CN103570776A - Refining method for extracting and separating polydatin - Google Patents
Refining method for extracting and separating polydatin Download PDFInfo
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- CN103570776A CN103570776A CN201310531365.2A CN201310531365A CN103570776A CN 103570776 A CN103570776 A CN 103570776A CN 201310531365 A CN201310531365 A CN 201310531365A CN 103570776 A CN103570776 A CN 103570776A
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- polidatin
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Abstract
The invention discloses a refining method for extracting and separating polydatin. The refining method comprises the following steps: (1) pretreating raw materials: drying and smashing polygonum cuspidatum; (2) extracting: reflux extracting by an organic solvent, filtering after extraction each time, and combining filtrates; (3) concentrating: vacuum concentrating the filtrate, and obtaining thick extractum; (4) mixing silica gel: adding silica gel into the thick extractum, mixing uniformly, drying to constant weight: (5) eluting: loading mixed silica gel into a chromatographic column, eluting through an eluent, and collecting eluant; (6) concentrating and crystallizing: vacuum concentrating the eluant, naturally cooling and crystallizing, filtering, drying, and obtaining the polydatin. The refining method is simple, needs few equipment, has low cost, short production cycle, and high yield and purity, is environment-friendly, and is suitable for industrial volume production.
Description
Technical field
The present invention relates to a kind of extraction separation and refining method of polidatin.
Background technology
Polidatin (Polydatin), has another name called Polydatin, piceid; Chemical name 3,4', 5-Trihydroxystilbene-3-beta-D-glucopyranoside, molecular formula C
20h
22o
8, molecular weight 390.40, CAS 65914-17-2.Polidatin is widely distributed in plant, and data shows, at least more than 70, in kind of plant, found at present polidatin.Polidatin is mainly derived from the dry rhizome of polygonaceae plant giant knotweed.Polidatin is on the architecture basics of trans-resveratrol, to increase a glucosyl group, has the activity similar with trans-resveratrol, in enteron aisle, under the effect of Glycosylase, can discharge trans-resveratrol.
Polidatin has enhancing cardiac contractility, regulates antiotasis, and anti-arterial endothelial injury thrombosis, improves microcirculation, alleviates the injuries of tissues and organs that free radical, intracellular toxin, extruding etc. cause, protection liver cell, reducing blood-fat and the effect such as anti-oxidant.
At present, the method that obtains polidatin is fewer, and product yield and purity that prior art is produced are all on the low side, so production cost is higher, is not suitable for large-scale industrial production.
Summary of the invention
Technical problem to be solved by this invention is, provides a kind of product yield high, and purity is high, is applicable to the extraction separation and refining method of the polidatin of large-scale industrial production.
The technical solution adopted for the present invention to solve the technical problems is: a kind of extraction separation and refining method of polidatin, comprises the following steps:
(1) raw materials pretreatment: the natural plant raw material containing polidatin is dried, pulverize;
(2) extract: raw material organic solvent refluxing extraction 2-4 time that will process through step (1), doubly, each extraction time is 2-4 hour to the 3-6 that the consumption that at every turn extracts organic solvent is raw material weight, each rear filtration, merging filtrate of extracting;
(3) concentrated: by step (2) gained filtrate in 40-80 ℃ of (preferably 60-75 ℃) concentrating under reduced pressure, to the volume 1/8-1/12(that is former filtrate volume preferably 1/10), obtain thick medicinal extract;
(4) silica gel mixed sample: add silica gel in the thick medicinal extract of step (3) gained, the consumption of silica gel is 1.0-1.5 times of thick medicinal extract weight, mixes, and dries to constant weight, must mix the silica gel of sample;
(5) wash-out: by the silica obtained chromatography column that packs into of step (4), use eluent wash-out, collect elutriant;
(6) condensing crystal: by step (5) gained elutriant in temperature 40-80 ℃ of (preferably 60-75 ℃) concentrating under reduced pressure, to the volume 1/18-1/22(that is former effluent volume preferably 1/20), naturally cooling crystallization, filter, obtain filter cake, dry, obtain polidatin.
Further, in step (1), the described natural phant containing polidatin is giant knotweed etc.
Further, in step (2), described organic solvent is methyl alcohol, ethanol, propyl alcohol, butanols or ethyl acetate etc.
Further, in step (5), described eluent is sherwood oil, tetrahydrofuran (THF), ethyl acetate, methyl alcohol, ethanol or Virahol etc.
Further, in step (5), the consumption of eluent is the preferred 3.0BV of 2.5-3.5BV().
Compared with prior art, the present invention has the following advantages: the solvent wide material sources of use, and environment-protecting asepsis side effect, technique is simple, and required equipment is few, and production cost is low, with short production cycle, and product yield and purity are high, environmental friendliness, suitability for industrialized batch production.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
embodiment 1
The present embodiment comprises the following steps:
(1) raw materials pretreatment: giant knotweed is dried, get 200Kg(containing polidatin 1.5wt%), pulverize, cross 60 mesh sieves;
(2) extract: the giant knotweed that will process through step (1) extracts 3 times by ethyl acetate backflow, the consumption that extracts for the first time ethyl acetate is 5 times of giant knotweed weight, extraction time is 3 hours, the consumption that extracts for the second time ethyl acetate is 5 times of giant knotweed weight, extraction time is 2 hours, and the consumption that extracts for the third time ethyl acetate is 4 times of giant knotweed weight, and extraction time is 2 hours, after each extraction, filter merging filtrate;
(3) concentrated: by step (2) gained filtrate in 75 ℃ of concentrating under reduced pressure, to volume be former filtrate volume 1/10, obtain thick medicinal extract 25Kg;
(4) silica gel mixed sample: add 25Kg silica gel in the thick medicinal extract of step (3) gained, mix, and dry to constant weight, must mix the silica gel of sample;
(5) wash-out: by the silica obtained chromatography column that packs into of step (4), use 3.0BV eluent ethyl acetate, collect elutriant 0.3m
3;
(6) condensing crystal: it is 15L that step (5) gained elutriant is evaporated to volume in 70 ℃, naturally cooling crystallization 8 hours, suction filtration, obtains filter cake, dries to constant weight for 60 ℃, obtains polidatin sterling 2.8Kg, and purity is 98.62%, and yield is 92.04%.
embodiment 2
The present embodiment comprises the following steps:
(1) raw materials pretreatment: giant knotweed is dried, get 300Kg(containing polidatin 1.5wt%), pulverize, cross 60 mesh sieves;
(2) extract: the giant knotweed that will process through step (1) extracts 3 times with methanol eddy, the consumption that extracts for the first time methyl alcohol is 5 times of giant knotweed weight, extraction time is 3 hours, the consumption that extracts for the second time methyl alcohol is 5 times of giant knotweed weight, extraction time is 2 hours, and the consumption that extracts for the third time methyl alcohol is 4 times of giant knotweed weight, and extraction time is 2 hours, after each extraction, filter merging filtrate;
(3) concentrated: by step (2) gained filtrate in 60 ℃ of concentrating under reduced pressure, to volume be former filtrate volume 1/10, obtain thick medicinal extract 46Kg;
(4) silica gel mixed sample: add 46Kg silica gel in the thick medicinal extract of step (3) gained, mix, and dry to constant weight, must mix the silica gel 90Kg of sample;
(5) wash-out: by the silica obtained chromatography column that packs into of step (4), use 3.0BV methanol-eluted fractions, collect elutriant 0.4m
3;
(6) condensing crystal: it is 20L that step (5) gained elutriant is evaporated to volume in 70 ℃, naturally cooling crystallization 8 hours, suction filtration, obtains filter cake, dries to constant weight for 60 ℃, obtains polidatin sterling 4.2Kg, and purity is 98.07%, and yield is 91.53%.
Claims (5)
1. an extraction separation and refining method for polidatin, is characterized in that, comprises the following steps:
(1) raw materials pretreatment: the natural plant raw material containing polidatin is dried, pulverize;
(2) extract: raw material organic solvent refluxing extraction 2-4 time that will process through step (1), doubly, each extraction time is 2-4 hour to the 3-6 that the consumption that at every turn extracts organic solvent is raw material weight, each rear filtration, merging filtrate of extracting;
(3) concentrated: step (2) gained filtrate, in 40-80 ℃ of concentrating under reduced pressure, to the 1/8-1/12 that volume is former filtrate volume, is obtained to thick medicinal extract;
(4) silica gel mixed sample: add silica gel in the thick medicinal extract of step (3) gained, the consumption of silica gel is 1.0-1.5 times of thick medicinal extract weight, mixes, and dries to constant weight, must mix the silica gel of sample;
(5) wash-out: by the silica obtained chromatography column that packs into of step (4), use eluent wash-out, collect elutriant;
(6) condensing crystal: in temperature 40-80 ℃ concentrating under reduced pressure, to the 1/18-1/22 that volume is former effluent volume, naturally cooling crystallization, filters, and obtains filter cake, dries, and obtains polidatin by step (5) gained elutriant.
2. the extraction separation and refining method of polidatin according to claim 1, is characterized in that, in step (1), the described natural phant containing polidatin is giant knotweed.
3. the extraction separation and refining method of polidatin according to claim 1 and 2, is characterized in that, in step (2), described organic solvent is methyl alcohol, ethanol, propyl alcohol, butanols or ethyl acetate.
4. the extraction separation and refining method of polidatin according to claim 1 and 2, is characterized in that, in step (5), described eluent is sherwood oil, tetrahydrofuran (THF), ethyl acetate, methyl alcohol, ethanol or Virahol.
5. the extraction separation and refining method of polidatin according to claim 1 and 2, is characterized in that, in step (5), the consumption of eluent is 2.5-3.5BV.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104688751A (en) * | 2015-03-23 | 2015-06-10 | 董鸣 | Application of polydatin to preparation of anti-arrhythmic product |
| CN108440616A (en) * | 2018-05-30 | 2018-08-24 | 云南海沣药业有限公司 | A kind of extraction separation method of polygonin |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104688751A (en) * | 2015-03-23 | 2015-06-10 | 董鸣 | Application of polydatin to preparation of anti-arrhythmic product |
| CN104688751B (en) * | 2015-03-23 | 2018-09-11 | 深圳大学 | Purposes of the polygonin in preparing anti-arrhythmia product |
| CN108440616A (en) * | 2018-05-30 | 2018-08-24 | 云南海沣药业有限公司 | A kind of extraction separation method of polygonin |
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Application publication date: 20140212 |