CN1272331C - Method of extracting effective components in kudzu vine root - Google Patents
Method of extracting effective components in kudzu vine root Download PDFInfo
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- CN1272331C CN1272331C CN 02155132 CN02155132A CN1272331C CN 1272331 C CN1272331 C CN 1272331C CN 02155132 CN02155132 CN 02155132 CN 02155132 A CN02155132 A CN 02155132A CN 1272331 C CN1272331 C CN 1272331C
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Abstract
The present invention relates to a method of extracting effective components from kudzu roots. The existing method of extracting the effective components of kudzu roots can only extract one kind of the effective components of kudzu roots and can not extract and separate two kinds of effective components including daidzin and daidzein simultaneously, which reduces the utility value of the kudzu roots and results in the waste of traditional Chinese medicinal material resources. The present invention is characterized in that during the separation of the effective components, adopted adsorptive resin is S-8 resin which is used to adsorb the effective components of concentrated extractive and is put in a chromatographic column for elution with ethanol or methanol of 30 to 50 %, 50 to 80 % and 80 to 100 % in concentration orderly, and eluted solution is collected respectively. During the post processing of the effective components, the three kinds of eluted solution are respectively concentrated, crystallized and dried. The present invention can extract and separate three kinds of effective components simultaneously, improve the utilization value of the kudzu roots and make full use of the traditional Chinese medicinal material resources.
Description
Technical field
The present invention relates to a kind of from the root of kudzu vine method of extracting effective components.
Background technology
The root of kudzu vine is a kind of traditional Chinese medicine, contain many kinds of effective constituents, wherein based on puerarin, daidzin, daidzein, puerarin has special effect at aspects such as treatment cardiovascular disorder, stenocardia, daidzin and daidzein are treating and are preventing aspect the symptoms such as female diseases such as mammary cancer, osteoporosis, hot flush special role is arranged, in present medical research, daidzin, daidzein and puerarin have all obtained attention.In the method for existing extraction kudzu vine root, water extract-alcohol precipitation method of purification, polyamide column chromatography method of purification, water extraction method, kudzuvine root starch processing waste water resin isolation method etc. are arranged.These methods all are only to extract a kind of effective constituent of puerarin, and the while extraction separation does not go out daidzin and these two kinds of effective constituents of daidzein, thereby make daidzin and daidzein in the root of kudzu vine not obtain utilizing, influenced the economic benefit of extracting the root of kudzu vine, reduce the utility value of the root of kudzu vine self, caused the waste of Chinese material medicine resource.
Summary of the invention
Technical problem to be solved by this invention is the defective that overcomes above-mentioned prior art, a kind of method that can extract three kinds of effective constituents simultaneously from the root of kudzu vine is provided, effective constituent in the root of kudzu vine is fully extracted, improved the utility value of the root of kudzu vine self, make full use of Chinese material medicine resource.
Technical scheme of the present invention is such: a kind of method of extracting three kinds of effective constituents in the root of kudzu vine, comprise extracts active ingredients, separation and aftertreatment, it is characterized in that in the sepn process of effective constituent, its polymeric adsorbent that adopts is the S-8 resin, with the effective constituent in the S-8 resin absorption extract concentrated solution, this resin is packed in the chromatography column, be that the ethanol of 30-50%, 50-80%, 80-100% or methanol-eluted fractions are contained in the resin in the chromatography column with concentration successively, collect the solution that above-mentioned wash-out comes out respectively; The aftertreatment of effective constituent be to three kinds of solution that above-mentioned wash-out obtains concentrate respectively, crystallization, drying treatment.Described S-8 resin is the commercial goods, it can adsorb three kinds of effective constituents, be puerarin, daidzin and daidzein, with concentration is to contain the puerarin composition in the ethanol of 30-50% or the solution that methanol-eluted fractions is come out, with concentration is to contain the daidzin composition in the ethanol of 50-80% or the solution that methanol-eluted fractions is come out, is to contain the daidzein composition in the ethanol of 80-100% or the solution that methanol-eluted fractions is come out with concentration.This method of three kinds of effective constituents of extraction separation simultaneously, it is fully extracted the effective constituent in the root of kudzu vine, has improved the utility value of the root of kudzu vine self, makes full use of Chinese material medicine resource.
Described a kind of method of extracting three kinds of effective constituents in the root of kudzu vine, the extraction step of effective constituent is: adopt the bright root of kudzu vine, powder of Radix Puerariae, kudzu, FI puerariae is a raw material, through oven drying at low temperature and pulverization process, the granularity of material is controlled at the 10-40 order, material is packed in the extractor, in material (gram): solvent (milliliter)=1: ratio (8-12) adds solvent, at 30-60 ℃ of following lixiviate 4-12 hour, filter, add inventory 5-7 solvent lixiviate doubly 3-9 hour in the filter residue, filter, merge filtrate twice, concentrate under the cryogenic vacuum condition, get extract concentrated solution, above-mentioned solvent is ethanol or the methyl alcohol of 20-80%.
Described a kind of method of extracting three kinds of effective constituents in the root of kudzu vine, polymeric adsorbent S-8 will pass through pre-treatment, pretreated process is that resin soaked respectively 40,3,5 hours with distilled water, 2% sodium hydroxide, 2% hydrochloric acid successively, be washed to neutrality, till being washed till effluent liquid and adding water and white opacity do not occur with dehydrated alcohol again, till being washed till effluent liquid and not having alcohol with distilled water at last.
Described a kind of method of extracting three kinds of effective constituents in the root of kudzu vine, during effective constituent in S-8 resin absorption extract concentrated solution, can adopt dynamic or static treatment, dynamichandling is: the S-8 polymeric adsorbent is packed in the chromatography column, then extract concentrated solution is passed through chromatography column continuously with certain flow velocity; Static treatment is: the S-8 polymeric adsorbent is dropped in the extract concentrated solution, soaks after 3-24 hour, separation polymeric adsorbent and solution are packed polymeric adsorbent in the chromatography column into.
Described a kind of method of extracting three kinds of effective constituents in the root of kudzu vine, the concentrated condition that three kinds of effective constituents that ethanol or methanol-eluted fractions are obtained are carried out: temperature is 40-70 ℃, vacuum tightness≤1 * 10
4Pa; Crystallization condition: with solvent ether and alcoholic acid volume ratio is to dissolve three kinds of concentrated solutions of gained in 1: 3,1: 2 and 1: 1 respectively, and corresponding puerarin, daidzin and three kinds of concentrated solutions of daidzein respectively are≤10 ℃ of following crystallizations; Drying conditions: temperature≤-40 ℃, vacuum tightness≤50Pa.
S-8 polymeric adsorbent of the present invention, can be with three kinds of effective constituent absorption in the root of kudzu vine, thereby energy is three kinds of effective constituents of extraction separation simultaneously, effective constituent in the root of kudzu vine is fully extracted, improved the utility value of the root of kudzu vine self, made full use of Chinese material medicine resource, improved and extract the economic benefit that the root of kudzu vine can bring.
Embodiment
Embodiment 1
Polymeric adsorbent is S-8, its pre-treatment is: resin was used distilled water, 2% sodium hydroxide, 2% salt acid soak 40,3,5 hours successively, be washed to neutrality, till being washed till effluent liquid and adding water and white opacity do not occur with dehydrated alcohol again, till being washed till effluent liquid and not having alcohol with distilled water at last.
Get the bright root of kudzu vine,, cross 20 mesh sieves through oven drying at low temperature and pulverizing.Take by weighing the root of kudzu vine material 1K g of pulverizing, in the extractor of packing into, add 10L80% ethanol, 50 ℃ of following lixiviates 10 hours.Use strainer filtering, add the lixiviate once more of 6L80% ethanol in the filter residue, merge twice extracting solution, be concentrated into 2L with the cryogenic vacuum concentrating instrument.
Take by weighing 100g S-8 resin, pack in the chromatography column, pass through resin column with concentrating the 2L concentrated solution that obtains, use 30% ethanol elution then, collection can obtain the elutriant of puerarin composition, the ethanol elution with 60%, and collection can obtain the elutriant of daidzin composition, with 90% edible ethanol wash-out, collection can obtain the elutriant of daidzein composition.Three kinds of elutriants that will contain puerarin, daidzin and daidzein concentrate respectively, crystallization, drying treatment, and the temperature when concentrating is 45 ℃, and vacuum tightness is 1 * 10
4Pa; Crystallization condition: with solvent ether and alcoholic acid volume ratio is to dissolve three kinds of concentrated solutions of gained in 1: 3,1: 2 and 1: 1 respectively, and corresponding puerarin, daidzin and three kinds of concentrated solutions of daidzein respectively are 10 ℃ of following crystallizations; Drying conditions: be lyophilize, temperature is-45 ℃, and vacuum tightness is 50Pa, just can obtain puerarin, daidzin and three kinds of pure product of isoflavones of daidzein, and wherein the puerarin yield is 1.0%, and purity is 98.1%; The daidzin yield is 0.6%, and purity is 90.7%; The daidzein yield is 0.2%, and purity is 97.2%.
Embodiment 2
Polymeric adsorbent is S-8, and its preprocessing process is identical with embodiment 1.
Get bright kudzu,, cross 20 mesh sieves through oven drying at low temperature and pulverizing.Take by weighing the kudzu material 1Kg of pulverizing, in the extractor of packing into, add 12L40% methyl alcohol, 50 ℃ of following lixiviates 10 hours.Use strainer filtering, add the lixiviate once more of 5L40% methyl alcohol in the filter residue, merge twice extracting solution, be concentrated into 2L with the cryogenic vacuum concentrating instrument.
Take by weighing 100g S-8 resin, drop in the 2L concentrated solution and soaked 24 hours, separate polymeric adsorbent and solution, polymeric adsorbent is packed in the chromatography column, use 25% methanol-eluted fractions then, collection can obtain the elutriant of puerarin composition, methanol-eluted fractions with 65%, collection can obtain the elutriant of daidzin composition, the methanol-eluted fractions with 100%, and collection can obtain the elutriant of daidzein composition.Three kinds of elutriants that will contain puerarin, daidzin and daidzein concentrate respectively, crystallization, drying treatment, and the temperature when concentrating is 60 ℃, and vacuum tightness is 5 * 10
3Pa; Crystallization: with solvent ether and alcoholic acid volume ratio is to dissolve three kinds of concentrated solutions of gained in 1: 3,1: 2 and 1: 1 respectively, and corresponding puerarin, daidzin and three kinds of concentrated solutions of daidzein respectively are 5 ℃ of following crystallizations; Drying is lyophilize, and temperature is-40 ℃, and vacuum tightness is 20Pa.Just can obtain puerarin, daidzin and three kinds of pure product of isoflavones of daidzein, wherein the puerarin yield is 0.6%, and purity is 97.3%; The daidzin yield is 0.1%, and purity is 92.7%; The daidzein yield is 0.07%, and purity is 95.2%.
Claims (6)
1, a kind of method of extracting three kinds of effective constituents in the root of kudzu vine, comprise extracts active ingredients, separation and aftertreatment, it is characterized in that in the sepn process of effective constituent, its polymeric adsorbent that adopts is the S-8 resin, with the effective constituent in the S-8 resin absorption extract concentrated solution, be that the ethanol of 30-50%, 50-80%, 80-100% or methanol-eluted fractions are contained in the resin in the chromatography column with concentration successively then, one by one corresponding to wash-out puerarin, daidzin, these three kinds of effective constituents of daidzein, and collect the solution that above-mentioned wash-out comes out respectively; The aftertreatment of effective constituent be to three kinds of solution that above-mentioned wash-out obtains concentrate respectively, crystallization, drying treatment.
2, a kind of method of extracting three kinds of effective constituents in the root of kudzu vine according to claim 1, it is characterized in that when the effective constituent of S-8 resin absorption extract concentrated solution, adopt dynamic or static treatment, dynamichandling is: the S-8 polymeric adsorbent is packed in the chromatography column, then extract concentrated solution is passed through chromatography column continuously; Static treatment is: the S-8 polymeric adsorbent is dropped in the extract concentrated solution, soaks after 3-24 hour, separation polymeric adsorbent and solution are packed polymeric adsorbent in the chromatography column into.
3, a kind of method of extracting three kinds of effective constituents in the root of kudzu vine according to claim 1 and 2, the extraction step that it is characterized in that effective constituent is: adopt the bright root of kudzu vine, powder of Radix Puerariae, kudzu, FI puerariae is a raw material, through oven drying at low temperature and pulverization process, the granularity of material is controlled at the 10-40 order, material is packed in the extractor, in material (gram): solvent (milliliter)=1: ratio (8-12) adds solvent, at 30-60 ℃ of following lixiviate 4-12 hour, filter, add inventory 5-7 solvent lixiviate doubly 3-9 hour in the filter residue, filter, merge filtrate twice, under the cryogenic vacuum condition, concentrate, get extract concentrated solution.
4, a kind of method of extracting three kinds of effective constituents in the root of kudzu vine according to claim 3 is characterized in that described solvent is ethanol or the methyl alcohol of 20-80%.
5, a kind of method of extracting three kinds of effective constituents in the root of kudzu vine according to claim 1, it is characterized in that described S-8 polymeric adsorbent will pass through pre-treatment, pretreated process is that resin soaked respectively 40,3,5 hours with distilled water, 2% sodium hydroxide, 2% hydrochloric acid successively, be washed to neutrality, till being washed till effluent liquid and adding water and white opacity do not occur with dehydrated alcohol again, till being washed till effluent liquid and not having alcohol with distilled water at last.
6, a kind of method of extracting three kinds of effective constituents in the root of kudzu vine according to claim 1, it is characterized in that described concentrated condition: temperature is 40-70 ℃, vacuum tightness≤1 * 10
4Pa; Crystallization condition: with solvent ether and alcoholic acid volume ratio is to dissolve three kinds of concentrated solutions of gained respectively in 1: 3,1: 2 and 1: 1 ,≤10 ℃ of following crystallizations; Drying conditions: temperature≤-40 ℃, vacuum tightness≤50Pa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02155132 CN1272331C (en) | 2002-12-10 | 2002-12-10 | Method of extracting effective components in kudzu vine root |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 02155132 CN1272331C (en) | 2002-12-10 | 2002-12-10 | Method of extracting effective components in kudzu vine root |
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| CN1506360A CN1506360A (en) | 2004-06-23 |
| CN1272331C true CN1272331C (en) | 2006-08-30 |
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| CN 02155132 Expired - Fee Related CN1272331C (en) | 2002-12-10 | 2002-12-10 | Method of extracting effective components in kudzu vine root |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1305888C (en) * | 2005-05-09 | 2007-03-21 | 何照范 | Method for producing puerarin in high purity and aglycon of soybean jointly |
| CN100387590C (en) * | 2006-08-23 | 2008-05-14 | 浙江大学 | Method of extracting, separating soybean aglucone from kudzu |
| CN101318955B (en) * | 2007-06-08 | 2010-12-22 | 中国科学院大连化学物理研究所 | Method for preparing effective component of kudzu root |
| CN103131578B (en) * | 2011-11-29 | 2016-04-27 | 中润益源(北京)生物科技有限公司 | A kind of scheme of root of kudzu vine comprehensive processing and utilization |
| CN105218533B (en) * | 2015-10-13 | 2018-01-30 | 江西农业大学 | A kind of method for isolating and purifying Puerarin and daidzein simultaneously from the root of kudzu vine |
| CN108144031A (en) * | 2018-02-08 | 2018-06-12 | 江西斯普瑞营养品有限公司 | A kind of Chinese medicine composition and its preparation process with prophylactic treatment breast disease and breast health-care effect |
| CN108640957B (en) * | 2018-06-28 | 2021-07-06 | 湖南华诚生物资源股份有限公司 | Method for simultaneously extracting various pueraria isoflavone glycosides from pueraria crude extract |
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