CN103224491A - Method for extracting high-purity puerarin by using water as solvent - Google Patents
Method for extracting high-purity puerarin by using water as solvent Download PDFInfo
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- CN103224491A CN103224491A CN201310192332XA CN201310192332A CN103224491A CN 103224491 A CN103224491 A CN 103224491A CN 201310192332X A CN201310192332X A CN 201310192332XA CN 201310192332 A CN201310192332 A CN 201310192332A CN 103224491 A CN103224491 A CN 103224491A
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Abstract
The invention relates to a method for extracting high-purity puerarin by using water as solvent, which comprises the following steps: extracting by using water as solvent, performing adsorption elution on the obtained pueraria total flavone extractum through an HPD-600 macroporous resin, performing adsorption elution through an AB-8 type macroporous adsorbent resin column, decolorizing through an aluminum oxide column, concentrating under reduced pressure, and drying to obtain a crude product; and adding chitosan into the crude product, and performing repeated crystallization to precipitate, thus obtaining puerarin of which the purity is more than 99%. According to the invention, puerarin is extracted by using water instead of organic solvent as solvent, thus obtaining the high-purity puerarin. The invention solves the organic residue problem and reduces the environmental pollution. Besides, the procedures are safe, and are reasonable, simple and direct in conjugation; and the method is easy to popularize.
Description
Technical field
Extract preparing technical field in the invention belongs to approximately, especially a kind of is the method that solvent extracts high purity puerarin with water.
Background technology
The root of kudzu vine (Radix puerariae) is the dry root of legume pueraria lobata Pueraria lobata (Wiolld) Ohwi, its flavor is sweet, hot, property flat, its main component is a starch, contain 12% the flavonoid compound of having an appointment in addition, comprise kind surplus soybean (soya bean) glucoside, daidzein, the puerarin etc. 10; And contain daucosterol, amino acid, coumarins etc.Be Chinese medicinal materials be again nutritious edible raw material.
The root of kudzu vine has functions such as spasmolysis is brought down a fever, promoted the production of body fluid, promoting eruption, the positive antidiarrheal of liter.Similar with other most of flavonoid compounds, the Radix Puerariae flavone compounds also has multiple pharmacological function, as improves blood circulation, hypotensive, hypoglycemic, reducing blood-fat, inhibition arteriosclerosis, anti-heart disorder, platelet aggregation-against, antitumor, anti-hypoxia and anti-oxidant etc.Puerarin is to extract a kind of isoflavonoid that obtains from the root of kudzu vine, is a kind of in the Radix Puerariae total flavones.Experimental results show that it has the expansion cardiovascular and cerebrovascular, reduce myocardium keto consumption, improve myocardium shrinkage function and promote the blood microcirculation effect, can be used for treating microcirculation disturbance diseases such as coronary heart disease, retina artery and vein obstruction and sudden deafness.Oneself is widely used in fields such as medicine industry, foodstuffs industry, daily-use chemical industry because of its significant pharmaceutical use for Radix Puerariae flavone and puerarin now.
In recent years, characteristics such as the natural phant effective ingredient is obvious because of its effect, natural low toxicity gain great popularity, and have caused worldwide and have used the natural herb plant to prevent and treat the upsurge of various diseases.Along with carrying out in a deep going way to natural plant crude drugs research, the research range of the root of kudzu vine has had further expansion, wherein the research of extraction of Radix Puerariae flavone and puerarin and purifying has been subjected to extensive concern, the main method of the extraction of Radix Puerariae total flavones has at present: (1) alcohol reflux method, mainly with solvents such as water, ethanol, alkaline alcohol, liming, methyl alcohol, acetone, reflux.Refluxing extraction 2～3 times is extracted Radix Puerariae total flavones; (2) alcohol percolation method; (3) pickling process; (4) microwave auxiliary extraction method; (5) enzymolysis circumfluence method; (6) ultrasonic counter-current extraction; (7) ion coordination extraction process.
Market is increasing to the demand of Radix Puerariae flavone.But because the deficiency of input in science and technology, domestic Radix Puerariae flavone preparation technique is backward relatively, and the extracting method of Radix Puerariae flavone and puerarin mostly is organic solvent extraction, and production efficiency is low, energy consumption is big, environmental pollution is serious, foreign matter content is high, and product lacks the market competitiveness.Doing solvent with water to replace organic solvent carries out high-purity extraction to Radix Puerariae flavone and puerarin and has solved organic residue problem.
Find two pieces of patent documentations related to the present invention by retrieval, one is Puerarin and its extraction method (CN1163127), mainly may further comprise the steps: (1) root of kudzu vine is pulverized, and decocting boils; (2) concentrate aqueous extract; (3) ethanol sedimentation gets pure medicinal extract; (4) polyamide column chromatography; (5) water elution concentrates; (6) place crystallization and get crude product; (7) refining.It two is production methods (CN1927876) of puerarin extract, mainly may further comprise the steps: (1) root of kudzu vine is pulverized decocting and is boiled; (2) resinbed is analysed; (3) macroporous resin chromatography; Above-mentioned patent documentation is the technical improvement at the puerarin purifying, but with the technical scheme of present patent application in essence different is arranged.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art part, providing a kind of is the method that solvent extracts high purity puerarin with water.
The objective of the invention is to be achieved through the following technical solutions:
(1) puerarin extracts: exsiccant root of kudzu vine phloem is ground into meal mixes with water, and in 1.5MPa, 60 ℃ of hot dipping 10h.Filter filtrate for later use.Adding waits water gaging in filter residue again, and hot dipping 15h under uniform temp and the pressure condition filters 3 times repeatedly.At vacuum tightness＜0.1MPa, filtrate is concentrated to more than 10% under 45～60 ℃ and can obtains Radix Puerariae total flavones medicinal extract, effective component extraction rate reaches more than 90%;
(2) puerarin purifying: the Radix Puerariae total flavones medicinal extract that obtains through the HPD-600 macroporous resin adsorb, wash-out.Use water-soluble impurities such as distilled water flush away carbohydrate, protein, tannin during wash-out earlier, use 60% ethanol elution then instead, elutriant concentrates and reclaims ethanol, and the medicinal extract that obtains is mixed with water-soluble liquid and adsorbs through AB-8 type macroporous adsorption resin chromatography post, uses 50% ethanol elution.Collect elutriant and concentrate recovery ethanol.
(3) puerarin decolouring: elutriant is through the decolouring of aluminium sesquioxide post, and again through being evaporated to 50% of former elutriant, concentrated solution leaves standstill after 24h separates out, suction filtration dry raw product.
(4) puerarin is refining: raw product adds chitosan periodic crystallisation precipitation, and the filtrate concentrate drying obtains purity greater than 99% puerarin.
And the mass ratio of middle root of kudzu vine phloem meal of described step (1) and water is 1g: 8mL;
And the condition of HPD-600 macroporous resin is in the described step (2): blade diameter length ratio is 1: 6, last sample concentration 50mg/mL, and maximum applied sample amount is 3BV, flow velocity is 1mL/min, eluent consumption 5BV;
And the condition of AB-8 type macroporous adsorption resin chromatography post is in the described step (2): blade diameter length ratio is 1: 5, and last sample concentration is 15mg/mL, and maximum applied sample amount is 2.5BV, and flow velocity is 3BV/h, eluent consumption 2.5BV;
And the method that raw product periodic crystallisation precipitation is adopted in the described step (4) is the solution that raw product is mixed with 0.1g/mL, add 1% chitosan acetate dissolution liquid in 1: 1 ratio,, leave standstill 2h then in 40 ℃ of stirring 15min, filter, repeat as stated above 3 times.
Advantage of the present invention and positively effect are:
The present invention is solvent with water, extracts to obtain high purity puerarin.This method water replaces in the past organic solvent to do solvent, has reduced organic residually and to the pollution of environment, has reduced production cost, has improved working efficiency.Operation safety, be connected rationally simple and direct, be easy to promote.
Embodiment
Below in conjunction with embodiment, the present invention is further described, and following embodiment is illustrative, is not determinate, can not limit protection scope of the present invention with following embodiment.
Specific examples of the present invention:
1,500g exsiccant root of kudzu vine phloem is ground into meal and mixes with the distilled water of 4L, in 1.5MPa, and 60 ℃ of hot dipping 10h.Filter filtrate for later use.Adding waits water gaging in filter residue again, and hot dipping 15h under uniform temp and the pressure condition filters 3 times repeatedly.At vacuum tightness＜0.1MPa, filtrate is concentrated to more than 10% under 45～60 ℃ and can obtains Radix Puerariae total flavones medicinal extract, effective component extraction rate reaches more than 90%;
2, the Radix Puerariae total flavones medicinal extract that obtains is mixed with the solution of 50mg/mL, through the HPD-600 macroporous resin adsorb, wash-out.HPD-600 macroporous resin blade diameter length ratio is 1: 6, and maximum applied sample amount is 3BV, and flow velocity is 1mL/min, eluent consumption 5BV.Earlier with water-soluble impurities such as distilled water flush away carbohydrate, protein, tannins, use 60% ethanol elution then instead during wash-out, elutriant concentrates and reclaims ethanol.The medicinal extract that obtains is mixed with water-soluble liquid and adsorbs through AB-8 type macroporous adsorption resin chromatography post, uses 50% ethanol elution.Blade diameter length ratio is 1: 5, and last sample concentration is 15mg/mL, and maximum applied sample amount is 2.5BV, and flow velocity is 3BV/h, and eluent consumption 2.5BV collects elutriant and concentrates recovery ethanol.
3, elutriant is through aluminium sesquioxide post decolouring, and again through being evaporated to 50% of former elutriant, concentrated solution leaves standstill after 24h separates out, suction filtration dry raw product.
4, raw product is mixed with the solution of 0.1g/mL, adds 1% chitosan acetate dissolution liquid in 1: 1 ratio, stir 15min in 40 ℃, leave standstill 2h then, filter, repeat as stated above 3 times, the filtrate concentrate drying obtains purity greater than 99% puerarin.
Claims (5)
1. one kind is the method that solvent extracts high purity puerarin with water, it is characterized in that:
Step is:
(1) puerarin extracts: exsiccant root of kudzu vine phloem is ground into meal mixes with water, and in 1.5MPa, 60 ℃ of hot dipping 10h.Filter filtrate for later use.Adding waits water gaging in filter residue again, and hot dipping 15h under uniform temp and the pressure condition filters 3 times repeatedly.At vacuum tightness＜0.1MPa, filtrate is concentrated to more than 10% under 45～60 ℃ and can obtains Radix Puerariae total flavones medicinal extract, effective component extraction rate reaches more than 90%;
(2) puerarin purifying: the Radix Puerariae total flavones medicinal extract that obtains is through the capable absorption of HPD-600, wash-out.Use water-soluble impurities such as distilled water flush away carbohydrate, protein, tannin during wash-out earlier, use 60% ethanol elution then instead, elutriant is concentrated and reclaim ethanol, and the medicinal extract that obtains is mixed with water-soluble liquid and adsorbs through AB-8 type macroporous adsorption resin chromatography post, uses 50% ethanol elution.Collect elutriant and concentrate and reclaim ethanol.
(3) puerarin decolouring: elutriant is through the decolouring of aluminium sesquioxide post, and again through being evaporated to 50% of former elutriant, concentrated solution leaves standstill after the 24h crystal separates out, suction filtration dry raw product.
(4) puerarin is refining: raw product adds chitosan periodic crystallisation precipitation, and the filtrate concentrate drying obtains purity greater than 99% puerarin.
2. according to claim 1 is the method that solvent extracts high purity puerarin with water, it is characterized in that: the mass ratio of root of kudzu vine phloem meal and water is 1g: 8mL in the described step (1).
3. according to claim 1 is the method that solvent extracts high purity puerarin with water, it is characterized in that: the condition of HPD-600 macroporous resin is in the described step (2): blade diameter length ratio is 1: 6, last sample concentration 50mg/mL, and maximum applied sample amount is 3BV, flow velocity is 1mL/min, eluent consumption 5BV.
4. according to claim 1 is the method that solvent extracts high purity puerarin with water, it is characterized in that: the condition of AB-8 type macroporous adsorption resin chromatography post is in the described step (2): blade diameter length ratio is 1: 5, last sample concentration is 15mg/mL, maximum applied sample amount is 2.5BV, flow velocity is 3BV/h, eluent consumption 2.5BV.
5. according to claim 1 is the method that solvent extracts high purity puerarin with water, it is characterized in that: the method that raw product periodic crystallisation precipitation is adopted in the described step (4) is the solution that raw product is mixed with 0.1g/mL, add 1% chitosan acetate dissolution liquid in 1: 1 ratio, stir 15min in 40 ℃, leave standstill 2h then, filter, repeat as stated above 3 times.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103864767A (en) * | 2014-03-26 | 2014-06-18 | 南阳理工学院 | Puerarin refining process |
| CN106924307A (en) * | 2015-12-30 | 2017-07-07 | 姚萍 | Application of the radix bupleuri in the medicine for preparing treatment virus B hepatitis |
| CN108610335A (en) * | 2016-12-13 | 2018-10-02 | 丹阳市香逸林果专业合作社 | A kind of extraction process of Puerarin |
| CN109456313A (en) * | 2018-11-05 | 2019-03-12 | 云南省农业科学院药用植物研究所 | A method of extracting the active Puerarin of high anti-oxidation from Pachyrhizua angulatus |
| CN110938066A (en) * | 2019-12-13 | 2020-03-31 | 宿迁旺葛农业科技开发有限公司 | Puerarin extraction method |
| CN111217787A (en) * | 2020-03-25 | 2020-06-02 | 陕西嘉禾药业有限公司 | Method for purifying daidzein in radix Puerariae |
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| CN1398872A (en) * | 2002-08-29 | 2003-02-26 | 中国科学院昆明植物研究所 | Puerarin preparing process |
| CN1524867A (en) * | 2003-02-27 | 2004-09-01 | 上海中医药大学 | Method for extracting kudzuvine root total flavone |
| CN101550133A (en) * | 2009-05-13 | 2009-10-07 | 南阳市海达生物技术有限公司 | Method for extracting puerarin and usage of kudzu vine root for preparing medicament protecting liver |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103864767A (en) * | 2014-03-26 | 2014-06-18 | 南阳理工学院 | Puerarin refining process |
| CN106924307A (en) * | 2015-12-30 | 2017-07-07 | 姚萍 | Application of the radix bupleuri in the medicine for preparing treatment virus B hepatitis |
| CN108610335A (en) * | 2016-12-13 | 2018-10-02 | 丹阳市香逸林果专业合作社 | A kind of extraction process of Puerarin |
| CN109456313A (en) * | 2018-11-05 | 2019-03-12 | 云南省农业科学院药用植物研究所 | A method of extracting the active Puerarin of high anti-oxidation from Pachyrhizua angulatus |
| CN110938066A (en) * | 2019-12-13 | 2020-03-31 | 宿迁旺葛农业科技开发有限公司 | Puerarin extraction method |
| CN111217787A (en) * | 2020-03-25 | 2020-06-02 | 陕西嘉禾药业有限公司 | Method for purifying daidzein in radix Puerariae |
| CN111217787B (en) * | 2020-03-25 | 2022-11-29 | 陕西嘉禾药业有限公司 | Method for purifying daidzein in radix Puerariae |
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Application publication date: 20130731 |