CN1450077A - Method for extracting polygonum cuspidatum tannic acid - Google Patents
Method for extracting polygonum cuspidatum tannic acid Download PDFInfo
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- CN1450077A CN1450077A CN 03116545 CN03116545A CN1450077A CN 1450077 A CN1450077 A CN 1450077A CN 03116545 CN03116545 CN 03116545 CN 03116545 A CN03116545 A CN 03116545A CN 1450077 A CN1450077 A CN 1450077A
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- tannic acid
- giant knotweed
- water
- ethyl acetate
- filtrate
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Abstract
The present invention relates to an extraction method of Chinese medicinal material polygonum cuspidatum extract-polygonum cuspidatum tannin. The polygonum cuspidatum tannin as main component of polygoum cuspidatum extract has alpha-glycosidase inhibiting activity, can be used as main active component for preparing medicine for reducing blood sugar, also can be used as raw material for preparing medicine for curing diabetes and obesity. Its extraction method in cludes the following steps: pulverizing raw material, using water and methyl alcohol or water-containing alcohol to make extraction under the condition of heating, filtering, using petroleum ether to degrease the filtrate, using active carbon to decolour, the concentrating at normal pressure or reduced pressure, making the concentrated filtrate pass through ion exchange resin.
Description
Technical field
The present invention relates to the extracting method of crude drug Rhizoma Polygoni Cuspidati extract giant knotweed tannic acid, belong to the herbal medicine chemistry and refine preparing technical field.
Background technology
Medicinal giant knotweed is the polygonaceae arsesmart, and medicinal part is a rhizome.Main chemical compositions is very wide a lot, has: Schuttgelb, chrysophanol, glycoside, polidatin, glucosides class, amino acid, trace element etc., and be rich in condensed tannin and saccharan.
Tannin in the Rhizoma Polygoni Cuspidati extract or tannic acid are the diabetes alpha-glucoside inhibiting activity, so can be used as hypoglycemic drug.
Summary of the invention
The purpose of this invention is to provide a kind of Rhizoma Polygoni Cuspidati extract with alpha-glucoside inhibiting activity, its significant part is the water-soluble giant knotweed tannic acid with good hypoglycemic activity.
Another object of the present invention provides a kind of preparation technology's method of Rhizoma Polygoni Cuspidati extract.
Above-mentioned purpose of the present invention reaches by the following technical programs.
The extracting method of a kind of Rhizoma Polygoni Cuspidati extract giant knotweed tannic acid of the present invention is characterized in that, this method comprises following processing step:
A. the crude drug giant knotweed is through after pulverizing, and water, methyl alcohol or aqueous alcohol are extracted under heating condition, during extraction
Between 2-30 hour, solvent load be crude drug 3-10 doubly;
B. filter or centrifugation, abandon filter residue, get filtrate or supernatant liquid, with filtrate or supernatant liquid in temperature
50-100 ℃ is incubated 5-30 minute, and refrigerator is placed and spent the night;
C. put into separating centrifuge,, get supernatant liquid 2000-5000rmp centrifugation 5-20 minute;
D. supernatant liquid is used petroleum ether degreasing 2-5 time in separatory funnel;
E. with the extracting solution activated carbon decolorizing after the degreasing, low molecular weight impurities is removed in ultrafiltration then;
F. gained filtrate is gone up storng-acid cation exchange resin, use the distilled water wash-out then, elutriant is regulated it
PH is heated to 60-100 ℃ and concentrates to neutrality under normal pressure or decompression, use ultra-filtration membrane then
Carry out ultrafiltration, can obtain the brown solid powder after drying, its main component is the giant knotweed tannic acid.
The extracting method of another kind of Rhizoma Polygoni Cuspidati extract giant knotweed tannic acid of the present invention is characterized in that, this method comprises following processing step:
A. with crude drug giant knotweed elder generation water, ethanol or aqueous alcohol are soaked, and macerate the back and pulverize with stamp mill, at heater strip
Under the part, extracted 2-30 hour, solvent load is 3-10 a times of crude drug;
B. filter, abandon filter residue, get filtrate and under normal pressure or decompression, be heated to 50-100 ℃, concentrate medicinal extract;
C. be dissolved in water, use the chloroform reflux, abandon chloroform layer, ethyl acetate extraction 2-3 time of gained water layer,
Get ethyl acetate layer, use NaOH aqueous solution extraction 2-3 time again, get the NaOH aqueous solution, transfer PH with HCl
Be worth to 2-6, add the 4-10% aqueous gelatin solution, get throw out;
D. precipitation is used the whizzer centrifugation then with the dissolving of 30-70% aqueous acetone solution, abandons precipitation, and it is molten to get acetone
Liquid concentrates its underpressure distillation, and reclaims acetone, obtains the colloidal solid thing;
E. with gained colloidal solid thing water dissolution, use ethyl acetate extraction again, the decompression of gained ethyl acetate layer is dense
Contract, and reclaim ethyl acetate, obtain spissated jelly;
F. jelly adds the suitable quantity of water dissolving, filters, and elimination precipitation insolubles obtains clear liquid, with the clear liquid lyophilize
Get orange-yellow powder, its main component is the giant knotweed tannic acid.
The prepared giant knotweed tannic acid of the inventive method, has alpha-glucoside inhibiting activity, its mechanism of action be the giant knotweed tannic acid by with digestive tube in many enzyme effects, particularly to the inhibition activity of alpha-glycosidase, thereby regulated and control the absorption of body to nutritive ingredients such as glucose, make it have anti-trophicity, for the diabetic subject of obesity, the giant knotweed tannic acid is lowering blood glucose effectively not only, and can reduce its absorption to nutritive ingredient, so the giant knotweed tannic acid can be used as glycosidase inhibitor class medicine, also can be used as the main component of diet tea.
The extraction process of the inventive method, use equipment is simple, and separation and Extraction is operated easily, and cost is also lower.
Prepared product giant knotweed tannic acid of the present invention can reduce the blood plasma blood sugar concentration as inhibitor.
Below test is the hypoglycemic activity of giant knotweed tannic acid inhibitor to the animal mouse.
Test 1, giant knotweed tannic acid inhibitor single administration are to the influence of normal mouse's blood sugar content: 45 of mouse, be divided into 5 groups at random, and irritate stomach physiological saline, glucobay (acarbose) (100mg/kg), tannic acid inhibitor (50mg/kg, 100mg/kg, 150mg/kg) respectively.Hematometry blood plasma blood sugar concentration is got in docking behind the fasting 3h.The result shows 100, and 150mg/kg dosage all can obviously reduce normal mouse blood sugar (seeing Table 1).
Table 1 inhibitor single administration is to the influence of normal mouse's blood sugar content
| Group | ????n | Dosage (mg/kg) | Blood glucose value (mmol/L) |
| Physiological saline | ????10 | ????- | ????7.80±0.48 |
| Glucobay (acarbose) | ????10 | ????100 | ????6.31±0.50 2 |
| Inhibitor | ????8 ????8 ????9 | ????50 ????100 ????150 | ????7.22±1.11 1????5.50±0.49 2????4.54±0.69 2 |
Compare with the physiological saline group:
1P＜0.005,
2P＜0.001
Above-mentioned glucobay (acarbose) contrast agents is Bayer A.G's product.
Test 2, the administration of giant knotweed tannic acid inhibitor continuous several times are to the influence of normal mouse's blood sugar content: 30 of mouse, be divided into 3 groups at random, and irritate stomach physiological saline, glucobay (acarbose) (100mg/kg), giant knotweed tannic acid inhibitor (100mg/kg) respectively, continuous eight days.Fasting 3h after the last administration measures blood sugar concentration.As seen, the mouse multiple dosing causes the reduction (seeing Table 2) of mouse blood sugar equally.
The administration of table 2 inhibitor continuous several times is to the influence of normal mouse's blood sugar content
| Group | ????n | Blood glucose value (mmol/L) |
| Physiological saline | ????10 | ?????6.30±0.89 |
| Glucobay (acarbose) | ????10 | ?????5.41±0.31 1 |
| Inhibitor | ????10 | ?????4.98±0.89 2 |
Compare with the physiological saline group:
1P＜0.005,
2P＜0.001
Above-mentioned glucobay (acarbose) contrast agents is Bayer A.G's product.
Test 3, inhibitor is to the influence of alloxan diabetes mouse's blood sugar content: 30 of alloxan diabetes mouse, be divided into 3 groups (blood glucose value difference is no more than 0.5mmol/L between group), irritate stomach physiological saline, glucobay (acarbose) (100mg/kg), inhibitor (100mg/kg) respectively, continuous eight days.Fasting 3h after the last administration gets blood and surveys blood sugar.The result shows that this inhibitor can significantly reduce the blood sugar of alloxan diabetes mouse (seeing Table 3).Table 3 inhibitor is to the influence of alloxan diabetes mouse's blood sugar content
| Group | ????n | Blood glucose value (mmol/L) |
| Physiological saline | ????10 | ????11.42±1.31 |
| Glucobay (acarbose) | ????10 | ????8.32±1.23 1 |
| Inhibitor | ????10 | ????6.85±0.98 1 |
Compare with the physiological saline group:
1P＜0.001
Above-mentioned glucobay (acarbose) contrast agents is Bayer A.G's product.
Embodiment
After now the embodiment of the extracting method of giant knotweed tannic acid of the present invention being described in.
Embodiment one: get 300g Chinese medicine giant knotweed and add 1200ml distilled water, macerate the back and pulverize with stamp mill, in 60 ℃ of insulations 24 hours, separate with separating centrifuge then, the separating centrifuge rotating speed is 5000rpm, and centrifugation time 10 minutes is abandoned filter residue, gets supernatant liquid.Supernatant liquid is heated to 80 ℃ of insulations 10 minutes, and refrigerator is placed and is spent the night then.Put into whizzer again, centrifugation is 10 minutes under the 5000rpm rotating speed, gets supernatant liquid.Supernatant liquid is used sherwood oil (30-60bp) degreasing 3-4 time in separating funnel.Extracting solution after the degreasing is crossed activated carbon column decoloring.Low molecular weight impurities is removed in ultrafiltration then, with last 732 storng-acid cation exchange resins of gained filtrate, uses the distilled water wash-out then.After transferring PH to arrive neutrality the elutriant, under normal pressure or decompression, be heated to 60-100 ℃ and concentrate, use ultra-filtration membrane (molecular weight cut-off 5000dalton) to carry out ultrafiltration and concentration then, remove low molecular impurity, can get the brown solid powder after drying, its main component is the giant knotweed tannic acid.
Embodiment two: after 300g giant knotweed meal is used 1500ml95% ethanol cold soaking 24hr, filter, abandon filter residue, get filtrate, filtrate decompression be heated to 80 ℃, concentrate medicinal extract, medicinal extract is dissolved in water, and refluxes with chloroform, abandons chloroform layer, ethyl acetate layer is got in ethyl acetate extraction 2-3 time of gained water layer, again with NaOH extraction 2-3 time, get the NaOH aqueous solution, transfer pH value to 4 with HCl, add 5% aqueous gelatin solution, get throw out.Throw out dissolves with 50% aqueous acetone solution, uses the whizzer centrifugation then, and rotating speed is 5000rmp, separates 10 minutes, abandons precipitation, gets acetone soln, its underpressure distillation is concentrated, and reclaim acetone, obtains the colloidal solid thing.With gained colloidal solid thing water dissolution, use ethyl acetate extraction again, with gained ethyl acetate layer concentrating under reduced pressure, and reclaim ethyl acetate, obtain spissated jelly.The gained jelly adds the suitable quantity of water dissolving, filters, and elimination precipitation insolubles obtains solution clearly, and the clear liquid lyophilize is got orange-yellow powder, and its main component is the giant knotweed tannic acid.
Claims (3)
1. the extracting method of a Rhizoma Polygoni Cuspidati extract giant knotweed tannic acid is characterized in that, this method comprises following processing step:
A. the crude drug giant knotweed is through after pulverizing, and water, methyl alcohol or aqueous alcohol are extracted under heating condition, during extraction
Between 2-30 hour, solvent load be crude drug 3-10 doubly;
B. filter or centrifugation, abandon filter residue, get filtrate or supernatant liquid, with filtrate or supernatant liquid in temperature
50-100 ℃ is incubated 5-30 minute, and refrigerator is placed and spent the night;
C. put into separating centrifuge,, get supernatant liquid 2000-5000rmp centrifugation 5-20 minute;
D. supernatant liquid is used petroleum ether degreasing 2-5 time in separatory funnel;
E. with the extracting solution activated carbon decolorizing after the degreasing, low molecular weight impurities is removed in ultrafiltration then;
F. gained filtrate is gone up storng-acid cation exchange resin, use the distilled water wash-out then, elutriant is regulated it
PH is heated to 60-100 ℃ and concentrates to neutrality under normal pressure or decompression, use ultra-filtration membrane then
Carry out ultrafiltration, can obtain the brown solid powder after drying, its main component is the giant knotweed tannic acid.
2. the extracting method of a Rhizoma Polygoni Cuspidati extract giant knotweed tannic acid is characterized in that, this method comprises following processing step:
A. with crude drug giant knotweed elder generation water, ethanol or aqueous alcohol are soaked, and macerate the back and pulverize with stamp mill, in heating
Under the condition, extracted 2-30 hour, solvent load is 3-10 a times of crude drug;
B. filter, abandon filter residue, get filtrate and under normal pressure or decompression, be heated to 50-100 ℃, concentrate medicinal extract;
C. be dissolved in water, use the chloroform reflux, abandon chloroform layer, gained water layer ethyl acetate extraction 2-3
Inferior, get ethyl acetate layer, use NaOH aqueous solution extraction 2-3 time again, get the NaOH aqueous solution, use
HCl transfers pH value to 2-6, adds the 4-10% aqueous gelatin solution, gets throw out;
D. precipitation is used the whizzer centrifugation then with the dissolving of 30-70% aqueous acetone solution, abandons precipitation, gets third
Ketone solution concentrates its underpressure distillation, and reclaims acetone, obtains the colloidal solid thing;
E. with gained colloidal solid thing water dissolution, use ethyl acetate extraction again, the gained ethyl acetate layer is reduced pressure
Concentrate, and reclaim ethyl acetate, obtain spissated jelly;
F. jelly adds the suitable quantity of water dissolving, filters, and elimination precipitation insolubles obtains clear liquid, and clear liquid is freezing dried
Dry orange-yellow powder, its main component is the giant knotweed tannic acid.
3. the tannic acid product that extracting method extracted of a kind of Rhizoma Polygoni Cuspidati extract giant knotweed tannic acid according to claim 1 and 2 owing to have alpha-glucoside inhibiting activity, can be used for making the raw material of the medicine for the treatment of diabetes, obesity etc.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CNB031165451A CN1313475C (en) | 2003-04-22 | 2003-04-22 | Method for extracting polygonum cuspidatum tannic acid |
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| CNB031165451A CN1313475C (en) | 2003-04-22 | 2003-04-22 | Method for extracting polygonum cuspidatum tannic acid |
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| CN1313475C CN1313475C (en) | 2007-05-02 |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102579603A (en) * | 2007-11-14 | 2012-07-18 | 中国医学科学院药物研究所 | Application of polygonum cuspidatum (PC) in prevention and treatment of insulin resistance and relative metabolic diseases |
| US20120183633A1 (en) * | 2009-12-29 | 2012-07-19 | Korea Institute Of Oriental Medicine | Compositions and functional foods for treating and preventing obesity using polygonum cuspidatum butanol fraction and ethyl acetate fraction |
| CN104026159A (en) * | 2014-07-08 | 2014-09-10 | 山东农业大学 | Preparing method for botanical pesticides |
| CN104892695A (en) * | 2014-03-05 | 2015-09-09 | 湖南省天金科技有限公司 | Preparation method for extracting tannin with camellia oleifera shells |
| CN108348557A (en) * | 2016-03-28 | 2018-07-31 | 心悦生医股份有限公司 | Composition and application thereof containing tannic acid |
| TWI686192B (en) * | 2017-02-13 | 2020-03-01 | 心悅生醫股份有限公司 | Compositions containing tannic acids and uses thereof |
| US11154531B2 (en) | 2020-02-08 | 2021-10-26 | Syneurx International (Taiwan) Corp. | Compounds and pharmaceutical uses thereof |
| US11793823B2 (en) | 2020-04-23 | 2023-10-24 | Syneurx International (Taiwan) Corp. | Compounds and pharmaceutical uses thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1323582A (en) * | 2001-05-29 | 2001-11-28 | 四川省中医药研究院中医研究所 | Prepn. of injecta powder containing tannic acid component |
| CN1159326C (en) * | 2002-09-03 | 2004-07-28 | 四川省中医药研究院中医研究所 | Process of extracting tannic acid from Geranium wilfordii root and the use of the extractive |
-
2003
- 2003-04-22 CN CNB031165451A patent/CN1313475C/en not_active Expired - Fee Related
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102579603A (en) * | 2007-11-14 | 2012-07-18 | 中国医学科学院药物研究所 | Application of polygonum cuspidatum (PC) in prevention and treatment of insulin resistance and relative metabolic diseases |
| US9504725B2 (en) * | 2009-12-29 | 2016-11-29 | Korea Institute Of Oriental Medicine | Compositions and functional foods for treating and preventing obesity using polygonum cuspidatum butanol fraction and ethyl acetate fraction |
| CN102596211B (en) * | 2009-12-29 | 2015-06-24 | 韩国韩医学研究院 | Compositions and functional foods for treating and preventing obesity using polygonum cuspidatum butanol fraction and ethyl acetate fraction |
| US20120183633A1 (en) * | 2009-12-29 | 2012-07-19 | Korea Institute Of Oriental Medicine | Compositions and functional foods for treating and preventing obesity using polygonum cuspidatum butanol fraction and ethyl acetate fraction |
| CN104892695A (en) * | 2014-03-05 | 2015-09-09 | 湖南省天金科技有限公司 | Preparation method for extracting tannin with camellia oleifera shells |
| CN104026159A (en) * | 2014-07-08 | 2014-09-10 | 山东农业大学 | Preparing method for botanical pesticides |
| CN104026159B (en) * | 2014-07-08 | 2016-03-30 | 山东农业大学 | A kind of preparation method of plant insecticide |
| CN108348557A (en) * | 2016-03-28 | 2018-07-31 | 心悦生医股份有限公司 | Composition and application thereof containing tannic acid |
| US11202791B2 (en) | 2016-03-28 | 2021-12-21 | Syneurx International (Taiwan) Corp. | Compositions containing tannic acids and uses thereof |
| TWI686192B (en) * | 2017-02-13 | 2020-03-01 | 心悅生醫股份有限公司 | Compositions containing tannic acids and uses thereof |
| US11154531B2 (en) | 2020-02-08 | 2021-10-26 | Syneurx International (Taiwan) Corp. | Compounds and pharmaceutical uses thereof |
| US11382924B2 (en) | 2020-02-08 | 2022-07-12 | Syneurx International (Taiwan) Corp. | Compounds and pharmaceutical uses thereof |
| US11779561B2 (en) | 2020-02-08 | 2023-10-10 | Syneurx International (Taiwan) Corp. | Compounds and pharmaceutical uses thereof |
| US11793823B2 (en) | 2020-04-23 | 2023-10-24 | Syneurx International (Taiwan) Corp. | Compounds and pharmaceutical uses thereof |
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| CN1313475C (en) | 2007-05-02 |
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Granted publication date: 20070502 Termination date: 20110422 |