CN1323776A - Prepn. of resveratrol and resveratrol glycoside - Google Patents
Prepn. of resveratrol and resveratrol glycoside Download PDFInfo
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- CN1323776A CN1323776A CN 01118461 CN01118461A CN1323776A CN 1323776 A CN1323776 A CN 1323776A CN 01118461 CN01118461 CN 01118461 CN 01118461 A CN01118461 A CN 01118461A CN 1323776 A CN1323776 A CN 1323776A
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Abstract
The present invention relates to method of separating and preparing high purity veralkol and veralkol glycoside from plants, animals, microbes, it is characterized in that column chromatography and high speed countercurrent chromatography are combined together to form a new technological process, it is simple in operation, the purity of product can reach higher than 99.0%.
Description
The present invention relates to a kind of method of from natural phant, separating preparation highly purified trans-resveratrol (resveratrol) and polidatin (piceid).
At present, in many natural phant, found the existence of trans-resveratrol and polidatin.As: the Vitis of Vitaceae, Ampelopsis, the Arachis of pulse family, Cassia, Sophora, liliaceous Veratrum, the eucalyptus of ma Yao Jin section belongs to, the Polygonum of polygonaceae etc.Wherein, many plants are common medicinal plants, as Cassia tora, black false hellebore, giant knotweed etc.; The then edible that has is as grape.Trans-resveratrol and the highest plant of trans-resveratrol salidroside content are giant knotweeds in the plant of finding at present.
Trans-resveratrol, promptly 3,4 ', 5-trihydroxy-toluylene has cis and trans two kinds of isomer, exists with stable trans forms usually in the natural phant.Polidatin claims Polydatin, piceid again, promptly 3,4 ', and 5-trihydroxy-toluylene-3-β-list-D glycoside exists with stable trans forms in the natural phant usually.
Pharmacological research shows: trans-resveratrol is influential to lipid metabolism and platelet aggregation, can prevent diseases such as coronary heart disease, atherosclerosis.(1) to the influence of lipid metabolism: the eighties, when separating the trans-resveratrol that obtains to the influencing of lipid metabolism from giant knotweed, research finds that the rabbit of fatty liver and hyperlipidemia is taken trans-resveratrol can suppress triglyceride and the total cholesterol deposition at liver; The mouse of intravenous injection trans-resveratrol, its liver by
14The fat that C-Palmiticacid forms significantly reduces, and trans-resveratrol also has concentration, the ratio of regulating low-density lipoprotein (LDL) that increases blood middle-high density lipoprotein (HDL), the effects such as oxidation that stop LDL simultaneously.(2) anti-platelet aggregation: platelet aggregation is caused by multiple stimulating factor, one of them mechanism is that arachidonic acid metabolism primary product thromboxane causes platelet aggregation, trans-resveratrol can suppress the formation of arachidonic acid metabolite, thereby VITAMIN B4 is examined the platelet aggregation that sweet bisphosphate (ADP), zymoplasm and collagen causes restraining effect is arranged.The chemical prevention of cancer is to reduce cancer morbidity and mortality ratio one of the most direct method at present.For seeking new anticarcinogen, people are index with the inhibition to cyclooxygenase (COX), hundreds of plant milk extracts have been screened, from the methanol extract of five jiaos of Cassia tora roots of leguminous plants of Peru, get its activeconstituents trans-resveratrol at last, three main phase of initial, the propagation of cancer, development are all had suppress and even reverse effect: suppress the initial of cancer by anti-oxidant and antimutagenic effect; By suppressing the propagation that cyclooxygenase (COX) and lipoxygenase (LOX) suppress cancer; Trans-resveratrol can be induced the differentiation of human promyelocytic leukemia cell, thereby has suppressed the development of cancer.Therefore, trans-resveratrol is listed in and suppresses and one of the most promising medicine of treatment cancer.Use another anticancer index--albumen-Tyrosylprotein kinase (PTK) activity that suppresses ox thymus gland is studied, and also gets the activeconstituents trans-resveratrol from the methanol extract of giant knotweed.Nearest research finds that again trans-resveratrol is by suppressing the transfer that the proteic expression of p53 suppresses tumour cell.Trans-resveratrol has anti-oxidant, anti-radical action: can obviously suppress the erythrocytic autoxidation haemolysis of rat and by H
2O
2The oxidation haemolysis that causes; To the generation of the inside and outside lipid peroxide of mouse core, liver, brain, kidney by obvious restraining effect; Can reduce the lipid peroxide content of cerebral tissue, reduce brain water content, alleviate the infringement of free radical reaction, the cerebral tissue of ischemic is had provide protection cerebral tissue.To gi tract H
+-K
+The effect of-ATP enzyme: gi tract H
+-K
+-ATP enzyme is the relevant ionic pump of a kind of and sour secretion, plays an important role in the final step of gastric acid secretion, and this kind of enzyme is a kind of important target of treatment stomach ulcer.Trans-resveratrol is as a kind of optionally gi tract H
+-K
+-atpase inhibitor might have purposes in the treatment of stomach ulcer.Anti-microbial effect: trans-resveratrol is made the plant antimicrobial that the time spent produces and is that the people is familiar with at unfavourable condition such as being subjected to fungi infestation, uviolizing as a kind of grape class plant at first.Find that trans-resveratrol has anti-grey mold, pathogenic bacteria, streptococcus aureus, staphylococcus epidermidis mycobacterium isoreactivity.To neural effect: the trans-resveratrol of lower concentration can be induced the phosphorylation that born of the same parents regulate kinases 1 (ERK1) kinases 2 (ERK2) outward in the human body neuroblastoma SH-SY5 cell, and ERK1 and ERK2 belong to cell fission activated protein (MAP) kinases.Map kinase is relevant with cell transduction, and especially the phosphorylation of ERK2 and memory and learning process interrelate.By taking in trans-resveratrol,, prevention and therapeutic action are preferably all arranged as parkinsonism, dementia, degenerative brain disorder, rheumatism etc. for the elderly's degenerative disease.Aspect makeup, the effect that trans-resveratrol has eliminating chloasma and brightens.The character of polidatin is stable than trans-resveratrol, and it can be decomposed into trans-resveratrol in human body, thereby plays the pharmacological action identical with trans-resveratrol.
At present, the method that the silica gel column chromatography of multistep combines with high performance liquid chromatography is mainly adopted in the extraction of trans-resveratrol and glucoside thereof in the plant, operate often more loaded down with trivial details because solid state adhesion body or carrier to absorption, the sex change of sample, cause the purity of product and the rate of recovery lower.High speed adverse current chromatogram (High-speed CountercurrentChromatography, HSCCC) be a kind of successive of growing up in nearly 30 years need not the solid support thing efficiently, liquid liquid distribution chromatography isolation technique fast, have characteristics such as fractional dose is big, sample free of losses, rate of recovery height, isolating environment mitigation, saving solvent, bibliographical information is arranged direct employing high speed adverse current chromatogram separate and obtain trans-resveratrol and polidatin, but, cause efficient lower owing to the content of trans-resveratrol in the sample and polidatin is too low.
The objective of the invention is column chromatogram chromatography and high speed adverse current chromatogram are combined, give full play to their advantages separately, develop a kind of purity and all higher operational path of the rate of recovery of easy and simple to handle, product.
Basic technology route of the present invention is: (1) at first contains plant, animal, the microorganism of trans-resveratrol and polidatin with the organic solvent lixiviate, obtain its extract, (2) the more extract obtained column chromatogram chromatography that carries out is obtained purity and is higher than 90% trans-resveratrol and purity and is higher than 70% polidatin product, (3) obtain purity with its product with the high speed adverse current chromatogram partition method and are higher than 99% trans-resveratrol and polidatin product.
The stationary phase that column chromatogram chromatography adopts is silica gel (granularity is the 10-500 order); The binary liquid mixture of the optional different ratios of moving phase: the A component can be selected from halohydrocarbon such as chloroform, methylene dichloride, tetracol phenixin; The B component can be selected from Fatty Alcohol(C12-C14 and C12-C18) or aliphatic ketones such as methyl alcohol, ethanol, propyl alcohol, acetone, preferred chloroform-methanol system.The volume ratio of A and B is 1-100: 1-2.
The high speed adverse current chromatogram of trans-resveratrol separates available solvent system and mainly contains three.All is stationary phase mutually, is moving phase mutually down.No. one solvent system is made of three components, the A component can be selected from halohydrocarbon such as chloroform, methylene dichloride, tetracol phenixin, the B component can be selected from Fatty Alcohol(C12-C14 and C12-C18) or aliphatic ketones such as methyl alcohol, ethanol, propyl alcohol, acetone, the C component is a water, preferred chloroform-methanol-aqueous systems, the volume ratio of A, B, C is 2-6: 2-5: 1-3.No. two solvent system is made of four components, the A component can be selected from halohydrocarbon such as chloroform, methylene dichloride, tetracol phenixin, the B component can be selected from alkane or ethers such as normal hexane, sherwood oil, hexanaphthene, the C component can be selected from Fatty Alcohol(C12-C14 and C12-C18) or aliphatic ketones such as methyl alcohol, ethanol, propyl alcohol, acetone, the D component is a water, preferred methylene dichloride-normal hexane-methanol-water system, the volume ratio of A, B, C, D is 2-5: 0.5-2: 2-5: 1-3.No. three solvent system is made of five components, A, C component can be selected from halohydrocarbon such as chloroform, methylene dichloride, tetracol phenixin, the B component can be selected from alkane or ethers such as normal hexane, sherwood oil, hexanaphthene, the D component can be selected from Fatty Alcohol(C12-C14 and C12-C18) or aliphatic ketones such as methyl alcohol, ethanol, propyl alcohol, acetone, the E component is a water, preferred tetracol phenixin-normal hexane-methylene chloride-methanol-aqueous systems, the volume ratio of A, B, C, D, E is 0.5-2: 0.5-2: 0.5-3: 2-5: 1-3.
The high speed adverse current chromatogram of polidatin separates available solvent system and mainly contains three.All is stationary phase mutually, is moving phase mutually down.No. one solvent system is made of three components, the A component can be selected from fatty ester classes such as ethyl acetate, propyl acetate, isopropyl acetate, n-butyl acetate, the B component can be selected from Fatty Alcohol(C12-C14 and C12-C18) or aliphatic ketones such as methyl alcohol, ethanol, propyl alcohol, acetone, the C component is a water, ethyl acetate-ethanol-water system, the volume ratio of A, B, C are 10-100: 0.5-2: 10-100.No. two solvent system also is made of three components, the A component can be selected from fatty ester classes such as ethyl acetate, propyl acetate, isopropyl acetate, n-butyl acetate, the B component can be selected from alkane or ethers such as normal hexane, sherwood oil, hexanaphthene, the C component is a water, ethyl acetate-normal hexane-aqueous systems, the volume ratio of A, B, C are 10-100: 0.5-2: 10-100.No. three solvent system is made of fatty ester and two components of water, ethyl acetate and water, and its volume ratio is 0.5-2: 0.5-2.
It is to carry out under 15 ℃-30 ℃ that experiment is suitable in room temperature.
Because trans-resveratrol and polidatin see that light is easily oxidized and decompose that all extraction operations and subsequent measurements work all will be carried out under strict lucifuge condition.Product should seal and be kept at lucifuge, in the environment of low temperature (below 0 ℃).
The method for preparing trans-resveratrol and polidatin of the present invention is that column chromatogram chromatography and high speed adverse current chromatogram are combined, give full play to their advantages separately, develop a kind of purity and all higher operational path of the rate of recovery of easy and simple to handle, product, the purity of its product can reach more than 99.0%.Present method is suitable for extracting trans-resveratrol and polidatin from all contain the plant, animal, microorganism of trans-resveratrol and polidatin, also is suitable for from through preparation trans-resveratrol and polidatin the plant of organic solvent lixiviate, animal, the microorganism extracts.
Embodiment 1
Separation and Extraction purity all is higher than 99% trans-resveratrol and polidatin from Rhizoma Polygoni Cuspidati extract: with silicagel column the 2g Rhizoma Polygoni Cuspidati extract is separated, wherein the content of trans-resveratrol is 9.67%, the content of polidatin is 17.73%, eluent is the ever-increasing chloroform-methanol solution of methanol content, the volume ratio of chloroform and methyl alcohol was respectively 20: 1,15: 1,10: 1,5: 1, substep is collected, the solvent that will contain trans-resveratrol and polidatin is evaporated to dried, purity is 95.64% trans-resveratrol 160.5mg, purity is 79.47% polidatin 380.5mg.Prepare high-purity resveratrol and polidatin with high speed adverse current chromatogram respectively again--adopt half countercurrent chromatography instrument, is furnished with the NS-1007 pump, the 20ml sampling valve, the tetrafluoroethylene post, column volume is 240ml, the 8823A-UV UV-detector, Yokogawa3057 potable recording instrument, FC-95 automatic fraction collector.Before the sample introduction, be full of whole pillar with stationary phase earlier, the adjustment engine speed is 800rpm, flow velocity with 2.0ml/min pumps into moving phase in the post, treat that whole system is set up running balance after, by the sampling valve sample introduction, then according to the detector uv atlas, the receiving target composition.The chromatographic condition of this two kinds of materials preparation is respectively: (1) is that chloroform-methanol-water of 4: 3: 2 is miscible in separating funnel with volume ratio, shakes up the back standing demix, gets its upper solution (going up phase) and is stationary phase, and lower floor's solution (following phase) is moving phase.Upper and lower phase mixed solution 20ml dissolving trans-resveratrol sample with 1: 1 separates.Obtain white trans-resveratrol product 149.5mg, analyze through HPLC, its purity is 99.52%.(2) be that 100: 1: 100 ethyl acetate, alcohol and water is miscible in separating funnel with volume ratio, shake up the back standing demix, get its upper solution (going up phase) and be stationary phase, lower floor's solution (following phase) is moving phase.With phased soln polidatin sample under the 40ml at twice sample introduction separate.Obtain faint yellow polidatin product 293.3mg altogether, analyze through HPLC, its purity is 99.41%.
Embodiment 2
Separation and Extraction purity all is higher than 99% trans-resveratrol and polidatin from natural giant knotweed: the 100g giant knotweed soaked 15 days with 500ml methyl alcohol, filter, the concentrating under reduced pressure methanol extract liquid, obtain 38.98g medicinal extract, wherein the content of trans-resveratrol is about 0.773%, the content of polidatin is about 5.37%, with silicagel column this medicinal extract of 10g is separated, and eluent is a dichloromethane-ethanol, volume ratio was respectively 20: 1,15: 1,10: 1,5: 1, substep is collected, the solvent that will contain trans-resveratrol and polidatin is evaporated to dried, purity is 96.10% trans-resveratrol 68.2mg, purity is 75.02% polidatin 608.4mg.Prepare high-purity resveratrol and polidatin with high speed adverse current chromatogram respectively again--adopt half countercurrent chromatography instrument, is furnished with the NS-1007 pump, the 20ml sampling valve, the tetrafluoroethylene post, column volume is 240ml, the 8823A-UV UV-detector, Yokogawa3057 potable recording instrument, FC-95 automatic fraction collector.Before the sample introduction, be full of whole pillar with stationary phase earlier, the adjustment engine speed is 800rpm, flow velocity with 2.0ml/min pumps into moving phase in the post, treat that whole system is set up running balance after, by the sampling valve sample introduction, then according to the detector uv atlas, the receiving target composition.The chromatographic condition of these two kinds of material preparations is respectively: (1) is 3: 1: 3 with volume ratio: methylene dichloride-normal hexane of 2-methanol-water is miscible in separating funnel, shake up the back standing demix, get its upper solution (going up phase) and be stationary phase, lower floor's solution (following phase) is moving phase.Upper and lower phase mixed solution 20ml dissolving trans-resveratrol sample with 1: 1 separates.Obtain white trans-resveratrol product 64.4mg, analyze through HPLC, its purity is 99.89%.(2) be that propyl acetate-hexanaphthene-water of 70: 1: 70 is miscible in separating funnel with volume ratio, shake up the back standing demix, get its upper solution (going up phase) and be stationary phase, lower floor's solution (following phase) is moving phase.Divide 3 sample introductions to separate with phased soln polidatin sample under the 60ml.Obtain faint yellow polidatin product 442.7mg altogether, analyze through HPLC, its purity is 99.01%.Embodiment 3
Separation and Extraction purity all is higher than 99% trans-resveratrol and polidatin from natural giant knotweed: the 100g giant knotweed soaked 15 days with 500ml methyl alcohol, filter, the concentrating under reduced pressure methanol extract liquid, obtain 38.98g medicinal extract, wherein the content of trans-resveratrol is about 0.773%, the content of polidatin is about 5.37%, with silicagel column this medicinal extract of 10g is separated, and eluent is tetracol phenixin-propyl alcohol, volume ratio was respectively 15: 1,10: 1,6: 1,4: 1, substep is collected, the solvent that will contain trans-resveratrol and polidatin is evaporated to dried, purity is 95.48% trans-resveratrol 70.03mg, purity is 73.08% polidatin 585.3mg.Prepare high-purity resveratrol and polidatin with high speed adverse current chromatogram respectively again--adopt half countercurrent chromatography instrument, is furnished with the NS-1007 pump, the 20ml sampling valve, the tetrafluoroethylene post, column volume is 240ml, the 8823A-UV UV-detector, Yokogawa3057 potable recording instrument, FC-95 automatic fraction collector.Before the sample introduction, be full of whole pillar with stationary phase earlier, the adjustment engine speed is 800rpm, flow velocity with 2.0ml/min pumps into moving phase in the post, treat that whole system is set up running balance after, by the sampling valve sample introduction, then according to the detector uv atlas, the receiving target composition.The chromatographic condition of these two kinds of material preparations is respectively: (1) is 2: 1: 1 with volume ratio: tetracol phenixin-normal hexane of 3: 2-methylene chloride-methanol-water is miscible in separating funnel, shake up the back standing demix, get its upper solution (going up phase) and be stationary phase, lower floor's solution (following phase) is moving phase.Upper and lower phase mixed solution 20ml dissolving trans-resveratrol sample with 1: 1 separates.Obtain white trans-resveratrol product 64.0mg, analyze through HPLC, its purity is 99.80%.(2) be that ethyl acetate-water of 1: 1 is miscible in separating funnel with volume ratio, shake up the back standing demix, get its upper solution (going up phase) and be stationary phase, lower floor's solution (following phase) is moving phase.Divide 3 sample introductions to separate with phased soln polidatin sample under the 60ml.Obtain faint yellow polidatin product 431.2mg altogether, analyze through HPLC, its purity is 99.12%.
Embodiment 4
Separation and Extraction purity all is higher than 99% trans-resveratrol and polidatin from natural giant knotweed: the 100g giant knotweed soaked 15 days with 500ml methyl alcohol, filter, the concentrating under reduced pressure methanol extract liquid, obtain 38.98g medicinal extract, wherein the content of trans-resveratrol is about 0.773%, the content of polidatin is about 5.37%, with silicagel column this medicinal extract of 10g is separated, and eluent is methylene dichloride-acetone, volume ratio was respectively 30: 1,20: 1,15: 1,8: 1, substep is collected, the solvent that will contain trans-resveratrol and polidatin is evaporated to dried, purity is 93.20% trans-resveratrol 72.0mg, purity is 72.03% polidatin 610.5mg.Prepare high-purity resveratrol and polidatin with high speed adverse current chromatogram respectively again--adopt half countercurrent chromatography instrument, is furnished with the NS-1007 pump, the 20ml sampling valve, the tetrafluoroethylene post, column volume is 240ml, the 8823A-UV UV-detector, Yokogawa3057 potable recording instrument, FC-95 automatic fraction collector.Before the sample introduction, be full of whole pillar with stationary phase earlier, the adjustment engine speed is 800rpm, flow velocity with 2.0ml/min pumps into moving phase in the post, treat that whole system is set up running balance after, by the sampling valve sample introduction, then according to the detector uv atlas, the receiving target composition.The chromatographic condition of these two kinds of material preparations is respectively: (1) is 3.5: 0.5: 3.5 with volume ratio: methylene dichloride-hexanaphthene of 2-alcohol-water is miscible in separating funnel, shake up the back standing demix, get its upper solution (going up phase) and be stationary phase, lower floor's solution (following phase) is moving phase.Upper and lower phase mixed solution 20ml dissolving trans-resveratrol sample with 1: 1 separates.Obtain white trans-resveratrol product 63.50mg, analyze through HPLC, its purity is 99.77%.(2) be that propyl acetate-normal hexane-water of 60: 1: 50 is miscible in separating funnel with volume ratio, shake up the back standing demix, get its upper solution (going up phase) and be stationary phase, lower floor's solution (following phase) is moving phase.Divide 3 sample introductions to separate with phased soln polidatin sample under the 60ml.Obtain faint yellow polidatin product 439.2mg altogether, analyze through HPLC, its purity is 99.23%.
Embodiment 5
Separation and Extraction purity all is higher than 99% trans-resveratrol and polidatin from peanut skin: the 100g peanut skin soaked 15 days with 500ml methyl alcohol, filter, the concentrating under reduced pressure methanol extract liquid, obtain 25.38g medicinal extract, wherein the content of trans-resveratrol is about 0.34%, the content of polidatin is about 0.58%, with silicagel column this medicinal extract is separated, and eluent is a dichloromethane-ethanol, volume ratio was respectively 18: 1,12: 1,8: 1,4: 1, substep is collected, the solvent that will contain trans-resveratrol and polidatin is evaporated to dried, purity is 93.02% trans-resveratrol 78.85mg, purity is 70.02% polidatin 184.74mg.Prepare high-purity resveratrol and polidatin with high speed adverse current chromatogram respectively again--adopt half countercurrent chromatography instrument, is furnished with the NS-1007 pump, the 20ml sampling valve, the tetrafluoroethylene post, column volume is 240ml, the 8823A-UV UV-detector, Yokogawa3057 potable recording instrument, FC-95 automatic fraction collector.Before the sample introduction, be full of whole pillar with stationary phase earlier, the adjustment engine speed is 800rpm, flow velocity with 2.0ml/min pumps into moving phase in the post, treat that whole system is set up running balance after, by the sampling valve sample introduction, then according to the detector uv atlas, the receiving target composition.The chromatographic condition of this two kinds of materials preparation is respectively: (1) is that methylene chloride-methanol-water of 4: 3: 2 is miscible in separating funnel with volume ratio, shakes up the back standing demix, gets its upper solution (going up phase) and is stationary phase, and lower floor's solution (following phase) is moving phase.Upper and lower phase mixed solution 20ml dissolving trans-resveratrol sample with 1: 1 separates.Obtain white trans-resveratrol product 73.20mg, analyze through HPLC, its purity is 99.90%.(2) be that isopropyl acetate-propyl alcohol-water of 70: 1: 70 is miscible in separating funnel with volume ratio, shake up the back standing demix, get its upper solution (going up phase) and be stationary phase, lower floor's solution (following phase) is moving phase.Divide 1 sample introduction to separate with phased soln polidatin sample under the 20ml.Obtain faint yellow polidatin product 128.36mg altogether, analyze through HPLC, its purity is 99.08%.
Claims (9)
1. the preparation method of trans-resveratrol and polidatin, it is characterized in that: basic technology route of the present invention is:
(1) at first contain plant, animal, the microorganism of trans-resveratrol and polidatin, obtain its extract with the organic solvent lixiviate,
(2) the more extract obtained column chromatogram chromatography that carries out is obtained purity and is higher than 90% trans-resveratrol and purity and is higher than 70% polidatin product,
(3) its product is obtained purity with the high speed adverse current chromatogram partition method and be higher than 99% trans-resveratrol and polidatin product;
2. the preparation method of a kind of trans-resveratrol according to claim 1 and polidatin is characterized in that: column chromatogram chromatography moving phase can be selected halohydrocarbon and Fatty Alcohol(C12-C14 and C12-C18) or alkenolic mixed solution, and volume ratio is 1-100: 1-2;
3. the preparation method of a kind of trans-resveratrol according to claim 1 and polidatin, it is characterized in that: it is chloroform, methylene dichloride, tetracol phenixin that column chromatogram chromatography moving phase can be selected halohydrocarbon, and Fatty Alcohol(C12-C14 and C12-C18) or aliphatic ketone are methyl alcohol, ethanol, propyl alcohol, acetone;
4. the preparation method of a kind of trans-resveratrol according to claim 1 and polidatin, it is characterized in that: the available solvent system of high speed adverse current chromatogram partition method of trans-resveratrol is: be made of three components, halohydrocarbon such as the optional chloroform of component, methylene dichloride, tetracol phenixin, Fatty Alcohol(C12-C14 and C12-C18) or aliphatic ketones such as methyl alcohol, ethanol, propyl alcohol, acetone, water, volume ratio is 2-6: 2-5: 1-3 successively;
5. the preparation method of a kind of trans-resveratrol according to claim 1 and polidatin, it is characterized in that: the available solvent system of high speed adverse current chromatogram partition method of trans-resveratrol is: be made of four components, halohydrocarbon such as the optional chloroform of component, methylene dichloride, tetracol phenixin, alkane or ethers such as normal hexane, sherwood oil, hexanaphthene, Fatty Alcohol(C12-C14 and C12-C18) or aliphatic ketones such as methyl alcohol, ethanol, propyl alcohol, acetone, water, preferred methylene dichloride-normal hexane-methanol-water, volume ratio is 2-5: 0.5-2: 2-5: 1-3;
6. the preparation method of a kind of trans-resveratrol according to claim 1 and polidatin, it is characterized in that: the available solvent system of high speed adverse current chromatogram partition method of trans-resveratrol is: be made of five components, halohydrocarbon such as the optional chloroform of component, methylene dichloride, tetracol phenixin, alkane or ethers such as normal hexane, sherwood oil, hexanaphthene, halohydrocarbon such as chloroform, methylene dichloride, tetracol phenixin, Fatty Alcohol(C12-C14 and C12-C18) or aliphatic ketones such as methyl alcohol, ethanol, propyl alcohol, acetone, water, volume ratio is 0.5-2: 0.5-2: 0.5-3: 2-5: 1-3 successively;
7. the preparation method of a kind of trans-resveratrol according to claim 1 and polidatin, it is characterized in that: the high speed adverse current chromatogram of polidatin separates available solvent system and is made of three components, fatty ester classes such as the optional ethyl acetate of component, propyl acetate, isopropyl acetate, n-butyl acetate, Fatty Alcohol(C12-C14 and C12-C18) or aliphatic ketones such as methyl alcohol, ethanol, propyl alcohol, acetone, water, volume ratio is 10-100: 0.5-2: 10-100 successively;
8. the preparation method of a kind of trans-resveratrol according to claim 1 and polidatin, it is characterized in that: the high speed adverse current chromatogram of polidatin separates available solvent system and is made of three components, fatty ester classes such as the optional ethyl acetate of component, propyl acetate, isopropyl acetate, n-butyl acetate, alkane or ethers such as normal hexane, sherwood oil, hexanaphthene, water, volume ratio is 10-100: 0.5-2: 10-100 successively;
9. the preparation method of a kind of trans-resveratrol according to claim 1 and polidatin, it is characterized in that: the high speed adverse current chromatogram of polidatin separates available solvent system and is made of fatty ester and two components of water, and its volume ratio is 0.5-2: 0.5-2.
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| CN103524594A (en) * | 2013-10-16 | 2014-01-22 | 中国药科大学 | Method for separating cyclopamine analogs from Veratrum plants by high-speed counter-current chromatography |
| CN103570776A (en) * | 2013-11-01 | 2014-02-12 | 湖南科源生物制品有限公司 | Refining method for extracting and separating polydatin |
| CN103755752A (en) * | 2013-12-28 | 2014-04-30 | 湘西自治州奥瑞克医药化工有限责任公司 | Production technology for extracting and purifying polydatin from polygonum cuspidatum |
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2001
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| US7393542B2 (en) | 2001-08-31 | 2008-07-01 | Akio Yoshihara | Remedies for allergic diseases using processed peanut seed coat |
| CN1935195B (en) * | 2005-09-21 | 2010-04-28 | 中国科学院大连化学物理研究所 | Method for extracting female sex hormone from polygonum cuspidatum |
| CN100434135C (en) * | 2005-09-23 | 2008-11-19 | 中国科学院过程工程研究所 | Method for separating and purifying natural product using three-phase counter current chromatograph |
| CN1948274B (en) * | 2006-10-25 | 2012-10-17 | 沈阳药科大学 | Verakanol derivative, preparation method and use thereof |
| CN101411716B (en) * | 2008-07-08 | 2011-05-04 | 中国人民解放军第二军医大学 | Use of polygonin for preparing product for resisting dementia |
| CN102070594B (en) * | 2009-11-24 | 2013-08-21 | 上海中药制药技术有限公司 | Separation preparation method for high-purity agarotetrol and 4'-methoxy agarotetrol |
| CN103524594A (en) * | 2013-10-16 | 2014-01-22 | 中国药科大学 | Method for separating cyclopamine analogs from Veratrum plants by high-speed counter-current chromatography |
| CN103524594B (en) * | 2013-10-16 | 2015-04-22 | 中国药科大学 | Method for separating cyclopamine analogs from Veratrum plants by high-speed counter-current chromatography |
| CN103570776A (en) * | 2013-11-01 | 2014-02-12 | 湖南科源生物制品有限公司 | Refining method for extracting and separating polydatin |
| CN103755752A (en) * | 2013-12-28 | 2014-04-30 | 湘西自治州奥瑞克医药化工有限责任公司 | Production technology for extracting and purifying polydatin from polygonum cuspidatum |
| CN103755752B (en) * | 2013-12-28 | 2016-04-06 | 湘西自治州奥瑞克医药化工有限责任公司 | A kind of production technique of extraction purification polygonin from giant knotweed |
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