CN1129700A - Extraction and application of Lobed Kudzuvine - Google Patents

Extraction and application of Lobed Kudzuvine Download PDF

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Publication number
CN1129700A
CN1129700A CN 95110343 CN95110343A CN1129700A CN 1129700 A CN1129700 A CN 1129700A CN 95110343 CN95110343 CN 95110343 CN 95110343 A CN95110343 A CN 95110343A CN 1129700 A CN1129700 A CN 1129700A
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puerarin
crystallization
crude product
ethanol
polymeric amide
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CN 95110343
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CN1057093C (en
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赵爱平
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赵爱平
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Abstract

The process for extracting puerarin (C20H21O9) in the form of white crystal from pueraria as Chinese medicinal herbs includes such steps as aqueous extraction, alcohol deposition, chromatographic analysis with polyamide column, eluting in water, concentration, laying aside to educe crude puerarin, chromatographic analysis with polyamide column, eduting in water, concentration, crystallization, freeze or spray drying or repeated crystallization with 70-80% alcohol to obtain refined puerarin. It features no environmental pollution, high content of puerarin up to over 90% and low cost.

Description

Puerarin and its extraction method and purposes
The present invention is a herbal medicine effective ingredient extract, particularly be from the herbal medicine root of kudzu vine, to extract to prevent and treat cardiovascular disorder, again cerebrovascular disease is had the puerarin (C of obvious curative effects simultaneously 20H 21O 9) and preparation method thereof.
The root of kudzu vine has been prevented and cured diseases the existing long history of Herba indigoferae Pseudotinctoriae in the proved recipe as herbal medicine, extracts the process that the research work our province of effective constituent wherein also has more than ten years.At present content of puerarin can only be reached for about 70% (HPLC methods) in its bulk drug of puerarin injection of listing, its preparation technology mainly be with reference to Japanese bavin field hold two and side's departure (the bavin field is held second-class: the chemical research of the research of oriental drug composition (first reports) root of kudzu vine composition; Pharmaceutical journal 1959 79:755; Fang Qicheng etc.: the research of Radix Puerariae flavone, Chinese Medical Journal 1974 54:271) method promptly uses ethanol extract with propyl carbinol-water liquid-liquid extraction, aluminum oxide decolouring, Glacial acetic acid crystallization.The organic solvent that this technology is inflammable because of a large amount of uses, toxicity is big has caused the environmental pollution of production and the infringement of workers ' health, and the cost height, production cycle is long, and content of puerarin is low in the product, and it is clean that the acetic acid that uses in the crystallisation process is difficult to volatilization, make the impure height of its extract, drug effect is low.
Application number is that the effective constituent that mainly contains that 91110602.2 " kudzu vine root extract and preparation method and purposes " extracted is an isoflavones in the patent documentation, its technology be the raw material root of kudzu vine decoctions-filtrations-concentrate-wine is sunk-De magma-magma is diluted or spraying drying makes effective ingredient extracting solution (or powder).Its purpose is also to have the low problem of effective component content for people provide a kind of medicine that can be used as anti-cancer.
The objective of the invention is to for people provide a kind of medicine that can be used as control, the cerebrovascular, multiple disease such as cardiovascular, and puerarin content is more than 90%, effective, have no side effect and cost low, free of contamination Puerarin and its extraction method.
The objective of the invention is to be achieved through the following technical solutions:
Puerarin of the present invention is a kind of natural compounds in the herbal medicine root of kudzu vine, and the middle crude product of extraction is nontoxic liquid, medicinal extract or the rough crystal of brown xanchromatic, gets white crystals elaboration, puerarin (C after repeating crystallization for several times 20H 21O 9) content is more than 90%.
The technical process of the extracting method of puerarin is: earlier with the raw material root of kudzu vine pulverizings-decocting-concentrate placement-Jia ethanol sedimentation-pure medicinal extract-can make puerarin crystallization elaboration by polyamide column chromatography-water elution-concentrate-separate out puerarin crystallization-again through lyophilize or spraying drying or with 70-80% ethanol repetition crystallization through polyamide column chromatography-water elution-concentrate-place-separate out puerarin crude product-once more.
The extracting method step of puerarin of the present invention is poly-as follows:
1. at first meal is mixed, cleans, is ground into to root of kudzu vine raw material clearly;
2. root of kudzu vine meal water is decocted 2-4 time, decocting time is 0.5-2 hour, then after filtration, concentrate and make thick paste;
3. thick paste adds ethanol, makes to contain alcohol amount and reach 70-85%, and reheat is little to boil, and stirs, places, filters, reclaims ethanol, root of kudzu vine alcohol medicinal extract;
4. with polyamide granules absorption root of kudzu vine alcohol medicinal extract, make it half-dried after, dry column-packing, its chromatography polymeric amide is the 14-30 order, the make a living 1/10-1/5 of dose of its consumption, the post blade diameter length ratio is 1: 2-7; The water wash-out, the control flow velocity, the Fractional Collections elutriant concentrates and places crystallization respectively, gets pale brown look puerarin crude product;
5. the process for purification of puerarin crude product is: after the raw product drying, use the small amount of ethanol heating for dissolving, adsorb with Silon again, behind the volatilization ethanol, be added to the polymeric amide chromatography post upper end of wet method dress post again, polymeric amide is the 60-200 order, and the post blade diameter length ratio is 1: 3-7, and crude product and polymeric amide amount ratio are 1: 3-5; The water wash-out, the Fractional Collections elutriant concentrates respectively and the placement crystallization, and the part of anhydrating is got rid of in the leaching crystallization, and lyophilize makes puerarin elaboration of the present invention.
The puerarin that aforesaid method extracts not only can be used for preventing and treating cardiovascular disorder, through clinical trial anti-platform cerebrovascular disease is had tangible curative effect effect.
Puerarin extracting method of the present invention is more a lot of than old method production advantage, because after this law is root of kudzu vine water extract-alcohol precipitation, through polyamide column chromatography, the water wash-out, concentrate and place, separate out the puerarin crude product, crude product passes through polyamide column chromatography once more, water elution, concentrate, separate out crystallization, again through lyophilize or spraying drying or repeat crystallization with 70-80% alcohol and make elaboration, so avoid using inflammable in the technology, the organic solvent of poisoning, the novel process three-waste free pollution, workers ' health is without prejudice, and the puerarin content height reaches more than 90% (the HPLC method), and is with short production cycle, cost is low, is easy to produce promote.The crude product that the present invention extracts is nontoxic also can do medicinal.
The extracting method embodiment of puerarin is as follows:
It is as follows that example 1 is extracted flow process:
1. with root of kudzu vine impurity elimination, clean, be ground into meal;
2. with meal decocting 4 times, each 0.5 hour after-filtration concentrates makes thick paste;
3. add ethanol and make and contain alcohol amount and reach 75%, heat and keep little and boil, and stir, place then, filter, reclaim ethanol, make root of kudzu vine alcohol medicinal extract;
4. again with 14-30 order polyamide granules absorption Radix Puerariae extractum, half-dried after, dry column-packing, polymeric amide consumption 1/5 of the dose of making a living, the post blade diameter length ratio is 1: 4, the water wash-out, the control flow velocity, the Fractional Collections elutriant, divide in addition concentrate, placement, crystallization, the puerarin crude product;
5. after the puerarin crude product oven dry, add dissolve with ethanol, again with Silon absorption, fling to ethanol after, be added to the polymeric amide chromatography post upper end of wet method dress post, used polymeric amide is the 80-180 order, the post blade diameter length ratio is 1: 4, crude product and polymeric amide amount ratio are 1: 3.5; The water wash-out, the Fractional Collections elutriant concentrates respectively and the placement crystallization, and the branch that anhydrates is got rid of in the leaching crystallization, and lyophilize makes the puerarin elaboration.
Embodiment 2:
1. the root of kudzu vine is cleaned and be ground into meal;
2. with meal decocting 3 times, respectively fried in shallow oil 1.5 hours, refilter concentratedly, make thick paste;
3. thick paste adds ethanol, makes to contain alcohol amount and reach 80%, and heated and stirred is placed, and reclaims ethanol and makes root of kudzu vine alcohol medicinal extract;
4. with 14-30 order polyamide granules absorption Radix Puerariae extractum, baking after half-dried, dry column-packing, chromatography is with polymeric amide consumption 1/7 of the dose of making a living, the post blade diameter length ratio is 1: 6, water wash-out, control flow velocity, Fractional Collections elutriant, concentrate respectively and place, crystallization makes the puerarin crude product;
5. after the puerarin crude product being dried, add small amount of ethanol dissolving after, adsorb with an amount of Silon again, after flinging to ethanol, be added to the polymeric amide chromatography post upper end of wet method dress post, polymeric amide is the 100-150 order, post blade diameter length ratio 1: 6, puerarin crude product and polymeric amide amount ratio are 1: 4.5; The water wash-out, the Fractional Collections elutriant concentrates respectively and the placement analysis of products, and the part of anhydrating is got rid of in the leaching crystallization, and lyophilize makes the puerarin elaboration.
Embodiment 3:
Above-mentioned the 4. the step obtain the puerarin crude product after system elaboration technology the puerarin crude product can also be added the less water heating for dissolving, through ceaselessly stirring, cool off, to be crystallizedly separate out complete back, filter 2-5 time so repeatedly, obtain the weak yellow liquid puerarin, spraying drying makes elaboration then;
Embodiment 4:
The process for refining other method of above-mentioned puerarin crude product be with puerarin coarse-grain product behind 2-5 recrystallization repeatedly, oven dry with 70-80% ethanol heating for dissolving, is placed crystallization, wait crystallization to produce fully after, leaching crystallization, oven dry promptly get the puerarin elaboration.

Claims (8)

1, a kind of puerarin, it is characterized in that it is a kind of natural compounds that extracts from the herbal medicine root of kudzu vine, middle crude product in the extraction is non-toxic aq, medicinal extract or the rough crystal of brown xanchromatic, and the elaboration after repeating crystallization for several times is the white crystals product, its puerarin (C 20H 21O 9) content is more than 90%.
2, a kind of method of extracting the described puerarin of claim 1, it is characterized in that: the extraction process flow process is: with raw material root of kudzu vine pulverizing-decocting-concentrate placements-Jia ethanol sedimentation-pure medicinal extract-can make puerarin crystallization elaboration by polyamide column chromatography-water elution-concentrate-separate out puerarin crystallization-again through lyophilize or spraying drying or with 70-80% ethanol repetition crystallization through polyamide column chromatography-water elution-concentrate-place-separate out puerarin crude product-once more.
3, according to the method for the described extraction puerarin of claim 2, it is characterized in that: extraction step is as follows:
1. at first meal is mixed, cleans, is ground into to root of kudzu vine raw material clearly;
2. root of kudzu vine meal water is decocted 2-4 time, decocting time is 0.5-2 hour, then after filtration, concentrate and make thick paste;
3. thick paste adds ethanol, makes to contain alcohol amount and reach 70-85%, and reheat is little to boil, and stirs, and places, and filters, and reclaims ethanol, root of kudzu vine alcohol medicinal extract;
4. with polyamide granules absorption root of kudzu vine alcohol medicinal extract, make it half-dried after, dry column-packing, its chromatography polymeric amide is the 14-30 order, the make a living 1/10-1/5 of dose of its consumption, the post blade diameter length ratio is 1: 2-7; The water wash-out, the control flow velocity, the Fractional Collections elutriant concentrates and places crystallization respectively, gets pale brown look puerarin crude product;
5. the process for purification of puerarin crude product is: after the raw product drying, use the small amount of ethanol heating for dissolving, adsorb with Silon again, behind the volatilization ethanol, be added to the polymeric amide chromatography post upper end of wet method dress post again, polymeric amide is the 60-200 order, and the post blade diameter length ratio is 1: 3-7, and crude product and polymeric amide amount ratio are 1: 3-5; The water wash-out, the Fractional Collections elutriant concentrates respectively and the placement crystallization, and the part of anhydrating is got rid of in the leaching crystallization, and lyophilize makes puerarin elaboration of the present invention.
4, puerarin extracting method according to claim 2 is characterized in that extraction step is:
1. with root of kudzu vine impurity elimination, clean, be ground into meal;
2. with meal decocting 4 times, each 0.5 hour after-filtration concentrates makes thick paste;
3. add ethanol and make and contain alcohol amount and reach 75%, heat and keep little and boil, and stir, place then, filter, reclaim ethanol, make root of kudzu vine alcohol medicinal extract;
4. again with 14-30 order polyamide granules absorption Radix Puerariae extractum, half-dried after, dry column-packing, polymeric amide consumption 1/5 of the dose of making a living, the post blade diameter length ratio is 1: 4, the water wash-out, the control flow velocity, the Fractional Collections elutriant concentrates respectively, placement, crystallization, the puerarin crude product;
5. after the puerarin crude product oven dry, add dissolve with ethanol, again with Silon absorption, fling to ethanol after, be added to the polymeric amide chromatography post upper end of wet method dress post, used polymeric amide is the 80-180 order, the post blade diameter length ratio is 1: 4, crude product and polymeric amide amount ratio are 1: 3.5; The water wash-out, the Fractional Collections elutriant concentrates respectively and the placement crystallization, and the branch that anhydrates is got rid of in the leaching crystallization, and lyophilize makes the puerarin elaboration.
5, puerarin extracting method according to claim 2 is characterized in that extracting the step and poly-ly is:
1. the root of kudzu vine is cleaned and be ground into meal;
2. with meal decocting 3 times, respectively fried in shallow oil 0.5 hour, refilter concentratedly, make thick paste;
3. thick paste adds ethanol, makes to contain alcohol amount and reach 80%, and heated and stirred is placed, and reclaims ethanol and makes root of kudzu vine alcohol medicinal extract;
4. with 14-30 purpose polyamide granules absorption Radix Puerariae extractum, baking after half-dried, dry column-packing, chromatography is with polymeric amide consumption 1/7 of the dose of making a living, the post blade diameter length ratio is 1: 6, water wash-out, control flow velocity, Fractional Collections elutriant, concentrate respectively and place, crystallization makes the puerarin crude product;
5. after the puerarin crude product being dried, add small amount of ethanol dissolving after, adsorb with an amount of Silon again, after flinging to ethanol, be added to the polymeric amide chromatography post upper end of wet method dress post, polymeric amide is the 100-150 order, post blade diameter length ratio 1: 6, crude product and polymeric amide amount ratio are 1: 4.5; The water wash-out, the Fractional Collections elutriant concentrates respectively and the placement crystallization, and the part of anhydrating is got rid of in the leaching crystallization, and lyophilize makes the puerarin elaboration.
6, puerarin extracting method according to claim 2, the process for purification that it is characterized in that the puerarin crude product in the 5th step in the extraction step is: the puerarin crude product is added the less water heating for dissolving, ceaselessly stir, cooling, to be crystallized separate out fully after, filter, 2-5 time so repeatedly, obtain the weak yellow liquid puerarin, spraying drying makes the puerarin elaboration then.
7, puerarin crude product refining method according to claim 5 is characterized in that: with the puerarin crude product behind 2-5 recrystallization repeatedly, oven dry, with 70-80% ethanol heating for dissolving, place crystallization, wait crystallization to produce fully after, the leaching crystallization, oven dry promptly gets the puerarin elaboration.
8, a kind of purposes of using the described puerarin of claim 1 that the described method of claim 2 extracts is characterized in that puerarin can be used as to prevent and treat cerebro-vascular diseases tangible curative effect effect is arranged.
CN95110343A 1995-02-23 1995-02-23 Extraction and application of Lobed Kudzuvine Expired - Fee Related CN1057093C (en)

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CN95110343A CN1057093C (en) 1995-02-23 1995-02-23 Extraction and application of Lobed Kudzuvine

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Application Number Priority Date Filing Date Title
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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1054068C (en) * 1996-01-18 2000-07-05 陕西镇坪制药厂 Method for preparation of puerarin
CN1312168C (en) * 2004-08-29 2007-04-25 徐卫臣 Puerarin preparing process
CN1872081B (en) * 2005-06-03 2010-07-28 天津天士力制药股份有限公司 Application of kudzuvine root flavone in preparing medicine for treating chronic insufficiency of blood supply for brain
CN101899041A (en) * 2009-05-31 2010-12-01 中国医学科学院药物研究所 Superior medicinal crystal-form solid substance of puerarin as well as preparation method and application thereof
CN105198865A (en) * 2015-10-26 2015-12-30 中国药科大学 Puerarin dihydrate
CN108719982A (en) * 2018-05-21 2018-11-02 湖北葛百岁葛业有限公司 Kudzuvine root starch preparation method rich in Puerarin

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1033914C (en) * 1991-11-06 1997-01-29 河南省医学科学研究所 Kudzu vine root extract, its preparation and use

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1054068C (en) * 1996-01-18 2000-07-05 陕西镇坪制药厂 Method for preparation of puerarin
CN1312168C (en) * 2004-08-29 2007-04-25 徐卫臣 Puerarin preparing process
CN1872081B (en) * 2005-06-03 2010-07-28 天津天士力制药股份有限公司 Application of kudzuvine root flavone in preparing medicine for treating chronic insufficiency of blood supply for brain
CN101899041A (en) * 2009-05-31 2010-12-01 中国医学科学院药物研究所 Superior medicinal crystal-form solid substance of puerarin as well as preparation method and application thereof
CN101899041B (en) * 2009-05-31 2015-01-21 山东益康药业股份有限公司 Superior medicinal crystal-form solid substance of puerarin as well as preparation method and application thereof
CN105198865A (en) * 2015-10-26 2015-12-30 中国药科大学 Puerarin dihydrate
CN108719982A (en) * 2018-05-21 2018-11-02 湖北葛百岁葛业有限公司 Kudzuvine root starch preparation method rich in Puerarin

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