CN1058628C - Method for extracting flavone and terlactone from ginkgo leaf by supercritical carbon dioxide - Google Patents
Method for extracting flavone and terlactone from ginkgo leaf by supercritical carbon dioxide Download PDFInfo
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- CN1058628C CN1058628C CN97116799A CN97116799A CN1058628C CN 1058628 C CN1058628 C CN 1058628C CN 97116799 A CN97116799 A CN 97116799A CN 97116799 A CN97116799 A CN 97116799A CN 1058628 C CN1058628 C CN 1058628C
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- extraction
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- gingko
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- 241000218628 Ginkgo Species 0.000 title claims abstract description 20
- 235000011201 Ginkgo Nutrition 0.000 title claims abstract description 20
- 235000008100 Ginkgo biloba Nutrition 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 14
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 title claims description 12
- 229910002092 carbon dioxide Inorganic materials 0.000 title claims description 6
- 239000001569 carbon dioxide Substances 0.000 title claims description 5
- 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 description 2
- 229930003944 flavone Natural products 0.000 title description 2
- 150000002212 flavone derivatives Chemical class 0.000 title description 2
- 235000011949 flavones Nutrition 0.000 title description 2
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 title description 2
- 238000000605 extraction Methods 0.000 claims abstract description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- -1 terpene lactone Chemical class 0.000 claims abstract description 11
- 235000007586 terpenes Nutrition 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000003607 modifier Substances 0.000 claims description 12
- AIFCFBUSLAEIBR-UHFFFAOYSA-N ginkgetin Chemical class C=1C(OC)=CC(O)=C(C(C=2)=O)C=1OC=2C(C=1)=CC=C(OC)C=1C1=C(O)C=C(O)C(C(C=2)=O)=C1OC=2C1=CC=C(O)C=C1 AIFCFBUSLAEIBR-UHFFFAOYSA-N 0.000 claims description 8
- 230000003068 static effect Effects 0.000 claims description 4
- 238000004090 dissolution Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 230000008676 import Effects 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 229930003935 flavonoid Natural products 0.000 abstract description 5
- 150000002215 flavonoids Chemical class 0.000 abstract description 5
- 235000017173 flavonoids Nutrition 0.000 abstract description 5
- 150000007965 phenolic acids Chemical class 0.000 abstract description 2
- 239000011347 resin Substances 0.000 abstract description 2
- 229920005989 resin Polymers 0.000 abstract description 2
- 244000194101 Ginkgo biloba Species 0.000 abstract 6
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 239000000284 extract Substances 0.000 description 5
- IYRMWMYZSQPJKC-UHFFFAOYSA-N kaempferol Chemical compound C1=CC(O)=CC=C1C1=C(O)C(=O)C2=C(O)C=C(O)C=C2O1 IYRMWMYZSQPJKC-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- 235000013824 polyphenols Nutrition 0.000 description 2
- QLHSZVGLSUHUOI-UHFFFAOYSA-N 3,5,6-trihydroxy-2-phenylchromen-4-one Chemical compound OC=1C(=O)C2=C(O)C(O)=CC=C2OC=1C1=CC=CC=C1 QLHSZVGLSUHUOI-UHFFFAOYSA-N 0.000 description 1
- 208000024172 Cardiovascular disease Diseases 0.000 description 1
- UBSCDKPKWHYZNX-UHFFFAOYSA-N Demethoxycapillarisin Natural products C1=CC(O)=CC=C1OC1=CC(=O)C2=C(O)C=C(O)C=C2O1 UBSCDKPKWHYZNX-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 206010044565 Tremor Diseases 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229930184727 ginkgolide Natural products 0.000 description 1
- MWDZOUNAPSSOEL-UHFFFAOYSA-N kaempferol Natural products OC1=C(C(=O)c2cc(O)cc(O)c2O1)c3ccc(O)cc3 MWDZOUNAPSSOEL-UHFFFAOYSA-N 0.000 description 1
- 235000008777 kaempferol Nutrition 0.000 description 1
- 150000002596 lactones Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- UXOUKMQIEVGVLY-UHFFFAOYSA-N morin Natural products OC1=CC(O)=CC(C2=C(C(=O)C3=C(O)C=C(O)C=C3O2)O)=C1 UXOUKMQIEVGVLY-UHFFFAOYSA-N 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 210000000582 semen Anatomy 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- ARSRJFRKVXALTF-UHFFFAOYSA-N tricetin Chemical compound C=1C(O)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC(O)=C(O)C(O)=C1 ARSRJFRKVXALTF-UHFFFAOYSA-N 0.000 description 1
- CMPNIWQMRYYTMK-UHFFFAOYSA-O tricetinidin Natural products [O+]=1C2=CC(O)=CC(O)=C2C=CC=1C1=CC(O)=C(O)C(O)=C1 CMPNIWQMRYYTMK-UHFFFAOYSA-O 0.000 description 1
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Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Medicines Containing Plant Substances (AREA)
Abstract
The present invention relates to a method for extracting gingko flavonoid and gingko terpene lactone from ginkgo by supercritical CO2, which comprises the steps that a polar modifying agent containing 70% of ethanol and 30% of water is added into gingko under pressure to be extracted at a temperature of 60 to 80 DEG C under a pressure of 20 to 30 megapascals for 2 to 3 hours; then, the gingko is concentrated by the macroporous resin in the prior art, the gingko flavonoid content in the extractants reaches as high as 37%, the gingko terpene lactone content is 8%, and the phenolic acid content is less than 4PPM. The method has the advantage of short flow path, and the extraction rate reaches as high as 85%.
Description
The present invention relates to take supercritical from Folium Ginkgo, to extract the method for ginkgetin class and Folium Ginkgo terpene lactones class.
In recent years, find the ginkgetin class (for example trihydroxyflavone alcohol Kaempferol and Tricetin Quericetin) in the Folium Ginkgo in the world of medicine, and Folium Ginkgo terpene lactones (for example Ginkgolides and bibolalide), for treatment cardiovascular diseases and cerebrovascular peculiar curative effect is arranged.But mostly be to adopt chemical solvent to extract, not only technological process is long, and solvent-oil ratio is big, the main product quality shakiness of being extracted, and yield is low.
The object of the present invention is to provide a kind of method that adopts supercritical carbon dioxide from Folium Ginkgo, to extract ginkgetin class and Folium Ginkgo terpene lactones class.
Embodiment of the present invention are as follows:
I, adopting supercritical CO
2Add the method that extracts ginkgetin class and Folium Ginkgo terpene lactones class with the polarity modifier of ethanol and aqueous mixtures.
Ii, its process conditions are as follows:
The volume ratio of two components is an ethanol in the polarity modifier: water=(60-90): (40: 10)
Extracting pressure is 20-30 MPa (MPa)
Extraction temperature is 60-80 ℃
The extraction time is 2-5 hour (wherein static extracting 1-2 hour, dynamic extraction is 1-4 hour)
The iii technological process is as follows: (consulting accompanying drawing)
To clean that to carry out grinding particle size be that 20 purpose Folium Ginkgos are put into extraction kettle, be warmed up to 60-80 ℃, start CO
2Pump, boost to 20-30MPa and enter in the extraction kettle static dissolution extraction 1-2 hour, start the modifier pump then and import polarity modifier simultaneously, dynamic extraction 1-4 hour by preheater.From two separators, tell product, CO
2Gas enters refrigerator, is condensed into liquid and is recycled to CO
2Pump.
Following preference is described in detail the present invention in conjunction with the accompanying drawings, but does not mean that limitation of the scope of the invention.
Example 1 is put into extraction kettle for 4.5 kilograms with the Folium Ginkgo (containing flavonoid 1.0%) of cleaning airing and is warmed up to 70 ℃, starts CO
2Pump boosts to 25MPa, be heated to 70 ℃ by preheater, the polarity modifier of 70% ethanol and 30% water enters extraction kettle after by preheater simultaneously, under 70 ℃, carried out dynamic dissolution extraction 3 hours, the flow of polarity modifier and the flow-rate ratio of carbon dioxide are 20: 80, then, and sample analysis from two height separators, obtain 0.17 kilogram of extract with the general analysis of color, see the following form:
The material flavonoid content % extraction time (time) extraction yield %
Stock silver Folium Pruni 1.0
Raffinate 0.3 3 70
Raffinate 0.15 4 85
Semen Ginkgo extrac again by prior art through the large aperture resin concentrate refining after in the extract ginkgetin class content reach 37%, Folium Ginkgo terpene lactones class 8.2%, phenolic content is less than 4PPM.
Example 2, removing extraction temperature is 80 ℃, pressure is 30 MPas, time is 5 hours, and the volume ratio of ethanol and water is outside 90: 10 in the polarity modifier, and all the other conditions are 80% with the example 1 identical extraction yield that records, after concentrating, ginkgetin class content is 38% in the extract, and the Folium Ginkgo terpene lactones class is 8.5%, and phenolic content is less than 5PPM.
Advantage of the present invention is as follows:
1, equipment is simple, and flow process is short, and extraction yield is up to 80%
2、CO
2Can recycle, consume few.
3, extract composition containing ginkgo flavonoids up to 37%, ginkgoterpene lactone class content also up to 8% with On, and the nuisance phenolic acid is less than 4PPM. Fig. 1: the 1.CO2 high-pressure pump, 2. modifier pump, 3. preheater, 4. extraction kettle,
5. separating still, 6. separating still, 7. refrigerator
Claims (2)
1, a kind of method that adopts supercritical carbon dioxide to extract ginkgetin class and Folium Ginkgo terpene lactones class from Folium Ginkgo is characterized in that:
Add polarity modifier in a, the extracting solution, wherein ethanol: the volume ratio of water is 60-90: 40: 10
B, extracting pressure are the 20-30 MPa, and temperature is 60-80 ℃, and the time is 2-5 hour
The volume ratio of c, polarity modifier and liquid CO 2 is 20: 80
D, technological process will be for will clean airing, and grinding particle size is that 20 purpose Folium Ginkgos are put into extraction kettle, and liter, temperature are started CO to 60-80 ℃
2Pump, boost to the 20-30 MPa, enter in the extraction kettle by preheater, static dissolution extraction 1-2 hour, the modifier pump of paying wages then, import polarity modifier simultaneously, dynamic extraction 1-4 hour, from two separators, tell product ginkgetin class and Folium Ginkgo terpene lactones class, CO
2Gas enters refrigerator, is condensed into liquid and is recycled to CO
2Pump.
2, according to the method for right 1, it is characterized in that: described extracting pressure is 25 MPas, and described extraction temperature is 70 ℃, and the described extraction time is static 1 hour, moves to reach 3 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97116799A CN1058628C (en) | 1997-08-22 | 1997-08-22 | Method for extracting flavone and terlactone from ginkgo leaf by supercritical carbon dioxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97116799A CN1058628C (en) | 1997-08-22 | 1997-08-22 | Method for extracting flavone and terlactone from ginkgo leaf by supercritical carbon dioxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1172670A CN1172670A (en) | 1998-02-11 |
| CN1058628C true CN1058628C (en) | 2000-11-22 |
Family
ID=5174110
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN97116799A Expired - Fee Related CN1058628C (en) | 1997-08-22 | 1997-08-22 | Method for extracting flavone and terlactone from ginkgo leaf by supercritical carbon dioxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1058628C (en) |
Families Citing this family (7)
| 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 |
| CN1094385C (en) * | 1999-01-25 | 2002-11-20 | 南开大学 | Modified natural macromolecular compound adsorbent and application thereof |
| CN1073562C (en) * | 1999-02-05 | 2001-10-24 | 孙传经 | Method for extracting material containing raw anthocyanidin from ginkgo leaf by supercritical carbon dioxide |
| US6524628B1 (en) * | 2000-11-06 | 2003-02-25 | Idaho Research Foundation, Inc. | Pressurized water extraction |
| CN1634925B (en) * | 2004-10-21 | 2010-04-28 | 潘见 | Separation and purification method for ginkgolide monomer |
| CN106038619B (en) * | 2016-06-08 | 2019-08-23 | 河南骏化发展股份有限公司 | A kind of ginkgo biloba p.e and preparation method thereof |
| CN106727745B (en) * | 2017-02-15 | 2021-01-01 | 宁波中药制药股份有限公司 | Method for preparing low-acid ginkgo leaf extract |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1085091A (en) * | 1993-05-31 | 1994-04-13 | 周维书 | With Folium Ginkgo with contain the Saponin plant and make the DANFU square preparation of preventing and treating cardiovascular and cerebrovascular vessel disease |
-
1997
- 1997-08-22 CN CN97116799A patent/CN1058628C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1085091A (en) * | 1993-05-31 | 1994-04-13 | 周维书 | With Folium Ginkgo with contain the Saponin plant and make the DANFU square preparation of preventing and treating cardiovascular and cerebrovascular vessel disease |
Non-Patent Citations (1)
| Title |
|---|
| 中国医药工业杂志1995,26(11) 1995.1.1 彭洪等，超临界二氧化碳萃取技术在生活活性物质萃取上的应用 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1172670A (en) | 1998-02-11 |
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