CN101613387A - The method of extracting purified puerarin by utilizing ion-exchange fiber - Google Patents
The method of extracting purified puerarin by utilizing ion-exchange fiber Download PDFInfo
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- CN101613387A CN101613387A CN200810126427A CN200810126427A CN101613387A CN 101613387 A CN101613387 A CN 101613387A CN 200810126427 A CN200810126427 A CN 200810126427A CN 200810126427 A CN200810126427 A CN 200810126427A CN 101613387 A CN101613387 A CN 101613387A
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- HKEAFJYKMMKDOR-VPRICQMDSA-N puerarin Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1C1=C(O)C=CC(C2=O)=C1OC=C2C1=CC=C(O)C=C1 HKEAFJYKMMKDOR-VPRICQMDSA-N 0.000 title claims abstract description 39
- RXUWDKBZZLIASQ-UHFFFAOYSA-N Puerarin Natural products OCC1OC(Oc2c(O)cc(O)c3C(=O)C(=COc23)c4ccc(O)cc4)C(O)C(O)C1O RXUWDKBZZLIASQ-UHFFFAOYSA-N 0.000 title claims abstract description 38
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- 238000000605 extraction Methods 0.000 claims description 14
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Landscapes
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The present invention utilizes ion-exchange fiber to extract a kind of method of purifying plant medicinal component puerarin.This method operation steps is specially: the root piece starting material clean dry that Pueraria lobota belongs to is pulverized back decoction leaching, at puerarin original liquid concentration 1.0～6.0gL
-110～80 ℃ of temperature; Flow velocity 0.5～10.0BVh
-1(BV: column volume); The pH value is under 6.0～12.0 the condition, to adsorb with the ion-exchange fiber post.Again with 10～90 ℃ of eluting temperatures; Flow velocity 0.2～15BVh
-1Eluent and acid concentration are 0.1～3.0molL
-1The volume ratio of pH regulator agent be 2～6: 1 elutriant wash-out.Collect elutriant, reclaim organism and get the puerarin extract powder.This method equipment maturation, operating procedure is simple, fiber utilization rate height, running cost is low, the processing efficiency height, energy-saving effect is remarkable, has improved product purity and yield, is applicable to suitability for industrialized production.
Description
Technical field
The present invention relates to the method with ion-exchange fiber extraction, separation and purifying natural plants ' medicinal component, specifically, is the method for extracting puerarin in the purifying herbal with ion-exchange fiber.
Background technology
(Ion Exchange Fiber is a kind of fibrous ion exchange sorbing material IEF) to ion-exchange fiber, and it is made of the monofilament of many even thickness, and its diameter range is between 20～300 μ m.Itself contain non diffusible ion and and the movable ion of non diffusible ion opposite in sign.When the solution with the compound that can dissociate contacts, the movable ion of ion-exchange fiber promptly with solution in the ion of same-sign exchange, so claim ion-exchange fiber.Compare with the particulate state ion-exchanger, ion-exchange fiber has that specific surface is big, and diameter is little, and absorption, desorption rate are fast, and exchange capacity is big, regeneration easily, characteristics such as type of service is various.
Ion-exchange fiber mainly is divided into four classes: strong-acid cation exchange fibre, Subacidity cation exchange fiber, strongly basic anion ion exchange fibre, weakly basic anion exchange fibre.
As if the skeleton of representing the strong base anion fiber with R, when then fiber fully contacted with puerarin solution, permutoid reaction took place, reaction process constantly consumes the cation exchange groups of strong base anion exchange fiber, causes the exchange capacity of fiber to weaken, even loses exchange capacity.In order to recover the exchange capacity of fiber, can make fiber recover exchange capacity with the layer of fibers of certain density NaOH solution by having lost efficacy.Therefore ion-exchange capacity is a reversible.This reversibility can be used fiber repeatedly.
The root of kudzu vine is the dry root of legume pueraria lobata [Pueraria lobata (Willd.) Ohwi], makes sweet Pueraria lobota, Pachyrhizua angulatus, the yellow root of kudzu vine, Pueraria lobota fiber crops eat again.The pharmaceutical use of the root of kudzu vine is all on the books in " herbal classic ", " not Lu ", Compendium of Material Medica, " typhoid fever miscellaneous diseases note " etc., has expelling pathogenic factors from muscles for reducing heat, promotes the production of body fluid, the merit of promoting eruption, the positive antidiarrheal of liter.Puerarin (Puerarin) is the main effective constituent of the Chinese medicine root of kudzu vine, contains osajin, three mushroom classes, aromatics isoreactivity composition in addition.The puerarin chemistry is called 4 ', 7-dihydroxyl-8-β-D-glucose isoflavones, and molecular formula is C
21H
20O
9, molecular weight is 416.37, chemical structure is as shown below.
Structural formula
Puerarin is white column crystallization, 187 ℃-188 ℃ of fusing points.Water-soluble and fat-soluble all very poor, solubleness is 0.462g/100ml in water.Need in the preparation to add solubility promoter, the polyethylene that has commonly used adjoins pyrrolidone (PVP) etc.Puerarin solubleness is 1.332g/100ml in the 4.3%PVP aqueous solution.Puerarin has vasodilation, reduces myocardial consumption of oxygen, improves myocardial contraction, and effect such as stimulate circulation clinically is used for the treatment of coronary heart disease, stenocardia, acute myocardial infarction etc. and heart and brain cycle penalty diseases associated with puerarin.Also have lowering blood glucose, blood fat, anti-oxidant, increase blood fluidity, reduce pulmonary hypertension, treat diabetic peripheral neuropathy and improve effects such as insulin resistant.Owing to its low toxicity, safety, high curative effect are widely used in clinical.Become domestic research focus in recent years.Puerarin was used for clinical by Ministry of Health's approval in 1993.
Along with the research of puerarin Application and Development, people are more and more urgent to the requirement of its high purity, single compound.Puerarin is mainly from the root of kudzu vine at present, and its extracting method mainly contains following several: column chromatography, Amberlyst process, acid-hydrolysis method, Glacial acetic acid recrystallization method, water extraction and alcohol precipitation method, n-butanol-water extraction process, ultrasonic extraction, aluminum oxide decoloring method, beta-cyclodextrin bonded stationary phase method etc.
But these method efficient are all lower, and the puerarin purity of separating is not high, poor repeatability, and link is many, and the consumption of chromatography column material is big, uses inflammable, deleterious organic solvent in a large number, easily causes environmental pollution, the production cost height, the cycle is long.Make the bad monitoring of index in the sepn process.
Summary of the invention
Technical problem to be solved by this invention is at existing technical deficiency, and a kind of method of separation and purification puerarin is provided, and makes to extract that foreign matter content is few, service efficiency is high, operating procedure is simple and direct, production cost is low, is suitable for the puerarin method of large-scale production.
The present invention for the technical scheme that solves the problems of the technologies described above employing is:
(1) the root starting material of Pueraria lobota platymiscium are clean, dry, pulverizing back decocts lixiviate;
(2) vat liquor adsorbs with the ion-exchange fiber post;
(3) will be adsorbed on puerarin desorb (wash-out) on the ion-exchange fiber post;
(4) the elutriant drying obtains the powder of puerarin.
Wherein, the decocting that the root of kudzu vine powder of step (1) can add water, alcohol, ester or its mixture boils, and the decocting that preferably contains methanol boils, and extraction temperature is 20～90 ℃, preferably near the temperature of solution boiling point; The pH value is 5.0～10.0, and preferred pH value is 6.5～9.0; Extraction time 1～5h, preferred 3h; Lixiviate number of times 2～5 times, preferred 3 times.
Wherein, the ion-exchange fiber that uses of step (2) is strong basicity ion-exchange fiber or Weak-alkaline ion exchange fibre.Preferred strong basicity ion-exchange fiber, the type fiber is used for the separation and purification of puerarin class, is to adopt first.The weight ratio of handled medicinal material and fiber is 2～30: 1, preferred 3～25: 1; Adorn post, the water of preferred 2～3 times of column volumes with the water wet method of 1～4 times of column volume earlier; Again with puerarin original liquid concentration 1.0～6.0gL
-1, preferred 3.0～4.0gL
-1Temperature is 10～80 ℃, preferred 30～70 ℃; Flow velocity 0.5～10.0BVh
-1, preferred 0.8～5.0BVh
-1The pH value is 6.0～12.0, and preferred pH value is 7.0～11.5 condition absorption.
Wherein, step (3) is the water elution of elder generation with 1～3 times of column volume, the water elution of preferred 2 times of column volumes; Again with water, alcohol or its mixed solution wash-out of 4～15 times of column volumes, 55～75% ethanol elutions of preferred 5～8 times of column volumes; Eluting temperature is 10～90 ℃, and preferred temperature is 50～80 ℃; Flow velocity 0.2～15.0BVh
-1, preferable flow rate 1.0～10.0BVh
-1Eluent and acid concentration are 0.1～3.0molL
-1The volume ratio of pH regulator agent is 2～6: 1, preferred 3～5.Collect alcohol eluen.
Wherein, step (4) is that organism gets concentrated solution in the recovery elutriant, gets powder through vacuum decompression drying or lyophilize again.
The present invention is suitable for any Pueraria lobota and belongs to raw-material puerarin extraction purifying.
Beneficial effect of the present invention is embodied in:
1. puerarin production method of the present invention has adopted unique alkali ion exchange fiber as chromatographic material, is to use first.
2. used production unit maturation, the medicinal material proportion of fibers is low, and extracting solution is directly gone up chromatography column without concentrating and any purification process, and technological operation is simple, and production stage is few, and production cost is low, and processing efficiency height, energy-saving effect are remarkable.
3. the inventive method has improved product purity and yield, and quality standard is controlled, and running cost is low, and solution can be recycled after distillation is reclaimed, and non-secondary pollution is applicable to suitability for industrialized production.
Specific embodiments
Below further set forth the present invention with embodiment, but therefore do not limit the present invention in the specific embodiment model.
Embodiment 1
Take by weighing 10g Radix Puerariae medicinal material, after clean dry is pulverized, add the 90mL decocting and boiled 3 hours, the pH value of solution value is 8.0, and the decocting with 60mL boiled 1 hour again, merged decoction liquor, and transferring the pH value of solution value this moment is 8.9 coolings, with flow velocity 1.5 BVh
-1, be that 0.5g, bed volume are that the strong basicity ion-exchange fiber post of 5mL adsorbs through weight.Again with flow velocity 6.0BVh
-1, the water elution of 3 times of column volumes, the back is with 60% ethanol (60% ethanol: 2molL of 5 times of column volumes
-1The volume ratio of hydrochloric acid 4: 1) wash-out reclaims ethanol and gets puerarin extract, and wherein puerarin content is 71%, and flour extraction rate is 2.3%.
Embodiment 2
Take by weighing 10g Radix Puerariae medicinal material, after clean dry is pulverized, the ethanol 100mL with 60%, the pH value of solution value is 8.1,60 ℃ of extraction temperatures, 3 hours extraction times are again with 60% ethanol 60mL decoction 1 hour.The puerarin crude product yield that obtains is 10.92%, and purity is 4.56%.Be 9.0 in upper prop soup pH value, flow velocity 3.0BVh
-1, liquor strength is 1.7mgmL
-1Condition under, the strong basicity ion-exchange fiber post of crossing weight and be 0.5g, bed volume and be 5mL adsorbs.With strippant is 60% ethanol and 3molL
-1The mixed solution of acetate (volume ratio 4: 1) 7BV, elution flow rate 6.0BVh
-1Carry out wash-out.Reclaim ethanol and get puerarin extract, wherein puerarin content is 78%, and flour extraction rate is 2.6%.
Embodiment 3
Taking by weighing 200g RADIX PUERARIAE medicinal material, add 60% ethanol 2000mL and located to decoct 2 hours at 60 ℃, decocted 1 hour with 60% ethanol 1000mL, merge pH value and be 8.2 decoction liquor, cool off, is 9.0 in upper prop soup pH value, flow velocity 3BVh
-1, liquor strength is 1.6mgmL
-1Condition under, the strong basicity ion-exchange fiber post of crossing weight and be 8.0g, bed volume and be 80mL adsorbs.With strippant is 70% ethanol and 1.5molL
-1The mixed solution of hydrochloric acid (volume ratio 4: 1) 7BV, elution flow rate 6BVh
-1Carry out wash-out.Reclaim ethanol and get puerarin extract, wherein puerarin content is 76%, and flour extraction rate is 2.2%.
Embodiment 4
Take by weighing 500g RADIX PUERARIAE medicinal material, add pure methyl alcohol 5000mL and located to decoct 2 hours at 64 ℃, decocted 1 hour with pure methyl alcohol 3000mL, merging pH value is 8.4 decoction liquor, and cooling is 11.04 in upper prop soup pH value, flow velocity 3BVh
-1, liquor strength is 2.1mgmL
-1Condition under, the strong basicity ion-exchange fiber post that cross weight and be 20.0, bed volume is 200mL adsorbs.With strippant is 65% ethanol and 2.0molL
-1The mixed solution of hydrochloric acid (volume ratio 4: 1) 8BV, elution flow rate 5BVh
-1Carry out wash-out.Reclaim the pure puerarin extract that gets, wherein puerarin content is 74%, and flour extraction rate is 2.1%.
Claims (13)
1. the production method of a puerarin extract comprises step:
(1) the root starting material of Pueraria lobota platymiscium are clean, dry, pulverizing back decocts lixiviate;
(2) vat liquor adsorbs with the ion-exchange fiber post;
(3) will be adsorbed on puerarin desorb (wash-out) on the ion-exchange fiber post;
(4) the elutriant drying obtains containing the powder of puerarin.
2. in accordance with the method for claim 1, wherein the extraction solvent that uses of step (1) is water, alcohol, ester or its mixture, and the weight ratio of digestion agent and raw material is 10～20: 1.
3. according to claim 1 or 2 described methods, extraction temperature is 20～90 ℃; The pH value is 5.0～10.0; The pH regulator agent is mineral alkali, mineral acid, organic acid, organic bases.
4. according to claim 1 or 2 described methods, extraction time is 1～5 hour; Lixiviate number of times 2～5 times.
5. according to the described method of one of claim 1～4, wherein the ion-exchange fiber that uses of step (2) is strong basicity ion-exchange fiber or Weak-alkaline ion exchange fibre.
6. according to claim 1 or 5 described methods, be to adorn post with the water wet method of 1～4 times of column volume earlier, again with puerarin original liquid concentration 1.0～6.0gL
-1Temperature is 10～80 ℃; Flow velocity 0.5～10.0BVh
-1The pH value is that 6.0～12.0 condition is adsorbed.
7. according to claim 1 or 5,6 described methods, wherein step (3) is the water elution of elder generation with 1～3 column volume, with water, alcohol or its mixed solution wash-out of 4～15 times of column volumes, collects elutriant again.
8. according to claim 1 or 5,6,7 described methods, eluting temperature is 10～90 ℃; Flow velocity 0.2～15.0BVh
-1Eluent and acid concentration are 0.1～3.0molL
-1The volume ratio of pH regulator agent be 2～6: 1.
9. according to claim 1 or 5,6,7,8 described methods, can carry out the adsorption-desorption of one or many ion-exchange fiber chromatography column.
10. according to claim 1 or 5,6,7,8,9 described methods, wherein the weight of step (2) use fiber and the ratio of medicinal material weight are 1: 2～30.
11. according to claim 1 or 5,6,7,8,9,10 described methods, wherein the root starting material of the Pueraria lobota platymiscium of step (1) use are the root starting material of elegant jessamine.
12. according to claim 1 or 5,6,7,8,9,10 described methods, its filamentary material is the strong basicity ion-exchange fiber or the Weak-alkaline ion exchange fibre of homemade or import; Extraction solvent is water, alcohol, ester or its mixture; Eluent is water, alcohol or its mixture; The pH regulator agent is mineral alkali, mineral acid, organic acid, organic bases.
13. according to the described method of one of claim 1～12, wherein, step (4) is that organism gets concentrated solution in the recovery elutriant, obtains powder through vacuum decompression drying or lyophilize again.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102304111A (en) * | 2011-07-12 | 2012-01-04 | 北京服装学院 | Method for extracting and purifying salvianolic acid B with ion exchange fiber |
| CN102532111A (en) * | 2010-12-24 | 2012-07-04 | 天津中新药业集团股份有限公司第六中药厂 | Method for extracting puerarin from traditional Chinese medicine kudzu |
| CN108567769A (en) * | 2017-03-09 | 2018-09-25 | 中国医学科学院药物研究所 | Puerarin is preparing the purposes in preventing and/or treating pulmonary hypertension and its complication medicine |
-
2008
- 2008-06-26 CN CN200810126427A patent/CN101613387A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102532111A (en) * | 2010-12-24 | 2012-07-04 | 天津中新药业集团股份有限公司第六中药厂 | Method for extracting puerarin from traditional Chinese medicine kudzu |
| CN102532111B (en) * | 2010-12-24 | 2016-04-27 | 天津中新药业集团股份有限公司第六中药厂 | A kind of method extracting puerarin from Chinese medicine elegant jessamine |
| CN102304111A (en) * | 2011-07-12 | 2012-01-04 | 北京服装学院 | Method for extracting and purifying salvianolic acid B with ion exchange fiber |
| CN108567769A (en) * | 2017-03-09 | 2018-09-25 | 中国医学科学院药物研究所 | Puerarin is preparing the purposes in preventing and/or treating pulmonary hypertension and its complication medicine |
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