CN1048724C - Process for extracting total flavone from ginkgo leaf - Google Patents
Process for extracting total flavone from ginkgo leaf Download PDFInfo
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- CN1048724C CN1048724C CN95118737A CN95118737A CN1048724C CN 1048724 C CN1048724 C CN 1048724C CN 95118737 A CN95118737 A CN 95118737A CN 95118737 A CN95118737 A CN 95118737A CN 1048724 C CN1048724 C CN 1048724C
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- amount
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- aqueous solution
- extracting
- alkaline aqueous
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- 238000000034 method Methods 0.000 title claims abstract description 22
- 229930003944 flavone Natural products 0.000 title claims abstract description 17
- 235000011949 flavones Nutrition 0.000 title claims abstract description 17
- 241000218628 Ginkgo Species 0.000 title claims abstract description 12
- 235000011201 Ginkgo Nutrition 0.000 title claims abstract description 12
- 235000008100 Ginkgo biloba Nutrition 0.000 title claims abstract description 12
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 title abstract description 4
- 150000002212 flavone derivatives Chemical class 0.000 title abstract description 4
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 title abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000000706 filtrate Substances 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 7
- 235000006708 antioxidants Nutrition 0.000 claims abstract description 7
- 239000011347 resin Substances 0.000 claims abstract description 5
- 229920005989 resin Polymers 0.000 claims abstract description 5
- 239000006228 supernatant Substances 0.000 claims abstract description 5
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical class [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims abstract description 4
- 239000007864 aqueous solution Substances 0.000 claims description 13
- 150000002213 flavones Chemical class 0.000 claims description 13
- 238000007654 immersion Methods 0.000 claims description 9
- 230000003078 antioxidant effect Effects 0.000 claims description 6
- 238000009835 boiling Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 4
- 229920001661 Chitosan Polymers 0.000 claims description 3
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 claims description 3
- 238000010828 elution Methods 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 230000032683 aging Effects 0.000 claims description 2
- 238000013019 agitation Methods 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims description 2
- 239000012141 concentrate Substances 0.000 claims 1
- 238000011084 recovery Methods 0.000 claims 1
- 239000000284 extract Substances 0.000 abstract description 7
- 239000000203 mixture Substances 0.000 abstract 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 abstract 2
- 239000003480 eluent Substances 0.000 abstract 2
- 230000001105 regulatory effect Effects 0.000 abstract 2
- 239000006188 syrup Substances 0.000 abstract 2
- 235000020357 syrup Nutrition 0.000 abstract 2
- 230000000274 adsorptive effect Effects 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 229910000029 sodium carbonate Inorganic materials 0.000 abstract 1
- 235000017550 sodium carbonate Nutrition 0.000 abstract 1
- 238000000605 extraction Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 244000194101 Ginkgo biloba Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000002526 effect on cardiovascular system Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
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- Medicines Containing Plant Substances (AREA)
Abstract
The present invention discloses a method for extracting total flavone from ginkgo leaves. The method comprises the following steps: ginkgo leaves washed, chopped and air-dried are soaked by a small amount of water for one night, and then extracted by alkaline water prepared from saturated lime water and a small amount of antioxidants three times; the mixture is filtered, filtrate of the three times is combined, concentrated in a vacuum mode and cooled, and a definite amount of adsorptive clarificant is added when the filtrate is agitated; the temperature is preserved for a certain time, the mixture is centrifuged and filtered, and a definite amount of ethanol is added to the filtrate and agitated; a definite amount of Na2CO3 whose concentration is 5% is subsequently added, the pH is regulated to 9 to 10, and the mixture is precipitated after still standing, centrifuged and filtered; 10% of hydrochloric acid is added to supernatant liquid, and the pH is regulated to 6 more or less again; the supernatant liquid is eluted by a D101 macroporous resin column and ethanol until no flavone reaction occurs; after the ethanol is recovered, eluent is concentrated in a vacuum mode until the eluent forms a syrup shape; yellow extract of a definite concentration is obtained by drying the syrup in a vacuum mode at a temperature of 60DEGC at most.
Description
The present invention relates to a kind of method of extracting total flavones, refer to a kind of method of from Ginkgo Leaf, extracting total flavones especially.
Ginko leaves flavone is the bulk drug of diseases such as at present both at home and abroad most popular treatment is cardiovascular, the cerebrovascular.But but there are a lot of problems in the technology of present various extraction flavones, mainly contains: the consumption of (1) ethanol and other organic solvent is big; (2) cost height; (3) production cycle is long.So just make the production and the application of flavones be subjected to very big restriction.
Purpose of the present invention just is to overcome the deficiency that existing production method exists, and a kind of new method of extracting total flavones from Ginkgo Leaf is provided.
The method of extracting total flavones from Ginkgo Leaf of the present invention comprises: will clean chopping air dried Ginkgo Leaf less water soaked overnight, alkaline water in order to saturated limewater, small amount of antioxidant preparation carries out three extractions then, filter and merge three filtrates, vacuum concentration, cooling, under agitation add a certain amount of absorptive clarificant, the insulation regular hour, centrifuging, the ethanol of adding a certain amount of 95% in filtrate, stir, add a certain amount of 5% N again
A2CO
3Making PH is 9-10, staticly settle, centrifuging, adding 10% hydrochloric acid in supernatant liquor, to pull back to PH be about 6, with D101 macroporous resin column, ethanol elution to there being the flavones reaction, after elutriant reclaims ethanol, vacuum concentration in vacuum-drying below 60 ℃, obtains certain density yellow extract to syrupy shape.
Among the present invention, its content of described small amount of antioxidant is the 0.02%-0.06% of total buck weight.
Among the present invention, described antioxidant can be N
aHSO
3Or N
A2B
4O
7
Among the present invention, described alkaline aqueous solution is meant that PH is 8～10 the aqueous solution.
Among the present invention, in described three extractions, the amount of extracting used alkaline aqueous solution for the first time is 8-12 a times of immersion leaf amount, and preferred 10 times, boiling time is 20-40min.
Among the present invention, in described three extractions, the amount of extracting used alkaline aqueous solution for the second time is 6-10 a times of immersion leaf amount, and preferred 8 times, boiling time is 10-30min.
Among the present invention, in described three extractions, the amount of extracting used alkaline aqueous solution for the third time is 5-7 a times of immersion leaf amount, preferred 6 times, and boiling time 10-30min.
Among the present invention, described extracting solution is cooled to 40-50 ℃ after concentrating.
Among the present invention, the 1-3 ‰ that the amount of described absorptive clarificant is (by concentrating the back liquid weight), preferred 1 ‰.
Among the present invention, described absorptive clarificant can be the acetyl chitosan, has commercially available.
Among the present invention, described soaking time can be insulation 3-6 hour, preferred 4 hours.
Among the present invention, the 2-4 that described 95% the alcoholic acid amount that is added in filtrate is a filtrate volume doubly.
Among the present invention, described D101 macroporous resin column has commercially available.
Among the present invention, wash-out can use 70% ethanolic soln with ethanol.
The method of from ginkgo, extracting total flavones provided by the present invention, its technology is simple, and extracting cycle is short, can save a large amount of ethanol, and reduce cost, for the mass production of flavones provides a new way.
Embodiment 1
Choose good Ginkgo Leaf 1kg and clean, chopping is dried, and uses the less water soaked overnight, then in order to saturated limewater, 0.04% (weight percent) N
aHSO
3The pH value of preparation is that 9 alkaline water extracts three times.The above-mentioned alkaline water that extracts with 9kg boiled 30 minutes for the first time, filtered; The above-mentioned alkaline water that extracts with 8kg boiled 20 minutes for the second time, filtered, and the above-mentioned alkaline water that extracts with 6kg boiled 20 minutes for the third time, filtered, and merged 3 times filtrate.Vacuum concentration, stirs when being cooled to 45 ℃ to 1000ml, adds to remove acetyl chitosan 1 gram, is incubated 4 hours, centrifuging, and 95% of adding 3000ml ethanol stirs in filtrate, adds 5% N again
A2CO
3Make PH transfer to 9, still aging, centrifuging, adding 10% hydrochloric acid in supernatant liquor, to transfer to PH be 6, last D101 macroporous resin column, ethanol elution with 70% is to there not being the flavones reaction, after elutriant reclaimed ethanol, straight sky was concentrated into syrupy shape, in vacuum-drying below 60 ℃, obtain yellow extract 76 grams, purity is 24%
Claims (13)
1, a kind of method of from Ginkgo Leaf, extracting total flavones, wherein, to clean chopping air dried Ginkgo Leaf less water soaked overnight, be that the alkaline water of the antioxidant preparation of 0.02%-0.06% carries out extracting for three times, merging three filtrates in order to saturated limewater, weight percent then, vacuum concentration, cooling, under agitation add absorptive clarificant by the 1-3 ‰ of the weight that concentrates back liquid, be incubated 3-6 hour, centrifuging, 2-4 times of the adding filtrate volume 95% ethanol stirs in filtrate, adds 5%N again
A2CO
3Make PH be 9-10, still aging, centrifuging, adding 10% hydrochloric acid in supernatant liquor, to pull back to PH be about 6, on the D101 macroporous resin column with 70% ethanol elution to there being the flavones reaction, behind the elutriant recovery ethanol, vacuum concentration is to syrupy shape, in vacuum-drying below 60 ℃.
2, the described method of claim 1, wherein said antioxidant is N
aHSO
3Or N
A2B
4O
7
3, the method described in the claim 1 or 2, the content of wherein said antioxidant are 0.04%.
4, the described method of claim 1, wherein said alkaline aqueous solution are that PH is 8～10 the aqueous solution.
5, the described method of claim 1, the amount of extracting used alkaline aqueous solution the wherein said first time are 8-12 times of immersion leaf amount, and boiling time is 20-40 minute.
6, the method described in the claim 1 or 5, the amount of extracting used alkaline aqueous solution the wherein said second time are 10 times of immersion leaf amount.
7, the described method of claim 1, the amount of extracting used alkaline aqueous solution the wherein said second time are 6-10 times of immersion leaf amount, and boiling time is 10-30 minute.
8, the method described in the claim 1 or 7, the amount of extracting used alkaline aqueous solution the wherein said second time are 8 times of immersion leaf amount.
9, the described method of claim 1, the wherein said amount of extracting used alkaline aqueous solution for the third time is 5-7 a times of immersion leaf amount, boiling time is 10-30 minute.
10, the method described in the claim 1 or 9, the wherein said amount of extracting used alkaline aqueous solution for the third time are 6 times of immersion leaf amount.
11, the described method of claim 1, wherein said absorptive clarificant is the acetyl chitosan.
12, the described method of claim 1, wherein said extracting solution is cooled to 40-50 ℃ after concentrating.
13, the described method of claim 1, wherein said soaking time is 4 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN95118737A CN1048724C (en) | 1995-11-15 | 1995-11-15 | Process for extracting total flavone from ginkgo leaf |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN95118737A CN1048724C (en) | 1995-11-15 | 1995-11-15 | Process for extracting total flavone from ginkgo leaf |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1129218A CN1129218A (en) | 1996-08-21 |
| CN1048724C true CN1048724C (en) | 2000-01-26 |
Family
ID=5081770
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN95118737A Expired - Fee Related CN1048724C (en) | 1995-11-15 | 1995-11-15 | Process for extracting total flavone from ginkgo leaf |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1048724C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100362011C (en) * | 2003-01-08 | 2008-01-16 | 浙江康恩贝制药股份有限公司 | Preparation method of ginkgo leaf extract |
Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6030621A (en) * | 1998-03-19 | 2000-02-29 | De Long; Xie | Ginkgo biloba composition, method to prepare the same and uses thereof |
| DE19829516B4 (en) * | 1998-07-02 | 2004-08-26 | Dr. Willmar Schwabe Gmbh & Co. Kg | Water-soluble native dry extract from Gingko biloba with a high content of terpenoids and flavone glycosides |
| WO2004056792A1 (en) * | 2002-11-11 | 2004-07-08 | Pro-Herb Gmbh | An organic extract of ginkgo, and the preparation method and use thereof |
| CN1318440C (en) * | 2003-01-08 | 2007-05-30 | 浙江康恩贝制药股份有限公司 | Preparation method of low-acid ginkgo leaf extract |
| EP1755629A1 (en) * | 2004-04-29 | 2007-02-28 | GOETECH GmbH | Ginkgo biloba extract and method for producing the same |
| CN100463683C (en) * | 2005-08-15 | 2009-02-25 | 黑龙江省珍宝岛制药有限公司 | Medicaments of 'thrombosis through' freezed drying powder injection (including dedicated solvent) and technique and adaptive disease |
| CN100528855C (en) * | 2005-12-27 | 2009-08-19 | 中国科学院山西煤炭化学研究所 | Process for producing kuh-seng total flavone and flavone salt by kuh-seng |
| CN101449805B (en) * | 2008-12-23 | 2012-08-08 | 浙江工业大学 | Method for extracting Gingko extract from ginkgo leaves |
| CN101703535B (en) * | 2009-11-05 | 2011-05-04 | 浙江大学 | Method for improving content of drug efficacy components of ginkgo leaf |
| CN101785559B (en) * | 2009-12-29 | 2012-08-08 | 孙羽菡 | Processing method utilizing gingko to prepare gingko detoxifying powder and co-generate crude ginkgo phenolic acid extract |
| CN101904877B (en) * | 2010-08-06 | 2011-09-28 | 合肥工业大学 | New preparation method of low-phenolic acid gingko flavone extractive |
| CN104189285A (en) * | 2014-09-12 | 2014-12-10 | 广西中医药大学 | Traditional Chinese medicine preparation with hypoglycemic effect |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04182434A (en) * | 1990-11-17 | 1992-06-30 | Seiichi Umeda | Method for acquiring ginkgo leaf extract |
| KR940002797B1 (en) * | 1989-08-09 | 1994-04-02 | 주식회사 코오롱 | Method of extraction and purification of high concentrated flavon glycosides |
| KR940002798B1 (en) * | 1989-10-06 | 1994-04-02 | 동국제약 주식회사 | Process for the extraction of flavon glycosides and its device |
-
1995
- 1995-11-15 CN CN95118737A patent/CN1048724C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR940002797B1 (en) * | 1989-08-09 | 1994-04-02 | 주식회사 코오롱 | Method of extraction and purification of high concentrated flavon glycosides |
| KR940002798B1 (en) * | 1989-10-06 | 1994-04-02 | 동국제약 주식회사 | Process for the extraction of flavon glycosides and its device |
| JPH04182434A (en) * | 1990-11-17 | 1992-06-30 | Seiichi Umeda | Method for acquiring ginkgo leaf extract |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100362011C (en) * | 2003-01-08 | 2008-01-16 | 浙江康恩贝制药股份有限公司 | Preparation method of ginkgo leaf extract |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1129218A (en) | 1996-08-21 |
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