In vitro culture.
At present, Rhizoma Anemarrhenae Chinese patent medicine or extract manufacturer majority when producing only extracts a kind of effective site, after extracting, remaining medical material does not take full advantage of and extracts its polysaccharide, cause the waste of resource, current sold Rhizoma Anemarrhenae extract is the ratio extract in addition, extraction process is coarse, and active constituent content is low.Chinese patent 03115509.X discloses a kind of Rhizoma Anemarrhenae extract and preparation method thereof, but its disclosed be the Rhizoma Anemarrhenae extract that in Rhizoma Anemarrhenae extract, the content summation of chimonin and Neomangiferin is greater than 50%.Chinese patent 200510024312.7 discloses the new purposes of extraced total timosaponin, but the main component of this total saponin extracts is the Rhizoma Anemarrhenae saponin B-Ⅱ compound, and content range is 30% ~ 70%.Chinese patent 200510054633.1 discloses a kind of Rhizoma Anemarrhenae total saponins and preparation method thereof, and the preparation method of this Rhizoma Anemarrhenae total saponins is for adopting the room temperature supersound extraction.Above patent has all only been extracted Rhizoma Anemarrhenae total saponins, and main constituent is different, content is different, and adopts extracting method also different; Extract and prepare three kinds of chemical composition groups in the Rhizoma Anemarrhenae simultaneously, the method for Rhizoma Anemarrhenae total saponins, anemarrhena total sapogenin, anemaran have not been reported.
Summary of the invention
The present invention is directed in above production and obtain not enough and technical difference, the whole preparation technology of three kinds of chemical composition groups of a kind of Rhizoma Anemarrhenae is provided, and the three kinds of extracts and the relevant dosage form thereof that according to this technique preparation, obtain.
The present invention completes by following technical method:
The whole preparation technology of three kinds of chemical composition groups of the Rhizoma Anemarrhenae, key step is as follows:
(1) Rhizoma Anemarrhenae is cleaned, added appropriate distilled water moistening 6 ~ 12h, cut sheet;
(2) Rhizoma Anemarrhenae sheet is extracted 2 times with 75 ~ 95% alcohol heating reflux, filter, merge extractive liquid,, decompression recycling ethanol, concentrated, obtain the alcohol extraction concentrated solution;
(3) the alcohol extraction concentrated solution, use macroporous adsorbing resin for purification, and with water and 75 ~ 95% ethanol elutions, water elution liquid discards respectively, merges ethanol elution, decompression recycling ethanol, and concentrated, drying under reduced pressure, obtain extraced total timosaponin, and its total saponins weight content is greater than 50%;
(4) the extraced total timosaponin adding distil water dissolves, and adds diluted acid, and heating hydrolysis generates aglycon, hydrolyzed solution is neutralized to neutrality with alkali, then by chloroform or ethyl acetate, extracts aglycon, reclaims solvent, drying under reduced pressure, obtain the anemarrhena total sapogenin extract, and its total sapogenins weight content is greater than 80%;
(5) by medicinal residues drying after alcohol extraction, use distilled water heating and refluxing extraction 2 ~ 3 times, filter, merging filtrate, concentrating under reduced pressure, obtain water extracting liquid;
(6) add 95% ethanol to water extracting liquid, making containing the alcohol amount is 75 ~ 85%, fully stirs standing over night;
(7) filter, collecting precipitation, centrifugal or sucking filtration, will precipitate the reduced vacuum drying, obtain amorphous powder, be the anemaran extract, and its polysaccharide weight content is greater than 50%;
Three kinds of extracts that obtain according to above preparation technology can utilize preparation technique to make acceptable pharmaceutical dosage form clinically with pharmaceutically acceptable excipient or pharmaceutical carrier.The dosage form of telling can be solid preparation, Solid Releasing Fresh-keeping Agent or injection.
This preparation technology has the following advantages:
(1) avoided because only extracting the herb resource waste that a kind of chemical composition causes.
(2) this preparation technology does not relate to poisonous hazardous solvent, non-pollutant discharge, environmental friendliness.
(3) be designed into process route in the preparation and be the industrialized great production common method, simple and easy to do, be applicable to commercial production.
The specific embodiment
Embodiment 1:
The whole preparation technology of three kinds of chemical composition groups of the Rhizoma Anemarrhenae:
(1) get Rhizoma Anemarrhenae 1kg, clean, add 10% medical material weight distilled water moistening 6h, the moisture content complete wetting, cut sheet;
(2) Rhizoma Anemarrhenae sheet is extracted 2 times with 8 times of weight, 75% alcohol heating reflux, filter, merge extractive liquid,, decompression recycling ethanol, concentrated, obtain alcohol extraction concentrated solution 4L;
(3) alcohol extraction concentrated solution, use the 500ml macroporous adsorbing resin for purification, and respectively with water and 75% ethanol elution, water elution liquid 1L discards, collect ethanol elution 2L, decompression recycling ethanol, be concentrated into thick paste, drying under reduced pressure, obtain extraced total timosaponin 20g, and its total saponins weight content is 55%;
(4) extraced total timosaponin 10g adding distil water 100ml dissolves, add diluted acid, heating hydrolysis generates aglycon, be that the molish reaction is negative, hydrolyzed solution is neutralized to neutrality with alkali, then uses the chloroform extraction aglycon, reclaim solvent, drying under reduced pressure, obtain anemarrhena total sapogenin extract 4g, and its total sapogenins weight content is 82%;
(5) by residue drying after alcohol extraction, by 10 times of amount distilled water heating and refluxing extraction 2 times, filter, merging filtrate, concentrating under reduced pressure, obtain water extracting liquid 500ml;
(6) add 95% ethanol 2L to water extracting liquid, making containing the alcohol amount is 75%, fully stirs standing over night;
(7) filter, collecting precipitation, centrifugal or sucking filtration, will precipitate the reduced vacuum drying, obtain amorphous powder 50g, be the anemaran extract, and its polysaccharide weight content is 52%;
Embodiment 2:
The whole preparation technology of three kinds of chemical composition groups of the Rhizoma Anemarrhenae:
(1) get Rhizoma Anemarrhenae 1kg, clean, add 10% medical material weight distilled water moistening 12h, the moisture content complete wetting, cut sheet;
(2) Rhizoma Anemarrhenae sheet is extracted 2 times with 8 times of weight, 95% alcohol heating reflux, filter, merge extractive liquid,, decompression recycling ethanol, concentrated, obtain alcohol extraction concentrated solution 3.5L;
(3) alcohol extraction concentrated solution, use the 500ml macroporous adsorbing resin for purification, and with water and 75% ethanol elution, water elution liquid discards respectively, collect ethanol elution 2L, decompression recycling ethanol, be concentrated into thick paste, drying under reduced pressure, obtain extraced total timosaponin 18g, and its total saponins weight content is 60%;
(4) extraced total timosaponin 10g adding distil water 100ml dissolves, add diluted acid, heating hydrolysis generates aglycon, be that the molish reaction is negative, hydrolyzed solution is neutralized to neutrality with alkali, then by ethyl acetate, extracts aglycon, reclaim solvent, drying under reduced pressure, obtain anemarrhena total sapogenin extract 4.2g, and its total sapogenins weight content is greater than 90%;
(5) by residue drying after alcohol extraction, by 10 times of amount distilled water heating and refluxing extraction 3 times, filter, merging filtrate, concentrating under reduced pressure, obtain water extracting liquid 500ml;
(6) add 95% ethanol 3L to water extracting liquid, making containing the alcohol amount is 85%, fully stirs standing over night;
(7) filter, collecting precipitation, centrifugal or sucking filtration, will precipitate the reduced vacuum drying, obtain amorphous powder 55g, be the anemaran extract, and its polysaccharide weight content is 55%;
Embodiment 3:
Getting content is 50% anemaran 20g, add 30 times of amount distilled water stirring and dissolving, micromolecule monosaccharide and oligosaccharide are removed in the ultrafilter membrane bag ultrafiltration that is 5kDa with molecular cut off, ultrafiltration apparatus adopts the small-sized cross-flow ultrafiltration system of Mi Libo Labscale, inlet pressure 30psi, circulating pressure 15psi, when the trapped fluid residue is 50ml, add the equal-volume distill water dialysis 3 times, collect trapped fluid 50ml, add 95% ethanol 500ml, make to reach 85% containing the alcohol amount, standing over night, centrifugal, get the precipitation drying under reduced pressure and must make with extra care anemaran, polysaccharide total amount content is 95%.
Claims (2)
1. the preparation method of Rhizoma Anemarrhenae chemical composition group extract, it is characterized in that: the method comprises following step:
(1) Rhizoma Anemarrhenae is cleaned, added appropriate distilled water moistening 6 ~ 12h, cut sheet;
(2) Rhizoma Anemarrhenae sheet is extracted 2 times with 75 ~ 95% alcohol heating reflux, filter, merge extractive liquid,, decompression recycling ethanol, concentrated, obtain the alcohol extraction concentrated solution;
(3) the alcohol extraction concentrated solution, use macroporous adsorbing resin for purification, and with water and 75 ~ 95% ethanol elutions, water elution liquid discards respectively, merges ethanol elution, decompression recycling ethanol, and concentrated, drying under reduced pressure, obtain extraced total timosaponin, and its total saponins weight content is greater than 50%;
(4) the extraced total timosaponin adding distil water dissolves, and adds diluted acid, heating, and hydrolysis generates aglycon, hydrolyzed solution is neutralized to neutrality with alkali, then by chloroform or ethyl acetate, extracts aglycon, reclaims solvent, drying under reduced pressure, obtain the anemarrhena total sapogenin extract, and its total sapogenins weight content is greater than 80%;
(5) by residue drying after alcohol extraction, use distilled water heating and refluxing extraction 2 ~ 3 times, filter, merging filtrate, concentrating under reduced pressure, obtain water extracting liquid;
(6) add 95% ethanol to water extracting liquid, making containing the alcohol amount is 75 ~ 85%, fully stirs standing over night;
(7) filter, collecting precipitation, centrifugal or sucking filtration, will precipitate the reduced vacuum drying, obtain amorphous powder, be the anemaran extract, and its polysaccharide weight content is greater than 50%.
2. the preparation method of Rhizoma Anemarrhenae chemical composition group extract according to claim 1, it is characterized in that: the polyoses extract obtained in described step (7) is further removed to the small molecular weight impurities such as monosaccharide, oligosaccharide with macroporous adsorbent resin decolouring, ultra-filtration filters, obtain the extract of anemaran content more than 50 ~ 95%.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107619096A (en) * | 2017-10-19 | 2018-01-23 | 王婧宁 | Acid contaminant cleanser in paper waste |
| CN107753500A (en) * | 2017-11-03 | 2018-03-06 | 黑龙江中医药大学 | The Preparation method and use of oligosaccharide compositions in the wind-weed |
| CN107913347A (en) * | 2017-12-31 | 2018-04-17 | 山东禹泽医药科技有限公司 | A kind of compound grape-seed extract with antioxidation |
| CN111803400A (en) * | 2020-08-18 | 2020-10-23 | 黑龙江中医药大学 | Traditional Chinese medicine polysaccharide moisturizing and freckle removing mask and preparation method thereof |
| CN112876577A (en) * | 2021-03-18 | 2021-06-01 | 华南理工大学 | Homogeneous rhizoma anemarrhenae polysaccharide and preparation method and application thereof |
| CN115572318A (en) * | 2022-10-23 | 2023-01-06 | 爱生泽(上海)生物科技有限公司 | Preparation method of anemarrhena oligosaccharide and application of anemarrhena oligosaccharide in cosmetics |
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| CN1732955A (en) * | 2004-08-03 | 2006-02-15 | 山东绿叶天然药物研究开发有限公司 | Pharmaceutical composition making anemarrhena total sapogenin as active ingredient, its preparation method and use |
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| CN101229316A (en) * | 2008-01-31 | 2008-07-30 | 广东药学院 | Rhizoma anemarrhenae extrac and applications as type 2 diabetes-curing medicine thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107619096A (en) * | 2017-10-19 | 2018-01-23 | 王婧宁 | Acid contaminant cleanser in paper waste |
| CN107753500A (en) * | 2017-11-03 | 2018-03-06 | 黑龙江中医药大学 | The Preparation method and use of oligosaccharide compositions in the wind-weed |
| CN107913347A (en) * | 2017-12-31 | 2018-04-17 | 山东禹泽医药科技有限公司 | A kind of compound grape-seed extract with antioxidation |
| CN111803400A (en) * | 2020-08-18 | 2020-10-23 | 黑龙江中医药大学 | Traditional Chinese medicine polysaccharide moisturizing and freckle removing mask and preparation method thereof |
| CN112876577A (en) * | 2021-03-18 | 2021-06-01 | 华南理工大学 | Homogeneous rhizoma anemarrhenae polysaccharide and preparation method and application thereof |
| CN112876577B (en) * | 2021-03-18 | 2022-02-22 | 华南理工大学 | Homogeneous rhizoma anemarrhenae polysaccharide and preparation method and application thereof |
| CN115572318A (en) * | 2022-10-23 | 2023-01-06 | 爱生泽(上海)生物科技有限公司 | Preparation method of anemarrhena oligosaccharide and application of anemarrhena oligosaccharide in cosmetics |
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Application publication date: 20140101 |