CN100554261C - A kind of preparation method of ampelopsin - Google Patents
A kind of preparation method of ampelopsin Download PDFInfo
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- CN100554261C CN100554261C CNB2006100196934A CN200610019693A CN100554261C CN 100554261 C CN100554261 C CN 100554261C CN B2006100196934 A CNB2006100196934 A CN B2006100196934A CN 200610019693 A CN200610019693 A CN 200610019693A CN 100554261 C CN100554261 C CN 100554261C
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- ampelopsin
- water
- extraction
- alcohol
- ampelopsis
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Abstract
A kind of method prepare ampelopsin of extracting from vine tea and other Vitaceae ampelopsis belongs to the extracts active ingredients field of crude drug.Comprise that first water or alcohol-water decoct extraction or refluxing extraction, extract one or many, filtered while hot, behind the united extraction liquid, add alkaline assistant (as weakly alkaline materials such as sodium bicarbonate, yellow soda ash, sodium sorbates), make extracting solution pH between 7～9, carry out thaumatropy, concentrated, crystallization process through heated and boiled, through the alcohol-water recrystallization, get the ampelopsin crystal again.Preparation process of the present invention is a solvent with water and ethanol only, and institute adds alkaline assistant and is the food auxiliary agent, and cost is low, pollutes for a short time, and extraction process is simple, is easy to suitability for industrialized production, and the ampelopsin purity that makes can reach more than 98%.
Description
Technical field
The present invention relates to a kind of preparation method of ampelopsin, is from vine tea or other Vitaceae ampelopsis specifically, as ampelopsis cantoniensis, and Cayratia japonica (Thunb.) Gagnep., no acupuncture root, the method for extraction ampelopsin in the Northeastern Caulis seu folium ampelopsis brevipedunculatae.The extracts active ingredients field that belongs to crude drug.
Background technology
The heart, cerebrovascular disease are the diseases of serious harm human health.(plateletactivating factor is platelet aggregation activator the strongest known to so far and important inflammatory mediator PAF) to platelet activating factor, and it can act on the various kinds of cell acceptor, produces biological effect widely.PAF participates in many pathophysiological change, and is closely related with all pathogenic processes oversensitive, cerebrovascular disease such as ischemia-reperfusion, inflammatory reaction, atherosclerosiss; The effect of antagonism PAF is to suppress thrombosis at present, improves multiple disturbance of blood circulation, the important channel of all oversensitive, cerebrovascular diseases such as prevention and treatment coronary heart disease, atherosclerosis etc.According to research reports, rabbit platelet gathering, 5-HT that ampelopsin can suppress the PAF mediation discharge and the interior calcium ion concn rising of thrombocyte, thereby play the cardiovascular effect of protection, and experimental result shows that its anti-PAF effect is stronger than the effective constituent hydroxyl radical carthamin yellow carthamus A effect of traditional blood-activating and stasis-removing safflower; Its mechanism of action is similar to the paf receptor antagonists Ginkgolides, is a kind of new paf receptor antagonists.In addition, research shows that also ampelopsin also has hypoglycemic, reducing blood-fat, anti-oxidant and liver protecting, multiple biological activity such as anticancer.Above result of study shows that ampelopsin is with a wide range of applications in preparation reducing blood-fat, hypoglycemic and antithrombotic medicine or healthcare products.
But ampelopsin in natural phant content seldom, according to domestic existing bibliographical information, the higher plant of ampelopsin content is the leaf of the Vitaceae ampelopsis Ampelopsis grossedentata of Guangxi vine tea and Zhangjiajie, Hunan, but content also has only 2.99% and 2.17%.Therefore, the medicine resource of research and development ampelopsin and extraction preparation method thereof have great importance.
Summary of the invention
The objective of the invention is in order to remedy in the nature plant ampelopsin content few, the extraction separation difficulty, be not easy to large-scale industrial production, and a kind of method for preparing ampelopsin of extracting from other Vitaceae ampelopsis such as vine tea and ampelopsis cantoniensis, Cayratia japonica (Thunb.) Gagnep., no acupuncture root, Vitis Amurensis is provided.
Vine tea and other Vitaceae ampelopsis, as ampelopsis cantoniensis, Cayratia japonica (Thunb.) Gagnep., no acupuncture root, the main component in the Vitis Amurensis is the flavonols composition, is mainly two hydrogen ampelopsin (dihydromyricetin), and contains a small amount of ampelopsin (myricetin).Its molecular formula is respectively C
15H
12O
8And C
15H
10O
8, structural formula is respectively figure below (I) and (II):
The present invention utilizes two hydrogen ampelopsin can be converted into the principle of ampelopsin under weak basic condition, extraction has multiple bioactive ampelopsin composition from above-mentioned medicinal material, and this composition can be used as preparation treatment or prevention cardio-cerebrovascular disorder and treatment or prevents the healthcare products or the pharmaceutical use of hyperlipidemia, hyperglycemia.
The present invention is achieved in that vine tea or other grape material ampelopsis raw medicinal material elder generation's water or alcohol-water decoction extraction or refluxing extraction, extract one or many, filtered while hot, behind the united extraction liquid, add alkaline assistant, make extracting solution pH between 7～9, carry out thaumatropy, concentrated, crystallization process through heated and boiled, through the alcohol-water recrystallization, get the ampelopsin crystal again.
Vine tea described in the aforesaid method is that the young stem and leaf of Vitaceae ampelopsis Ampelopsis grossedentata forms through tradition processing, kneading, drying, also can be other Vitaceae ampelopsis, as ampelopsis cantoniensis, and Cayratia japonica (Thunb.) Gagnep., no acupuncture root, Vitis Amurensis etc.Extract solvent and can be water or alcohol-water, alcohol wherein can be methyl alcohol or ethanol, and the ratio of alcohol-water can be 10～95%; Described alkaline assistant can be weakly alkaline materials such as sodium bicarbonate, yellow soda ash, sodium sorbate, the purpose of its adding is to impel the two hydrogen ampelopsin in the extracting solution to be converted into ampelopsin, its consumption is 1～3% of a medicinal material amount, the method of its adding is: can add when solubilizing agent extracts, also can boil the back at united extraction liquid adds, make extracting solution pH between 7～9, heated and boiled, conversion, extremely two hydrogen ampelopsin are converted into till the ampelopsin fully; Concentrated, crystallization again through alcohol-water recrystallization, get the ampelopsin crystal.
The alcohol of ampelopsin recrystallization-water ratio can be 10～95%, and alcohol wherein can be methyl alcohol or ethanol.
The present invention can adopt all Vitaceae ampelopsis, preferably uses vine tea (young stem and leaf that is Vitaceae ampelopsis Ampelopsis grossedentata forms through tradition processing, kneading, drying), Cayratia japonica (Thunb.) Gagnep., ampelopsis cantoniensis, no acupuncture root, Vitis Amurensis etc.
The invention has the advantages that preparation process is a solvent with water and ethanol only, institute adds alkaline assistant and is the food auxiliary agent, and cost is low, pollutes for a short time, and extraction process is simple, and the ampelopsin productive rate can reach more than 8%, is easy to suitability for industrialized production; The product purity height that makes, the ampelopsin purity for preparing can reach more than 98%.
Embodiment
Describe the present invention in detail by the following examples. but should be appreciated that these embodiment just illustrate the present invention, rather than in office where face limits the scope of the invention.
Embodiment 1: extract ampelopsin from vine tea
Get vine tea 1500 grams, add after about 12 times of water gagings fully soak, heated and boiled decocted 1 hour, filtered while hot, residue add 8 times of water gagings again and decocted filtered while hot 0.5 hour, united extraction liquid, boil the back and add sodium bicarbonate 20 grams, keep little and boil more than 2 hours, TLC checks that extremely two hydrogen ampelopsin are converted into till the ampelopsin fully; Concentrated, crystallization, the crystallization that leaching is separated out again with about 500ml 50% aqueous ethanolic solution recrystallization, gets yellow or yellow-green colour crystallization, productive rate 8.6%; Fusing point＞300 ℃ are dissolved in hot ethanol, methyl alcohol, are insoluble to acetone, chloroform, sherwood oil.The reaction of hydrochloric acid magnesium powder is rose, and ferric chloride reaction is atropurpureus, is strong yellow-green fluorescence with the aluminum chloride reaction; The alphanaphthol reaction feminine gender; With zirconates-citric acid reactions, aureus does not take off; UV λ
Max MeOHNm:375nm (band I), 301 (sh), 278 (sh) and 254nm (band II); Add sodium methylate, band I red shift 48nm, and spectrum fails gradually; Add AlCl
3After, band I is with II red shift 15nm than the UV spectrum red shift 75nm that records in the methyl alcohol; Add hydrochloric acid again, band I adds AlCl
3Person's violet shift 19nm, band II violet shift 2nm; After adding sodium-acetate, spectrum fails rapidly; Add sodium-acetate and boric acid, band I is than the UV spectrum red shift 17nm that records in the methyl alcohol, but band II moves hardly; Illustrate that crystallization is the flavonols composition, the A ring and C ring both has 3,5,7 hydroxyls, and the B ring has the ortho position poly-hydroxy
[8]IR (KBr, cm
-1): 3575,3380,3255 (V
OH), the 1646 (V of alpha, beta-unsaturated ketone carbonyl
C=0), 1612,1550,1505,1454 (skeletal vibrations of aromatic ring C=C), gained spectrum through with the spectral comparison basically identical of known ampelopsin reference substance.FAB-MSm/z(％)：319(M
++H，100)，318(M
+，23.5)。Brilliant II is made acetylate, get white, needle-shaped crystals, mp.210-211 ℃,
1HNMR (CDCl
3) ppm: δ 7.61 (2H, s, C
2`, 6`-H), δ 7.33 (1H, d, C
8-H), δ 6.87 (1H, d, C
6-H), δ 2.42 (3H, s, OCOCH
3), δ 2.31 (15H, m, 5 * OCOCH
3).According to above physico-chemical property and spectroscopic data analysis, it is 3,5 that the conclusive evidence novel method is extracted the crystallization that obtains, 7,3 ', 4 ', 5 '-quercetagetin, i.e. ampelopsin (Myricetin).
Embodiment 2: extract ampelopsin from Cayratia japonica (Thunb.) Gagnep.
Will be through the Cayratia japonica (Thunb.) Gagnep. medicinal material 1500 gram flush away dust of dry processing, add about 10 times of amount 50% ethanol, after fully soaking, heating and refluxing extraction 40 minutes, filter, residue added 8 times of amount 50% alcohol reflux 30 minutes again, filtered united extraction liquid, after being concentrated into 8 times of amounts of medicinal material volume, add anhydrous sodium carbonate 22 grams, keep little and boil more than 2 hours, TLC checks that extremely two hydrogen ampelopsin are converted into till the ampelopsin fully; Concentrated, crystallization, the crystallization that leaching is separated out with about 500ml 60% aqueous ethanolic solution dissolving, is filtered again, and concentrated, crystallization get yellow or yellow-green colour crystallization, productive rate 8.0%.
Through TLC inspection and UV, IR,
1HNMR measures, and shows that product is identical with the product that embodiment 1 obtains.
Embodiment 3: extract ampelopsin from ampelopsis cantoniensis
Will be through the ampelopsis cantoniensis medicinal material 1500 gram flush away dust of dry processing, add after about 10 times of water gagings fully soak, heated and boiled decocted 40 minutes, filtered while hot, residue add 8 times of water gagings again and decocted filtered while hot 30 minutes, united extraction liquid, boil the back and add sodium sorbate 25 grams, keep little and boil more than 2 hours, TLC checks that extremely two hydrogen ampelopsin are converted into till the ampelopsin fully; Concentrated, crystallization, the crystallization that leaching is separated out again with about 500ml 95% aqueous ethanolic solution recrystallization, gets yellow or yellow-green colour crystallization, productive rate 8.2%.
Through TLC inspection and UV, IR,
1HNMR measures, and shows that product is identical with the product that embodiment 1 obtains.
Claims (1)
1, a kind of preparation method of ampelopsin, it is characterized in that: with vine tea or other Vitaceae ampelopsis raw medicinal material elder generation's water or alcohol-water boiling and extraction or refluxing extraction, extract one or many, filtered while hot behind the united extraction liquid, adds alkaline assistant, make extracting solution pH between 7～9, carry out thaumatropy, concentrated, crystallization process through heated and boiled,, get the ampelopsin crystal again through the alcohol-water recrystallization.
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| CN100554261C true CN100554261C (en) | 2009-10-28 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103275049B (en) * | 2013-05-21 | 2015-02-04 | 中南大学 | Method for preparing myricetin by using vine tea and application of pyrosulfite |
| CN103304194B (en) * | 2013-06-27 | 2015-08-12 | 平顶山市安泰华矿用安全设备制造有限公司 | A kind of grout material for bag type paste injection hole sealing device |
| CN103804335B (en) * | 2014-01-22 | 2016-05-18 | 贵州大学 | Nitrogenous analog derivative of a kind of myricetin and its production and use |
| CN104045616B (en) * | 2014-06-26 | 2016-02-10 | 无锡市崇安区科技创业服务中心 | A kind of extracting method of myricetin |
| CN105037310B (en) * | 2015-06-05 | 2017-10-13 | 柳州市绿翔生物技术有限公司 | It is a kind of while extracting the technique of myricetin and dihydromyricetin |
| CN106045958B (en) * | 2016-07-29 | 2018-09-28 | 湖南绿蔓生物科技股份有限公司 | A method of separating-purifying myricetin and dihydromyricetin from vine tea |
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2006
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Non-Patent Citations (6)
| Title |
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| 广西瑶族藤茶化学成分的研究. 覃洁萍等.天然产物研究与开发，第9卷第4期. 1997 |
| 广西瑶族藤茶化学成分的研究. 覃洁萍等.天然产物研究与开发，第9卷第4期. 1997 * |
| 无刺根中蛇葡萄素和杨梅素的含量测定. 陈缵光等.中药材，第20卷第1期. 1997 |
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