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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 PDF

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Publication number
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
hour
gingko
class
pump
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Expired - Fee Related
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CN97116799A
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CN1172670A (en
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孙云鹏
孙明华
孙传经
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孙云鹏
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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • Y02P20/54Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

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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 method of supercritical carbon dioxide extracting flavone and terpene lactones from Folium Ginkgo
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.
CN97116799A 1997-08-22 1997-08-22 Method for extracting flavone and terlactone from ginkgo leaf by supercritical carbon dioxide Expired - Fee Related CN1058628C (en)

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

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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

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CN1172670A CN1172670A (en) 1998-02-11
CN1058628C true CN1058628C (en) 2000-11-22

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Families Citing this family (7)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
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

Patent Citations (1)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
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 *

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