CN103570775A - Method for preparing stibene glucoside from polygonum multiflorum by rapid separation - Google Patents
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Abstract
The invention relates to a method for preparing stibene glucoside from polygonum multiflorum by rapid separation and belongs to the technical field of extraction and separation of stibene glucoside. According to the invention, the stibene glucoside product is prepared by using raw polygonum multiflorum as the raw material through the steps of preparing extract of the raw material, degreasing the extract of the raw material and preparing a crude product and a fine product of stibene glucoside. The method has the characteristics of high extraction efficiency, simple separation preparation process, rapid and time-saving separation process, high purity and good reproducibility of the prepared product, sufficient utilization of the raw material, low production cost and the like. The method can be widely applied to preparation of the stibene glucoside product from polygonum multiflorum by separation and can effectively meet the requirement on preparation of a high-purity sample in the conventional pharmacodynamic experimental research.
Description
Technical field
The invention belongs to the extraction and separation technology field of stilbene glucoside, be specifically related to the method for supersound extraction and middle pressure preparative chromatography fast separating and purifying stilbene glucoside from Tuber Fleeceflower Root medicinal material.
Background technology
Stilbene glucoside claims again 2,3,5,4'-tetrahydroxyl diphenylethylene-2-O-BETA-D-glucoside, belongs to Polyhydroxystibene, and stilbene glucoside is distinctive bioactive ingredients in Tuber Fleeceflower Root medicinal material, is the specificity index component of Tuber Fleeceflower Root medicinal material, soluble in water, methyl alcohol, ethanol.Pharmacological research shows, stilbene glucoside have oxidation and removing free radicals, anti-ageing, reduce cholesterol, protect the liver and neuroprotective, can develop treatment senile dementia, reducing blood-fat and antiatherogenic novel drugs.
Middle pressure preparative chromatography is according to separated component adsorptive power difference and retention time is different on chromatographic column fixed phase, thereby realizes separated chromatographic technique.By optimizing operation parameters, realize material composition sharp separation and prepare, save time.With respect to normal pressure chromatogram, middle pressure chromatographic velocity is very fast, and eluting solvent range of choice is wider, and solvent elution process can linear transformation, is conducive to sharp separation and the preparation of target components.
Existing from Tuber Fleeceflower Root the separated method of preparing stilbene glucoside, as the publication No. of announcing on October 17th, 2012 " preparation technology of the Tuber Fleeceflower Root stilbene glucoside " patent that is CN102731586A, disclosed method is: first adopting Diluted Alcohol is to extract solvent Tuber Fleeceflower Root medicinal material is carried out to refluxing extraction, then use ethyl acetate to extract extracting solution, again ethyl acetate extract layer is carried out to silica gel column chromatography and Sephadex LH-20 column chromatography for separation successively, finally prepare content and be 85% stilbene glucoside.The main drawback of the method is: 1. adopt high temperature reflux to extract stilbene glucoside, and easily oxidized and glycosidic link fracture of stilbene glucoside under hot conditions, this extracting method damages stilbene glucoside; 2. adopt normal pressure column chromatography separating for several times, loaded down with trivial details, the consuming time length of process, solvent consumption is large, has improved preparation cost; 3. component overstand and produce dead absorption in normal pressure pillar, sample losses is large, and the rate of recovery is lower.
Summary of the invention
The object of the invention is the deficiency for existing stilbene glucoside method for separating and preparing, provide a kind of from Tuber Fleeceflower Root medicinal material sharp separation prepare the method for stilbene glucoside, there is extraction efficiency high, separation preparation is simple, sepn process saves time fast, the features such as preparing product purity is high, favorable reproducibility, and prepared using is abundant, and production cost is low.
The technical scheme that realizes the object of the invention is: a kind of from Tuber Fleeceflower Root medicinal material sharp separation prepare the method for stilbene glucoside: take Radix Polygoni Multiflori medicinal material as raw material, through raw materials medicinal extract, the degreasing of raw material medicinal extract, prepare stilbene glucoside crude product and fine work and toluylene glycoside product.The concrete steps of described method are as follows:
(1) raw materials medicinal extract:
The pharmaceutical decocting piece of Radix Polygoni Multiflori of take is raw material, take Diluted Alcohol as extracting solvent.First raw material is put into pulverizer and pulverize, and sieve through 50～100 object iron sieves, collect the raw material powder sieving, unsifted raw material is put into pulverizer again and is pulverized.Then in the quality of raw material powder (g): the ratio of the volume of Diluted Alcohol (mL) is 1: 5～15 ratio, raw material powder and Diluted Alcohol are positioned in supersound extraction device, first be uniformly mixed, at ultrasonic power, be that 300～500W, ultrasonic operating frequency are that 30～60KHZ, temperature are under 50～70 ℃ of conditions again, carry out for the first time after supersound extraction 0.5～1.5h, extracting solution is filtered for the first time, collect respectively primary filtrate and filter residue.The filter residue of collecting is for the first time positioned in supersound extraction device again, again in the quality of filter residue (g): the ratio of the volume of Diluted Alcohol (mL) is 1: 5～15 ratio, again filter residue and the Diluted Alcohol collected are for the first time placed in to supersound extraction device, first be uniformly mixed, at ultrasonic power, be that 300～500W, ultrasonic operating frequency are that 30～60KHZ, temperature are under 50～70C condition again, carry out for the second time after supersound extraction 0.5～1.5h, again extracting solution is filtered for the second time, collect respectively again filtrate and filter residue, so repeat 1～2 time.The filtrate that finally merges each collection, and the most latter incorporated filtrate is positioned over to Rotary Evaporators is evaporated to medicinal extract shape, just prepare raw material medicinal extract I; The filter residue of last collection be can be used for to continual exploitation utilization polysaccharide fraction wherein.
(2) raw material medicinal extract I degreasing:
After (1) step completes, the quality (g) of the raw material medicinal extract I first preparing according to (1) step: the ratio of the volume of sherwood oil (mL) is 1: 5～10 ratio, raw material medicinal extract I and sherwood oil are added in water-bath refluxing extraction device, in the water-bath environment of 60～100 ℃, carry out for the first time refluxing extraction after 0.5～1.5 hour, filter for the first time, collect respectively filtrate (being petroleum ether solvent layer) and filter residue (being lotion).Again according to the quality (g) of the filter residue of collecting for the first time: the volume of sherwood oil (mL) is than the ratio that is 1: 5～10, filter residue and the sherwood oil collected are for the first time added in water-bath refluxing extraction device, again in the water-bath environment of 60～100 ℃, carry out for the second time refluxing extraction 0.5～1.5 hour, filter for the second time again, collect respectively again filtrate (being petroleum ether solvent layer) and filter residue (being lotion), so repeat 1～2 time.The filter residue of finally collecting, just makes the raw material medicinal extract II after skimming treatment; The filtrate that finally merges each collection can be used for the preparation of the products such as Schuttgelb.
(3) prepare stilbene glucoside crude product
After (2) step completes, the quality (g) of the raw material medicinal extract II first making according to (2) step: the ratio of the volume of pure water (mL) is 1: 5～10 ratio, raw material medicinal extract II and pure water are joined in container, be stirred to dissolving, just make sample III to be separated.Centering presses preparative chromatograph to arrange again, adopt initial eluting solvent to carry out separator column balance, adjustment flow rate pump is 3～20mL/min, it is 0.5～2Mpa that post is pressed, after post pressure is stable, again sample III to be separated being positioned in middle pressure preparative chromatograph and being adsorbed after 0～10min, is that the ODS of 50～70 μ m or SBC MCI GEL reverse phase filler, eluting solvent are to carry out middle pressure chromatographic separation under A and two yuan of mixed solvent system conditions of B at separating column packing.Wherein: solvent orange 2 A is water; Solvent B is methyl alcohol or acetonitrile; Solvent orange 2 A: the volume ratio of solvent B is 0-100.Before loading, with initial eluting solvent equilibrium separation post, adjustment flow rate pump is 3～20mL/min, and it is 0.5～2Mpa that post is pressed, until post press stable after, sample III to be separated is pumped in separator column, adsorb start after 0～10min separated; Under the detection wavelength of 320nm, collect out peak flow point again, the peak flow point that goes out of collecting is positioned in Rotary Evaporators and is concentrated, just make stilbene glucoside crude product IV.
(4) prepare toluylene glycoside product
After (3) step completes, in the stilbene glucoside crude product IV making in step (3), add the pure water of 50～70 ℃, be stirred to dissolving, be just prepared into the hot saturated aqueous solution of described stilbene glucoside crude product IV.Then by millipore filtration, filter, collect respectively filtrate and filter residue, then, by filtrate standing 10～24h crystallization at 0～25 ℃, crystal just makes toluylene glycoside product V after vacuum lyophilization; Filter residue discharges after processing.
The present invention adopts after technique scheme, mainly contains following effect:
1. the present invention be take Radix Polygoni Multiflori medicinal material as raw material, through raw materials medicinal extract, the degreasing of raw material medicinal extract, prepare stilbene glucoside crude product and fine work and toluylene glycoside product.Preparation technology is simple, and preparation process is saved solvent, and production cost is low, can realize the sharp separation preparation of product;
2. the present invention adopts stilbene glucoside in supersound extraction Tuber Fleeceflower Root medicinal material coarse powder, utilize hyperacoustic cavatition, mechanical effect and heat effect etc. to accelerate release, diffusion and the dissolving of active substance in born of the same parents, significantly improve extraction efficiency, shortened extraction time, avoided the destruction of long-time high temperature reflux to stilbene glucoside, improved the extraction efficiency of stilbene glucoside, and technical process is simple, easy to operate;
3. the present invention suppresses for chromatographic separation and prepares stilbene glucoside in adopting, and has separation efficiency high, and instrument requires the advantages such as configuration is simple and easy, and solvent range of choice is wide, and sample separation amount is larger.Whole separation process completes in 300min, target compound loss and a large amount of solvent consumption of having avoided conventional column chromatography method repeatable operation to bring, separating obtained stilbene glucoside content in crude product nearly 90%; By the control to separation condition, can make separating resulting there is good circulation ratio;
4. in the present invention, Tuber Fleeceflower Root prepared using is abundant, can produce toluylene glycoside product, and the filter residue after the first step extraction again can be as the extraction raw material of Polygonum polysaccharide; The filtrate of skimming treatment in second step (being petroleum ether layer) can be used as products such as producing Schuttgelb again, thereby further reduces production costs;
The present invention can be widely used in separation from Tuber Fleeceflower Root and prepare toluylene glycoside product, can effectively meet high purity sample preparation in the research of conventional pharmacodynamic experiment demand.
Embodiment
Below in conjunction with embodiment, further illustrate the present invention.
Embodiment 1
A kind of from Tuber Fleeceflower Root medicinal material the concrete steps of the method for sharp separation stilbene glucoside as follows:
(1) raw materials medicinal extract
The pharmaceutical decocting piece of Radix Polygoni Multiflori of take is raw material, take 60% Diluted Alcohol as extracting solvent.First raw material is put into pulverizer and pulverize, and sieve through 80 object iron sieves, collect the raw material powder sieving, unsifted raw material is put into pulverizer again and is pulverized.Then in the quality of raw material powder (g): the ratio that the ratio of the volume of Diluted Alcohol (mL) is 1: 10, raw material powder and Diluted Alcohol are positioned in supersound extraction device, first be uniformly mixed, at ultrasonic power, be that 300W, ultrasonic operating frequency are that 40KHZ, temperature are under 60 ℃ of conditions again, carry out for the first time after supersound extraction 0.5h, extracting solution is filtered for the first time, collect respectively primary filtrate and filter residue.The filter residue of collecting is for the first time positioned in supersound extraction device again, again in the quality of filter residue (g): the ratio that the ratio of the volume of Diluted Alcohol (mL) is 1: 10, again filter residue and the Diluted Alcohol collected are for the first time placed in to supersound extraction device, first be uniformly mixed, at ultrasonic power, be that 300W, ultrasonic operating frequency are that 40KHZ, temperature are under 60 ℃ of conditions again, carry out for the second time after supersound extraction 0.5h, again extracting solution is filtered for the second time, collect respectively again filtrate and filter residue, so repeat 1 time.The filtrate that finally merges each collection, and the most latter incorporated filtrate is positioned over to Rotary Evaporators is evaporated to medicinal extract shape, just prepare raw material medicinal extract I; The filter residue of last collection be can be used for to continual exploitation utilization polysaccharide fraction wherein.
(2) raw material medicinal extract I degreasing:
After (1) step completes, the quality (g) of the raw material medicinal extract I first preparing according to (1) step: the ratio that the ratio of the volume of sherwood oil (mL) is 1: 8, raw material medicinal extract I and sherwood oil are added in water-bath refluxing extraction device, in the water-bath environment of 90 ℃, carry out for the first time refluxing extraction after 1.0 hours, filter for the first time, collect respectively filtrate (being petroleum ether solvent layer) and filter residue (being lotion).Again according to the quality (g) of the filter residue of collecting for the first time: the volume of sherwood oil (mL) is than the ratio that is 1: 8, filter residue and the sherwood oil collected are for the first time added in water-bath refluxing extraction device, again in the water-bath environment of 90 ℃, carry out for the second time refluxing extraction 1.0 hours, filter for the second time again, collect respectively again filtrate (being petroleum ether solvent layer) and filter residue (being lotion), so repeat 1 time.The filter residue of finally collecting, just makes the raw material medicinal extract II after skimming treatment; The filtrate that finally merges each collection can be used for the preparation of the products such as Schuttgelb.
(3) prepare stilbene glucoside crude product
After (2) step completes, the quality (g) of the raw material medicinal extract II first making according to (2) step: the ratio that the ratio of the volume of pure water (mL) is 1: 8, raw material medicinal extract II and pure water are joined in container, be stirred to dissolving, just make sample III to be separated.Centering presses preparative chromatograph to arrange again, adopt initial eluting solvent to carry out separator column balance, adjustment flow rate pump is 5mL/min, post is pressed as 0.7Mpa, after post pressure is stable, again sample III to be separated is positioned in middle pressure preparative chromatograph and is adsorbed after 10min, SBC MCI GEL reverse phase filler, the eluting solvent that is 50～701 μ m at separating column packing is to carry out middle pressure chromatographic separation under A and two yuan of mixed solvent system conditions of B.Wherein: solvent orange 2 A is water; Solvent B is methyl alcohol or acetonitrile; The volume fraction of solvent B is increased to 100% gradually from 0% in time.Then under the detection wavelength of 320nm, collect out peak flow point, it is concentrated that flow point is placed in Rotary Evaporators, just makes stilbene glucoside crude product IV.
(4) prepare toluylene glycoside product
After (3) step completes, in the stilbene glucoside crude product IV making in step (3), add the pure water of 60 ℃, be stirred to dissolving, be just prepared into the hot saturated aqueous solution of described stilbene glucoside crude product IV.By millipore filtration, filter, collect respectively filtrate and filter residue, then, by filtrate standing 24h crystallization at 25 ℃, crystal just makes toluylene glycoside product V after vacuum lyophilization; Filter residue discharges after processing.
Embodiment 2
In adopting, press a method for stilbene glucoside in preparative chromatography sharp separation Tuber Fleeceflower Root, with embodiment 1, wherein:
In (1) step: after Tuber Fleeceflower Root medicinal material 500.0g is pulverized, cross 100 mesh sieves, medicinal powder after sieving and 50% Diluted Alcohol solution are according to the quality of raw material powder (g): the ratio of the volume of Diluted Alcohol (mL) is 1: 8, at ultrasonic power, be that 500W, ultrasonic operating frequency are 50KHZ, extracting temperature is under 70 ℃ of conditions, extract 1.0h, so repeat 2 times, prepare raw material medicinal extract I.
In (2) step: the quality of described raw material medicinal extract (g): the ratio of the volume of sherwood oil (mL) is 1: 10, in the water-bath environment of 95 ℃, refluxing extraction 0.5h, repeats operation 2 times, makes the raw material medicinal extract II of skimming treatment.
In (3) step: described raw material medicinal extract II quality (g): the ratio of pure water volume (mL) is 1: 5; The acetonitrile that the volume fraction of take is 25% is initial solvent equilibrium separation post, adjustment flow velocity is 8mL/min, then sample III to be separated is pumped in middle pressure separator column, after absorption 8min, at column packing, be 50-70 μ mSBC MCI GEL, eluting solvent A is water, solvent B is acetonitrile, and solvent orange 2 A is 75: 25 with the ratio of the volume of solvent B, condition under carry out separation, make stilbene glucoside crude product IV.
In (4) step: described hot saturated aqueous solution temperature is 50 ℃, standing 12h crystallization at 4 ℃ then, crystal obtains toluylene glycoside product V after lyophilize.
Embodiment 3
In adopting, press a method for stilbene glucoside in preparative chromatography sharp separation Tuber Fleeceflower Root, with embodiment 1, wherein:
In (1) step: after Tuber Fleeceflower Root medicinal material 500.0g is pulverized, cross 60 mesh sieves, medicinal powder after sieving and 40% Diluted Alcohol solution are according to the quality of raw material powder (g): the ratio of the volume of Diluted Alcohol (mL) is 1: 15, be added in ultrasonic extraction device, at ultrasonic power, be that 350W, ultrasonic operating frequency are 40KHZ, extracting temperature is under 65 ℃ of conditions, carries out after supersound extraction 1.5h, repetitive operation 2 times, prepares raw material medicinal extract I.
In (2) step: the quality of described raw material medicinal extract (g): the ratio of the volume of sherwood oil (mL) is 1: 5, in the water-bath environment of 60 ℃, refluxing extraction 1.5h, repeats operation 2 times, makes the raw material medicinal extract II of skimming treatment.
In (3) step: described raw material medicinal extract II quality (g): the ratio of pure water volume (mL) is 1: 10; The methyl alcohol that the volume fraction of take is 15% is initial solvent equilibrium separation post, adjustment flow velocity is 15mL/min, then sample III to be separated is pumped in middle pressure separator column, after absorption 5min, at column packing, be 50-70 μ m ODS, eluting solvent A is water, solvent B is acetonitrile, and solvent orange 2 A is 85: 15 with the ratio of the volume of solvent B, condition under carry out separation, make stilbene glucoside crude product IV.
In (4) step: described hot saturated solution temperature is 70 ℃, then time of repose 10h crystallization under 0 ℃ of condition, obtains toluylene glycoside product V after crystal lyophilize.
Experimental result
By method described in the present invention, the toluylene glycoside product V preparing, with reference to the testing method under the assay item of stilbene glucoside (TSG) in Tuber Fleeceflower Root medicinal material in < < Chinese Pharmacopoeia > > 2010 editions, recording stilbene glucoside content in the Tuber Fleeceflower Root medicinal material using in the present invention is 3.6%, embodiment 1 prepares 2.1g toluylene glycoside product from 20g raw material medicinal extract I, extraction yield product purity to stilbene glucoside is measured, and concrete grammar is as follows:
(1) calculation formula of extraction yield is as follows:
(2) high-efficient liquid phase chromatogram condition of stilbene glucoside assay: take octadecyl silane as weighting agent, sample size 10 μ L, the acetonitrile-water (25: 75) of take is moving phase, detects wavelength 320nm, flow velocity 1mL/min.Theoretical plate number is calculated as 3745 by 2,3,5,4 '-tetrahydroxystilbene-2-O-β-D-Glucose glycosides peak.
Measurement result is as follows:
By above-mentioned experimental result, known, it is to extract solvent that the present invention adopts Diluted Alcohol, the method of stilbene glucoside in supersound extraction Tuber Fleeceflower Root, have, short, stilbene glucoside consuming time destroys the feature little, extraction yield is high, the stilbene glucoside content of pressing preparative chromatograph initial gross separation to obtain in warp is high, and further the stilbene glucoside product purity after recrystallization is up to 98.1%.The sharp separation preparation that technique that the present invention prepares stilbene glucoside is simple, can realize product, can be widely used in separation from Tuber Fleeceflower Root and prepare toluylene glycoside product, can effectively meet high purity sample preparation in conventional pharmacodynamic experiment research demand.
Claims (1)
1. from Tuber Fleeceflower Root, sharp separation is prepared the method for stilbene glucoside, it is characterized in that the concrete steps of described method are as follows:
(1) raw materials medicinal extract
The pharmaceutical decocting piece of Radix Polygoni Multiflori of take is raw material, take Diluted Alcohol as extracting solvent, first raw material being put into pulverizer pulverizes, and sieve through 50～100 object iron sieves, the raw material powder that collection is sieved, unsifted raw material is put into pulverizer again and is pulverized, then in the quality of raw material powder: the ratio of the volume of Diluted Alcohol is the ratio of 1g: 5～15mL, raw material powder art and Diluted Alcohol are positioned in supersound extraction device, first be uniformly mixed, at ultrasonic power, be 300～500W again, ultrasonic operating frequency is 30～60KHZ, temperature is under 50～70 ℃ of conditions, carry out for the first time after supersound extraction 0.5～1.5h, extracting solution is filtered for the first time, collect respectively primary filtrate and filter residue, the filter residue of collecting is for the first time positioned in supersound extraction device again, again in the quality of filter residue: the ratio of the volume of Diluted Alcohol is the ratio of 1g: 5～15mL, again filter residue and the Diluted Alcohol collected are for the first time placed in to supersound extraction device, first be uniformly mixed, at ultrasonic power, be 300～500W again, ultrasonic operating frequency is 30～60KHZ, temperature is under 50～70 ℃ of conditions, carry out for the second time after supersound extraction 0.5～1.5h, again extracting solution is filtered for the second time, collect respectively again filtrate and filter residue, so repeat 1～2 time, the filtrate that finally merges each collection, and the most latter incorporated filtrate is positioned over to Rotary Evaporators is evaporated to medicinal extract shape, just prepare raw material medicinal extract I, the filter residue of last collection be can be used for to continual exploitation utilization polysaccharide fraction wherein,
(2) raw material medicinal extract I degreasing
After (1) step completes, the quality (g) of the raw material medicinal extract I first preparing according to (1) step: the ratio of the volume of sherwood oil (mL) is 1: 5～10 ratio, raw material medicinal extract I and sherwood oil are added in water-bath refluxing extraction device, in the water-bath environment of 60～100 ℃, carry out for the first time after refluxing extraction 0.5～1.5h, filter for the first time, collect respectively filtrate, be petroleum ether solvent layer and filter residue, it is lotion, again according to the quality of the filter residue of collecting for the first time: the ratio of the volume of sherwood oil is the ratio of 1g: 5～10mL, filter residue and the sherwood oil collected are for the first time added in water-bath refluxing extraction device, again in the water-bath environment of 60～100 ℃ 0, carry out refluxing extraction 0.5～1.5h for the second time, filter for the second time again, collect respectively again filtrate and filter residue, so repeat 1～2 time, the filter residue of finally collecting, just make the raw material medicinal extract II after skimming treatment, the filtrate that finally merges each collection can be used for the preparation of the products such as Schuttgelb,
(3) prepare stilbene glucoside crude product
After (2) step completes, the quality of the raw material medicinal extract II first making according to (2) step: the ratio of the volume of pure water is the ratio of 1g: 5～10mL, raw material medicinal extract II and pure water are joined in container, be stirred to dissolving, just make sample III to be separated, centering presses preparative chromatograph to arrange again, adopt initial eluting solvent to carry out separator column balance, adjustment flow rate pump is 3～20mL/min, it is 0.5～2Mpa that post is pressed, after post pressure is stable, again sample III to be separated is positioned in middle pressure preparative chromatograph and is adsorbed after 0～10min, at separating column packing, be ODS or the SBC MCI GEL reverse phase filler of 50～70 μ m, eluting solvent is to carry out middle pressure chromatographic separation under A and two yuan of mixed solvent system conditions of B, wherein: solvent orange 2 A is water, solvent B is methyl alcohol or acetonitrile, solvent orange 2 A: the volume ratio of solvent B is 0-100, then under the detection wavelength of 320nm, collect out peak flow point, the peak flow point that goes out of collecting is positioned in Rotary Evaporators and is concentrated, just make stilbene glucoside crude product IV,
(4) prepare toluylene glycoside product
After (3) step completes, in the stilbene glucoside crude product IV making in step (3), add the pure water of 50～70 ℃, be stirred to dissolving, just be prepared into the hot saturated aqueous solution of described stilbene glucoside crude product IV, by millipore filtration, filter again, collect respectively filtrate and filter residue, then by filtrate standing 10～24h crystallization at 0～25 ℃, crystal just makes toluylene glycoside product V after vacuum lyophilization, and filter residue discharges after processing.
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Citations (3)
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| CN101560229A (en) * | 2008-04-17 | 2009-10-21 | 霸王（广州）有限公司 | Extracting method of stilbene glycoside of radix-polygoni multiflori extract |
| CN102731586A (en) * | 2011-04-01 | 2012-10-17 | 北京双鹭药业股份有限公司 | Preparation technology of stilbene glucoside in polygonum multiflorum |
| CN103242388A (en) * | 2013-05-15 | 2013-08-14 | 南京泽朗医药科技有限公司 | Method for preparing stibene glucoside from fleece-flower root |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101560229A (en) * | 2008-04-17 | 2009-10-21 | 霸王（广州）有限公司 | Extracting method of stilbene glycoside of radix-polygoni multiflori extract |
| CN102731586A (en) * | 2011-04-01 | 2012-10-17 | 北京双鹭药业股份有限公司 | Preparation technology of stilbene glucoside in polygonum multiflorum |
| CN103242388A (en) * | 2013-05-15 | 2013-08-14 | 南京泽朗医药科技有限公司 | Method for preparing stibene glucoside from fleece-flower root |
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