CN102078341A - High-purity ginkgo flavone and composition thereof - Google Patents
High-purity ginkgo flavone and composition thereof Download PDFInfo
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- CN102078341A CN102078341A CN 201010600829 CN201010600829A CN102078341A CN 102078341 A CN102078341 A CN 102078341A CN 201010600829 CN201010600829 CN 201010600829 CN 201010600829 A CN201010600829 A CN 201010600829A CN 102078341 A CN102078341 A CN 102078341A
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Abstract
The invention relates to a high-purity ginkgo flavone and a composition thereof. The high-purity ginkgo flavone is light brownish yellow, and tastes slightly bitter; the content of ginkgo flavone is greater than or equal to 50%, the peak ratio of quercetin to kaempferol is 0.8-1.2, the peak ratio of isorhamnetin to quercetin is greater than or equal to 0.15, the concentration of ginkgoic acid is smaller than 5ppm, and the content of residue on ignition is smaller than 0.8%. The water content is smaller than 5.0%. The method for preparing the high-purity ginkgo flavone comprises the following steps: extracting by heating ginkgo leaves, which are used as the raw material, under reflux with a 20-80 wt% ethanol solution; concentrating the extracting solution to recover ethanol; separating by passing through macroporous resin columns; carrying out ethanol desorption; diluting the product by adding water; adsorbing by passing the product through a gel-type hydrogen bond adsorption resin which is mainly based on hydrogen bond adsorption, and desorbing; and collecting the effluent liquid and the desorption liquid, concentrating and drying. The preparation technique is simple and reliable, has the advantage of low cost, and does not use toxic organic solvents in the process, thereby being environment-friendly. The high-purity ginkgo flavone can be made into a composition as an effective constituent, and the composition can be used as various preparations (capsules, tablets, oral liquids, granules, powder, injections and the like) of ginkgo flavone medicines or health products.
Description
Technical field
The present invention relates to a kind of high-purity ginkgetin and compositions, in particular to the production technology of from Folium Ginkgo, extracting the high-purity ginkgetin.
Background technology
Semen Ginkgo (Ginkgo biloba L.) is a kind of important medicinal plants, and Folium Ginkgo is the leaf of Ginkgoaceae plant Ginkgo biloba, and its bitter and puckery flavor, property are put down, and Ginkgo total flavones that it is contained and terpene lactones have important medical value.The seventies in last century, Germany takes the lead in having formulated quality standard, i.e. standard silver Fructus Pruni extract (Ginkgo total flavones 〉=24%, terpene lactones 〉=6% for Semen Ginkgo extrac (being called for short GBE), ginkgoic acid≤10ppm), this standard and then also become the international international standard of Semen Ginkgo extrac.Studies show that further the ginkgetin that exceeds purity has better therapeutic than common standard silver Fructus Pruni extract aspect the treatment cardiovascular and cerebrovascular disease, therefore the production method of high-purity ginkgetin also becomes the research focus of industry in recent years.At present, less about the extracting method report of high-purity ginkgetin.Nankai University reported once that the mode that adopts non-aqueous system coordination absorption is separated and obtained the gingko flavone extractive of purity more than 50%, but resin that this method is used need be introduced the so-called part of metal ion, absorption simultaneously also will be carried out at non-aqueous system, and there are a lot of problems in actual applications in this method.CN 200610068733.4 once mentioned the preparation of high-purity ginkgetin, but from the actual implementation content of patent, was a kind of preparation method of standard silver Fructus Pruni extract.CN200810068890 mentions a kind of extracting method of high-purity ginkgo flavone aglycone, and this patent adopts multistep reactions such as hydrochloric acid hydrolysis, has prepared the high-purity ginkgo flavone aglycone, but resulting product has lost the personal feature of Semen Ginkgo extrac.
In a word, high-purity gingko flavone extractive extensive market, its crucial production technology still remain further ripe, invent a kind of simply, production technology efficiently, will have vast market value and great social significance.
Summary of the invention
Purpose of the present invention just is to provide a kind of high-purity ginkgetin and compositions.Preparation technology of the present invention is simple, reliable.The high-purity ginkgetin is made various preparations (capsule, tablet, oral liquid, electuary, powder, the injection etc.) use that compositions can be used as ginkgetin medicine or health product as effective ingredient.
Purpose of the present invention can realize by following technical scheme:
High-purity ginkgetin provided by the invention is the sundown powder, and mildly bitter flavor, ginkgetin 〉=50%, Quercetin and kaempferol peak are than between the 0.8--1.2, and isorhamnetin and Quercetin peak compare 〉=0.15, ginkgoic acid＜5ppm, residue on ignition＜0.8%.Water content＜5.0%, dissolubility: 5 grams/100 ml waters.Preparation method is to be raw material with the Folium Ginkgo, with mass fraction is that the lixiviate of 20-80% alcoholic solution reflux is extracted, extracting solution concentrates and reclaims ethanol, crossing macroporous resin column separates, alcohol desorption, reclaim ethanol once more, the direct thin up of gained solution or drying got behind the Semen Ginkgo extrac powder behind the thin up, be the gel-type hydrogen bonding adsorption resin absorption and the desorbing of main effect by adding again with the adsorption by hydrogen bond, collect effluent and stripping liquid, concentrated, dry, promptly obtain high-purity gingko flavone extractive (〉=50%) product.
The step that high-purity ginkgetin preparation method provided by the invention comprises:
1) with the Folium Ginkgo being raw material, is that 70-90 ℃ of reflux lixiviate of 20-80% alcoholic solution extracted each 0.5-3 hour 2 times with mass fraction.Extracting solution concentrates and reclaims ethanol.
2) cross macroporous resin column and separate, the post of adsorption column is directly than being 3-10: 1, and the weight ratio of resin and Folium Ginkgo is 0.5-3: 1, use the 50%-90% alcohol desorption, preferred 50-70%.The absorption and the flow velocity of desorbing be 0.5-3BV/H (BV: bed volume, H: hour), reclaim ethanol once more.
3) the direct thin up of gained solution or drying got behind the Semen Ginkgo extrac powder behind the thin up (concentration is 0.1-20%)), be the gel-type hydrogen bonding adsorption resin adsorption and desorption of main effect by adding again with the adsorption by hydrogen bond, the post of adsorption column is directly than being 3-10: 1, collect effluent and stripping liquid, the flow velocity of absorption and desorbing is 0.5-3BV/H.Stripping liquid is the ethanol water of 50%-90%.Preferred 50-70%.
4) concentrated, dry, promptly obtain high-purity gingko flavone extractive (〉=50%) product.
Used macroporous resin is for being macroporous resin FL-2, AB-8 or the D101 of main skeleton with styrene in the described separation process.Described gel-type adsorbent resin is MG-1, MG-2, OU-1.
Compositions provided by the invention is as effective ingredient with the high-purity ginkgetin, being equipped with medicine is to go up the acceptable auxiliary agent to make compositions, and the various preparations (capsule, tablet, oral liquid, electuary, powder, injection etc.) that can be used as ginkgetin medicine or health product use.
The present invention does from the source, thereby has guaranteed the stable and controllable of products obtained therefrom quality.Preparation technology is simple, reliable, and cost is low, does not use toxic organic solvent in the process, is a kind of environmentally friendly technology.The high-purity ginkgetin is made various preparations (capsule, tablet, oral liquid, electuary, powder, the injection etc.) use that compositions can be used as ginkgetin medicine or health product as effective ingredient.
The specific embodiment
Can further specify the present invention below in conjunction with embodiment:
Embodiment 1
The extraction of Folium Ginkgo: get the 400g Folium Ginkgo, adding for the first time is the ethanol water (2000ml) of 5 times of amounts 20% of Folium Ginkgo quality, and 70 ℃ of reflux, extract, 3 hours add the ethanol water (1600ml) of 4 times of amounts 20% for the second time, 70 ℃ of reflux, extract, 2 hours.Merge extracted twice liquid, reclaim ethanol, thin up left standstill 4 hours, filtered, and must clarify extracting solution.
Separation and purification: will go up step gained extracting solution and feed adsorption resin column FL-2 (400g) (Tianjin Ourui Biology Technology Co., Ltd., public offering), resin column is directly than 10: 1, and the absorption flow velocity is 1BV/H.After absorption finishes, with ethanol water (2400ml) desorbing of 4BV 70%, flow velocity 1BV/H.Stripping liquid reclaims ethanol, gets paste GBE product.
The preparation of high-purity ginkgetin: above-mentioned paste GBE thin up to 400ml, is fed MG-2 (200g) adsorption resin column, and resin column is directly than 8: 1, and the absorption flow velocity is 1.5BV/H.After absorption finishes, with the water flushing of 2BV, 50% ethanol water (600ml) desorbing, flow velocity 1.5BV/H, stripping liquid concentrates, and vacuum drying gets Ginkgo total flavones content 65.8% product.
Embodiment 2
The extraction of Folium Ginkgo: get the 400kg Folium Ginkgo, add for the first time the ethanol water (2000L) of 5 times of amounts 80%, 70 ℃ of reflux, extract, 3 hours add the ethanol water (1600L) of 4 times of amounts 80% for the second time, 70 ℃ of reflux, extract, 2 hours.Merge extracted twice liquid, reclaim ethanol, thin up left standstill 4 hours, filtered, and must clarify extracting solution.
Separation and purification: will go up step gained extracting solution and feed adsorption resin column FL-2 (600kg) (Tianjin Ourui Biology Technology Co., Ltd.), resin column is directly than 7: 1, and the absorption flow velocity is 1BV/H.After absorption finishes, with ethanol water (2400L) desorbing of 4BV 70%, flow velocity 1BV/H.Stripping liquid reclaims ethanol, gets paste GBE product
The preparation of high-purity ginkgetin: above-mentioned paste GBE thin up to 400L, is fed MG-2 (200kg) adsorption resin column (Tianjin Ourui Biology Technology Co., Ltd., public offering), and resin column is directly than 8: 1, and the absorption flow velocity is 1.5BV/H.After absorption finishes, with the water flushing of 2BV, 50% ethanol water (600L) desorbing, flow velocity 2BV/H, stripping liquid concentrates, and vacuum drying gets Ginkgo total flavones content 65.8% product.
Embodiment 3
The extraction of Folium Ginkgo: get the 400kg Folium Ginkgo, add for the first time the ethanol water (2000L) of 5 times of amounts 50%, 70 ℃ of reflux, extract, 3 hours add the ethanol water (1600L) of 4 times of amounts 50% for the second time, 70 ℃ of reflux, extract, 2 hours.Merge extracted twice liquid, reclaim ethanol, thin up left standstill 4 hours, filtered, and must clarify extracting solution.
Separation and purification: will go up step gained extracting solution and feed adsorption resin column FL-2 (600kg) (Tianjin Ourui Biology Technology Co., Ltd.), resin column is directly than 8: 1, and the absorption flow velocity is 1BV/H.After absorption finishes, with ethanol water (2400L) desorbing of 4BV 50%, flow velocity 1BV/H.Stripping liquid reclaims ethanol, obtains standard GBE powder after vacuum or the spray drying.
The preparation of high-purity ginkgetin: above-mentioned paste GBE thin up to 400L, is fed MG-2 (200kg) adsorption resin column (Tianjin Ourui Biology Technology Co., Ltd., public offering), and resin column is directly than 5: 1, and the absorption flow velocity is 1.5BV/H.After absorption finishes, with the water flushing of 2BV, 50% ethanol water (600L) desorbing, flow velocity 2BV/H, stripping liquid concentrates, and vacuum drying gets Ginkgo total flavones content 52.1% product.
Claims (6)
1. a high-purity ginkgetin is characterized in that it is the sundown powder, and mildly bitter flavor, ginkgetin 〉=50%, Quercetin and kaempferol peak are than between the 0.8--1.2, and isorhamnetin and Quercetin peak compare 〉=0.15, ginkgoic acid＜5ppm, residue on ignition＜0.8%.Water content＜5.0%, dissolubility: 5 grams/100 ml waters; Preparation method is to be raw material with the Folium Ginkgo, with mass fraction is that the lixiviate of 20-80% alcoholic solution reflux is extracted, extracting solution concentrates and reclaims ethanol, cross macroporous resin column and separate, alcohol desorption reclaims ethanol once more, the direct thin up of gained solution or drying got behind the Semen Ginkgo extrac powder behind the thin up, be the gel-type hydrogen bonding adsorption resin absorption and the desorbing of main effect with the adsorption by hydrogen bond by adding again, collect effluent and stripping liquid, concentrated, dry.
2. the preparation method of the described high-purity ginkgetin of claim 1 is characterized in that the step that it comprises:
1) with the Folium Ginkgo being raw material, is that the 20-80% alcoholic solution extracts 2 times in 70-90 ℃ of reflux lixiviate with mass fraction, and each 0.5-3 hour, extracting solution concentrated and reclaims ethanol;
2) cross macroporous resin column and separate, the post of adsorption column is directly than being 3-10: 1, and the weight ratio of resin and Folium Ginkgo is 0.5-3: 1, use the 50%-90% alcohol desorption, preferred 50-70%; The flow velocity of absorption and desorbing is 0.5-3BV/H, reclaims ethanol once more;
3) the direct thin up of gained solution or drying got thin up behind the Semen Ginkgo extrac powder, concentration is 0.1-20%, be the gel-type hydrogen bonding adsorption resin absorption and the desorbing of main effect by adding again with the adsorption by hydrogen bond, the post of adsorption column is directly than being 3-10: 1, collect effluent and stripping liquid, the flow velocity of absorption and desorbing is 0.5-3BV/H; Stripping liquid is the ethanol water of 50%-90%;
4) concentrated, dry, promptly obtain high-purity ginkgetin extract product.
3. in accordance with the method for claim 1, it is characterized in that macroporous resin used in the described separation process is for being macroporous resin FL-2, AB-8 or the D101 of main skeleton with styrene.
4. in accordance with the method for claim 1, it is characterized in that described gel-type hydrogen bonding adsorption resin is MG-1, MG-2, OU-1.
5. the compositions of the described high-purity ginkgetin of claim 1, it is characterized in that it be with the high-purity ginkgetin as effective ingredient, being equipped with medicine is to go up the compositions that the acceptable auxiliary agent is made.
6. the ginkgetin medicine made of the compositions of the described high-purity ginkgetin of claim 5 or capsule, tablet, oral liquid, electuary, powder or the injection of health product.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102293790A (en) * | 2011-07-26 | 2011-12-28 | 天津泰阳制药有限公司 | High purity ginkgolide composition |
| CN102351826A (en) * | 2011-09-26 | 2012-02-15 | 重庆大学 | Extraction method of ginkgo leaf flavonoids based on steam explosion |
| CN103300469A (en) * | 2013-06-27 | 2013-09-18 | 南京林业大学 | Ginkgo leaf cigarette and preparation method thereof |
| CN107684568A (en) * | 2017-09-18 | 2018-02-13 | 临沂金卓生物科技有限公司 | A kind of method of the Hydrolysis kinetics high-purity silver flavone from ginkgo leaf |
| CN108853464A (en) * | 2018-09-26 | 2018-11-23 | 浙江圣博康药业有限公司 | A kind of preparation method of ginkgo-leaf oral liquor |
| CN112439000A (en) * | 2019-08-31 | 2021-03-05 | 北京化工大学 | Method for extracting flavonoid compounds from ginkgo leaves by combining eutectic solvent with macroporous resin purification |
Citations (1)
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| CN101134767A (en) * | 2006-09-01 | 2008-03-05 | 颜廷和 | Highly effective abstraction method for preparation of high-purity ginko flavonoid |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101134767A (en) * | 2006-09-01 | 2008-03-05 | 颜廷和 | Highly effective abstraction method for preparation of high-purity ginko flavonoid |
Non-Patent Citations (1)
| Title |
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| 《华东理工大学学报(自然科学版)》 20060630 陈艳立等 后交联均孔树脂的筛分性能及其对银杏叶黄酮的纯化 第32卷, 第6期 2 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102293790A (en) * | 2011-07-26 | 2011-12-28 | 天津泰阳制药有限公司 | High purity ginkgolide composition |
| CN102351826A (en) * | 2011-09-26 | 2012-02-15 | 重庆大学 | Extraction method of ginkgo leaf flavonoids based on steam explosion |
| CN103300469A (en) * | 2013-06-27 | 2013-09-18 | 南京林业大学 | Ginkgo leaf cigarette and preparation method thereof |
| CN107684568A (en) * | 2017-09-18 | 2018-02-13 | 临沂金卓生物科技有限公司 | A kind of method of the Hydrolysis kinetics high-purity silver flavone from ginkgo leaf |
| CN108853464A (en) * | 2018-09-26 | 2018-11-23 | 浙江圣博康药业有限公司 | A kind of preparation method of ginkgo-leaf oral liquor |
| CN112439000A (en) * | 2019-08-31 | 2021-03-05 | 北京化工大学 | Method for extracting flavonoid compounds from ginkgo leaves by combining eutectic solvent with macroporous resin purification |
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