CN1059825C - Method for extracting and separating flavone and terlactone from ginkgo leaf by supercritical carbon dioxide - Google Patents
Method for extracting and separating flavone and terlactone from ginkgo leaf by supercritical carbon dioxide Download PDFInfo
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- CN1059825C CN1059825C CN97116798A CN97116798A CN1059825C CN 1059825 C CN1059825 C CN 1059825C CN 97116798 A CN97116798 A CN 97116798A CN 97116798 A CN97116798 A CN 97116798A CN 1059825 C CN1059825 C CN 1059825C
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Abstract
The present invention relates to a method for extracting and separating ginkgetin and ginkgo terpene lactones from ginkgo leaves by adopting supercritical carbon dioxide, which comprises: adopting a composition of 3 to 7% of ethanol and 93 to 97% of water as a polar modifying agent; extracting the ginkgo leaves for 3 to 5 hours in a dynamic manner to discharge extraction residues containing 22 to 26% of ginkgetin in an extraction kettle and separate extracts containing 85 to 90% of ginkgo terpene lactones in a separator at an extraction temperature of 50 to 60 DEG C and under the pressure of 25 to 35 megapascals.
Description
The present invention relates to a kind of employing supercritical CO
2The method of extract and separate ginkgetin class and Folium Ginkgo terpene lactones class from Folium Ginkgo.
As everyone knows, the ginkgetin class and the Folium Ginkgo terpene lactones class mixture that from Folium Ginkgo, extract at present, mostly be to adopt the chemical solvent method, its shortcoming is that solvent-oil ratio is big, flow process is numerous and diverse and extraction yield is extremely low, the former is effective especially for the treatment cardiovascular diseases, and therefore the latter then evident in efficacy for the treatment cerebrovascular, how to work out one-step extracting and divides the problem that to exceed this two component be current the world of medicine.
The object of the present invention is to provide the super CO that faces of a kind of employing
2From Folium Ginkgo one-step extracting and isolate ginkgetin class (as trihydroxyflavone alcohol Kaempferol etc.) and the Folium Ginkgo terpene lactones class as the method for (as Ginkgolides).
This embodiment is as follows: add in extraction process and with 3-7% ethanol and 93-97% aqueous polar modifier strong polar ginkgetin class is not extracted to stay in the extraction kettle, semipolar Folium Ginkgo terpene lactones class then can be extracted, and separates from separator.Its extraction process condition is:
Folium Ginkgo is packed in the extraction kettle, be warmed up to 50-60 ℃, start CO
2Pump boosts to the 25-35 MPa, starts the modifier pump and makes CO
2Preheating in preheater enters extraction kettle again with modifier, dynamic extraction 3-5 hour, left alone without help pump blood pressure lowering, emits the extract that contains the ginkgetin class, the separating medium of emitting the Folium Ginkgo terpene lactones class in separator in extraction kettle.
Following preference is described in detail the present invention, but does not mean that limitation of the scope of the invention in conjunction with flow chart.
Example 1, the Semen Ginkgo pyrite class that contains that will clean airing are 7 kilograms of 1% Folium Ginkgos, put into general extraction kettle, be warmed up to 58 ℃, start CO
2Pump, boost to 30 MPas, with flow velocity be 30 liters/time, be preheating to 58 ℃ by preheater, start the modifier pump simultaneously, with flow velocity be 1.5 liters/time send 5% ethanol, the modifier that 95% water is formed is also by preheater and be preheating to 58 ℃, and these two bursts of logistics are all by extractor and two placed in-line separators, gaseous state CO
2Be condensed into the liquid recirculation by refrigerator and return CO
2Pump, dynamic extraction be after 4 hours, termination of pumping, emits to contain 6.6 kilograms of ginkgetin class raffinate and respectively emit the 0.4 kilogram of analysis result of extract that contains Folium Ginkgo terpene lactones class mixture from 2 series connection separators from extractor and see Table 1
Table 1
| Extraction kettle | Separating still | ||||
| Example | Folium Ginkgo weight (kilogram) before the extraction | Extraction back raffinate weight (kilogram) | Raffinate contains flavone % | Extract weight (kilogram) | Contain terpene lactones % |
| 1 | 7.0 | 6.6 | 26 | 0.4 | 80 |
| 2 | 7.0 | 6.4 | 24 | 0.6 | 85 |
Example 2, remove extraction temperature and change 52 ℃ into, extracting pressure changes 25 MPas into, it is that 3% water is to change into outside 3 hours 97% compositions and extraction time that modifier changes ethanol into, and all the other conditions are identical with example 1, each gets 6.4 kilograms of the apricot yellow ketone raffinate of argentiferous and contains 0.6 kilogram of Semen Ginkgo terpene lactones extract.Analysis result also sees Table 1.
Advantage of the present invention is:
1, yield was high at a high speed soon in short minute for flow process.
2, extraction, thing argentiferous flavonoids be up to more than 22%, and lactone content is below 0.01%, high this 85-90% of extract composition containing ginkgo terpene lactones in the separator.
Fig. 1. 1. CO2 high-pressure pump, 2. modifier pump, 3 preheaters, 4. extraction kettle,
5. separating still, 6. separating still, 7. refrigerator
Claims (2)
1, a kind of method that adopts supercritical carbon dioxide extract and separate ginkgetin class and Folium Ginkgo terpene lactones class from Folium Ginkgo, it is characterized in that: Folium Ginkgo is packed in the extraction kettle, be warmed up to 50-60 ℃, start carbon dioxide pump, boost to the 25-35 MPa, flow velocity be 30 liters/time, start the modifier pump with flow velocity be 1.5 liters/time send 5% ethanol, the modifier that 95% water is formed is also by the preheating and send into extraction kettle in preheater of preheater carbon dioxide and modifier, dynamic extraction 3-5 hour, termination of pumping, blood pressure lowering, emit from extraction kettle and to contain ginkgetin class raffinate and in separator, to emit Folium Ginkgo terpene lactones class extract.
2, according to the method for claim 1, it is characterized in that: following extraction conditions is:
A, extraction temperature are 58 ℃, and extracting pressure is 30 MPas, and the extraction time is 4 hours
B, modifier contain the compositions of 5% ethanol, 95% water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97116798A CN1059825C (en) | 1997-08-22 | 1997-08-22 | Method for extracting and separating flavone and terlactone from ginkgo leaf by supercritical carbon dioxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97116798A CN1059825C (en) | 1997-08-22 | 1997-08-22 | Method for extracting and separating flavone and terlactone from ginkgo leaf by supercritical carbon dioxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1172669A CN1172669A (en) | 1998-02-11 |
| CN1059825C true CN1059825C (en) | 2000-12-27 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN97116798A Expired - Fee Related CN1059825C (en) | 1997-08-22 | 1997-08-22 | Method for extracting and separating flavone and terlactone from ginkgo leaf by supercritical carbon dioxide |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN1236836C (en) * | 2003-12-08 | 2006-01-18 | 曹培生 | A process for extraction and apparatus thereof |
| CN100343375C (en) * | 2005-08-11 | 2007-10-17 | 江苏同源堂生物工程有限公司 | Supercritical carbon dioxide extraction method for extracting gingko oil from gingko fruit |
| CN101905090B (en) * | 2010-05-31 | 2012-08-15 | 中国农业大学 | Method for extracting polar or medium polar plant source natural product |
| CN106726806B (en) * | 2016-11-23 | 2020-10-09 | 烟台新时代健康产业日化有限公司 | Supercritical extraction method for extracting effective components from pine pollen |
| 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 |
|---|---|---|---|---|
| US5178735A (en) * | 1987-09-07 | 1993-01-12 | Chlorine Engineers | Process for the supercritical extraction and separation of solid samples |
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1997
- 1997-08-22 CN CN97116798A patent/CN1059825C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5178735A (en) * | 1987-09-07 | 1993-01-12 | Chlorine Engineers | Process for the supercritical extraction and separation of solid samples |
Non-Patent Citations (3)
| Title |
|---|
| 《中药》1995.3.30 姚崴溪 * |
| 《中药药剂学》1986.11.30 曹春林主编 * |
| 《中药药剂学》1986.11.30 曹春林主编;《中药》1995.3.30 姚崴溪 * |
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| CN1172669A (en) | 1998-02-11 |
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