CN101134767A - Highly effective abstraction method for preparation of high-purity ginko flavonoid - Google Patents
Highly effective abstraction method for preparation of high-purity ginko flavonoid Download PDFInfo
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- CN101134767A CN101134767A CNA2006100687334A CN200610068733A CN101134767A CN 101134767 A CN101134767 A CN 101134767A CN A2006100687334 A CNA2006100687334 A CN A2006100687334A CN 200610068733 A CN200610068733 A CN 200610068733A CN 101134767 A CN101134767 A CN 101134767A
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Abstract
The present invention is high efficiency extracting process of high purity gingko flavone compound, and belongs to the field of natural plant medicine extracting technology. The extracting process includes the following steps: collecting green gingko leaf in autumn and stoving, crushing, extracting with 50-90 % concentration alcohol solution, concentrating the extracted solution to recover alcohol, diluting the concentrate and cooling to precipitate, adsorbing the supernatant with macroporous resin, desorbing with alcohol, vacuum concentrating the eluted solution, vacuum drying, crushing and packing. The process has no harmful matter residue, simple control and high extracting rate, and product has high effective component content and stable quality.
Description
(1) technical field
The present invention relates to a kind of natural medicinal plants extractive technique, specifically a kind of is raw material with the Ginkgo Leaf, therefrom extracts the high efficiency preparation method of high purity gingkgo flavonoids.
(2) background technology
Ginkgo is one of the most ancient in the world seeds, be described as " living fossil ", Ginkgo Leaf is a kind of important medicinal, healthy food material, its extract has very strong antioxygenation, modern age, medical science studies show that, the ginkgolic flavone glycoside glycosides, bilobalide and bilobalide are the main components of Folium Ginkgo extract, they have the radical of catching, suppress platelet activation factor (PAF), stimulate circulation and function such as brain metabolism, it is to senile dementia, hypertension, ypotension, heart trouble, arteriosclerosis, diseases such as Aging all have good preventive and therapeutic effect.In recent years, both at home and abroad, particularly countries such as Germany, Japan, the U.S., France carry out big quantity research to the chemical ingredients in the Ginkgo Leaf, separation method, have obtained bigger progress.Representative is to prepare Folium Ginkgo extract with solvent-extracted method, S ehwabe as Germany, the Flaschman pharmaceutical factory, be mainly the dried meal of Ginkgo Leaf, 60% acetone extracting, press filtration is with the tetracol phenixin degreasing, and the acetone water layer closes with ammonium sulfate is full, extracts with methylethylketone, be made into certain density ethanolic soln behind the extracting solution concentrating under reduced pressure, add an amount of lead hydroxide and filter, close so that ammonium sulfate is full after filtrate concentrates again, methylethylketone extracts, the dry back that concentrates of extracting solution is with the dry Folium Ginkgo extract that gets of the refining reconcentration of ethanol, this kind method, use organic,, the inorganic chemistry medium is many, complex process, the cost height, and easily cause the residual quality product that influences.The production technology of present domestic Folium Ginkgo extract adopts water or alcoholic solvent to extract more, and again through the macroporous resin adsorption mode, but its extraction yield is low, and extractive content is not high yet.
(3) summary of the invention
Technical assignment of the present invention is at the deficiencies in the prior art, and a kind of high extraction and the highly effective abstraction method for preparation of high-purity ginko flavonoid that reaches the Folium Ginkgo extract (GBE) of pharmacopeia required standard are provided.
The technical solution adopted for the present invention to solve the technical problems is:
The present invention prepares according to the following steps:
A, the Ginkgo Leaf when employing leaf in autumn is yellow, preserve the oven dry back;
B. Ginkgo Leaf is pulverized, standby;
C, extract with ethanol;
D, extracting solution concentrating under reduced pressure reclaim ethanol;
E, with concentrated solution dilution, cooling-sedimentation;
F, clear liquid advance the styrene type macroporous resin adsorption column and adsorb;
G, use the alcohol solution wash-out;
H, elutriant concentrating under reduced pressure, vacuum-drying, crushing packing.
The described Ginkgo Leaf processing mode of above-mentioned steps A is oven dry, but not dries, and bake out temperature is at 60-180 ℃.
The described grinding particle size of above-mentioned steps B should be between the 2-5 millimeter.
Above-mentioned steps C is for use the 50-90% extraction using alcohol, extracts temperature and is between the normal temperature to 50 ℃, the dynamic agitation extraction.
The described concentrated solution thinner of above-mentioned steps E is tap water or purified water.
The described cooling-sedimentation temperature of above-mentioned steps E is between 0-20 ℃.
The described resin of above-mentioned steps F is the DM-130 resin.
The described eluent of above-mentioned steps G is the ethanolic soln of 60-95%.
Above-mentioned steps H elutriant thickening temperature is less than 75 ℃, and the vacuum-drying temperature is less than 75 ℃.
Highly effective abstraction method for preparation of high-purity ginko flavonoid of the present invention compared with prior art, the beneficial effect that is produced is: the present invention is a kind of Folium Ginkgo extract production method, used medium does not have objectionable impurities residual, technology controlling and process is easy, the extraction yield height, product active constituent content height, and stay in grade.
(4) embodiment
Embodiment 1:
A, the Ginkgo Leaf when employing leaf in autumn is yellow are dried under 120 ℃ temperature, and preserve the oven dry back;
B, Ginkgo Leaf is pulverized, grinding particle size is 4 millimeters, and is standby;
C, the ethanolic soln with 80% extract, and temperature is controlled to be normal temperature during extraction;
D, extracting solution concentrate and reclaim ethanol, the temperature when concentrating is not higher than 65 ℃;
E, with the dilution of concentrated solution water or purified water, cooling-sedimentation, cold heavy temperature is controlled at 10 ℃.
F, clear liquid advance styrene type macroporous resin adsorption column (as DM-130) and adsorb;
G, to use alcoholic solution wash-out, the concentration of elutriant be 70%;
H, elutriant concentrating under reduced pressure, when concentrating temperature 60-70 ℃, vacuum-drying, drying temperature 60-70 ℃, crushing packing.
Embodiment 2:
A, the Ginkgo Leaf when employing leaf in autumn is yellow are dried under 85 ℃ temperature, and preserve the oven dry back;
B, Ginkgo Leaf is pulverized, 3 millimeters of grinding particle sizes are standby;
C, the ethanol with 70% extract, and temperature is controlled at 50 ℃ during extraction;
D, extracting solution concentrate and reclaim ethanol, the temperature when concentrating is 75 ℃;
E, with the dilution of concentrated solution water or purified water, cooling-sedimentation, cold heavy temperature is controlled at 15 ℃;
F, clear liquid advance styrene type macroporous resin adsorption column (as D 101) and adsorb;
G, use the alcohols desorb, the stripping liquid i.e. concentration of alcohol is 80%;
H, elutriant concentrating under reduced pressure, the temperature when concentrating is 60-70 ℃, vacuum-drying, crushing packing.
Embodiment 3:
A, the Ginkgo Leaf when employing leaf in autumn is yellow are dried under 160 ℃ temperature, and preserve the oven dry back;
B, Ginkgo Leaf is pulverized, grinding particle size is 5 millimeters, and is standby;
C, the ethanol with 50% extract, and temperature is controlled at 50 ℃ during extraction;
D, extracting solution concentrate and reclaim ethanol, the temperature when concentrating is 60 ℃;
E, with the dilution of concentrated solution water or purified water, cooling-sedimentation, cold heavy temperature is controlled at 5 ℃:
F, clear liquid advance styrene type macroporous resin adsorption column (D 201) and adsorb;
G, use the alcohols desorb, the stripping liquid i.e. concentration of alcohol is 90%;
H, elutriant concentrating under reduced pressure, the temperature when concentrating is 60 ℃, vacuum-drying, crushing packing.
Claims (9)
1. highly effective abstraction method for preparation of high-purity ginko flavonoid is characterized in that may further comprise the steps:
A, the Ginkgo Leaf when employing leaf in autumn is yellow, preserve the oven dry back;
B. Ginkgo Leaf is pulverized, standby;
C, extract with ethanol;
D, extracting solution concentrating under reduced pressure reclaim ethanol;
E, with concentrated solution dilution, cooling-sedimentation;
F, clear liquid advance the styrene type macroporous resin adsorption column and adsorb;
G, use the alcohol solution wash-out;
H, elutriant concentrating under reduced pressure, vacuum-drying, crushing packing.
2. highly effective abstraction method for preparation of high-purity ginko flavonoid according to claim 1 is characterized in that: the described Ginkgo Leaf processing mode of steps A is oven dry, but not dries, and bake out temperature is at 60-180 ℃.
3. highly effective abstraction method for preparation of high-purity ginko flavonoid according to claim 1 is characterized in that: the described grinding particle size of step B should be between the 2-5 millimeter.
4. highly effective abstraction method for preparation of high-purity ginko flavonoid according to claim 1 is characterized in that: step C is for use the 50-90% extraction using alcohol, extracts temperature and is between the normal temperature to 50 ℃, the dynamic agitation extraction.
5. highly effective abstraction method for preparation of high-purity ginko flavonoid according to claim 1 is characterized in that: the described concentrated solution thinner of step e is tap water or purified water.
6. highly effective abstraction method for preparation of high-purity ginko flavonoid according to claim 1 is characterized in that: the described cooling-sedimentation temperature of step e is between 0-20 ℃.
7. highly effective abstraction method for preparation of high-purity ginko flavonoid according to claim 1 is characterized in that: the described resin of step F is styrene type macroporous resin such as resins such as DM-130, D201, D101.
8. highly effective abstraction method for preparation of high-purity ginko flavonoid according to claim 1 is characterized in that: the described eluent of step G is the ethanolic soln of 60-95%.
9. highly effective abstraction method for preparation of high-purity ginko flavonoid according to claim 1 is characterized in that: 60-90 ℃ of step H elutriant thickening temperature, 60-90 ℃ of vacuum-drying temperature.
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2006100687334A CN101134767A (en) | 2006-09-01 | 2006-09-01 | Highly effective abstraction method for preparation of high-purity ginko flavonoid |
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| CNA2006100687334A CN101134767A (en) | 2006-09-01 | 2006-09-01 | Highly effective abstraction method for preparation of high-purity ginko flavonoid |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102078341A (en) * | 2010-12-22 | 2011-06-01 | 天津泰阳制药有限公司 | High-purity ginkgo flavone and composition thereof |
| CN102727538A (en) * | 2012-05-17 | 2012-10-17 | 江苏颐海药业有限责任公司 | Process for extracting ginkgo biloba flavone, ginkgo biloba lactone and ginkgo biloba phenolic acid from ginkgo biloba leaves |
| CN102772452A (en) * | 2012-08-17 | 2012-11-14 | 天津泰阳制药有限公司 | Method for producing ultra-low-acid ginkgo leaf extract |
| CN103251659A (en) * | 2013-06-03 | 2013-08-21 | 青岛三九九洲生物技术有限公司 | Preparation method of ginkgo leaf essence |
| CN104116764A (en) * | 2014-06-27 | 2014-10-29 | 黄霄 | Method for extracting active ingredients general flavone and terpene lactones in ginkgo leaf |
| CN105125597A (en) * | 2014-06-05 | 2015-12-09 | 四川新荷花中药饮片股份有限公司 | Penthorum chinense processing technology |
| CN105175465A (en) * | 2015-08-12 | 2015-12-23 | 河北工业大学 | Method for extracting Ginkgo biloba leaf flavonoid |
-
2006
- 2006-09-01 CN CNA2006100687334A patent/CN101134767A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102078341A (en) * | 2010-12-22 | 2011-06-01 | 天津泰阳制药有限公司 | High-purity ginkgo flavone and composition thereof |
| CN102078341B (en) * | 2010-12-22 | 2012-08-22 | 天津泰阳制药有限公司 | High-purity ginkgo flavone and composition thereof |
| CN102727538A (en) * | 2012-05-17 | 2012-10-17 | 江苏颐海药业有限责任公司 | Process for extracting ginkgo biloba flavone, ginkgo biloba lactone and ginkgo biloba phenolic acid from ginkgo biloba leaves |
| CN102727538B (en) * | 2012-05-17 | 2015-01-07 | 江苏颐海药业有限责任公司 | Process for extracting ginkgo biloba flavone, ginkgo biloba lactone and ginkgo biloba phenolic acid from ginkgo biloba leaves |
| CN102772452A (en) * | 2012-08-17 | 2012-11-14 | 天津泰阳制药有限公司 | Method for producing ultra-low-acid ginkgo leaf extract |
| CN103251659A (en) * | 2013-06-03 | 2013-08-21 | 青岛三九九洲生物技术有限公司 | Preparation method of ginkgo leaf essence |
| CN103251659B (en) * | 2013-06-03 | 2015-04-22 | 青岛三九九洲生物技术有限公司 | Preparation method of ginkgo leaf essence |
| CN105125597A (en) * | 2014-06-05 | 2015-12-09 | 四川新荷花中药饮片股份有限公司 | Penthorum chinense processing technology |
| CN104116764A (en) * | 2014-06-27 | 2014-10-29 | 黄霄 | Method for extracting active ingredients general flavone and terpene lactones in ginkgo leaf |
| CN105175465A (en) * | 2015-08-12 | 2015-12-23 | 河北工业大学 | Method for extracting Ginkgo biloba leaf flavonoid |
| CN105175465B (en) * | 2015-08-12 | 2019-04-12 | 河北工业大学 | A method of extracting ginko leaves flavone |
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