CN106220598A - A kind of Semen Euphorbiae extracts the method for aesculetin - Google Patents
A kind of Semen Euphorbiae extracts the method for aesculetin Download PDFInfo
- Publication number
- CN106220598A CN106220598A CN201610590812.5A CN201610590812A CN106220598A CN 106220598 A CN106220598 A CN 106220598A CN 201610590812 A CN201610590812 A CN 201610590812A CN 106220598 A CN106220598 A CN 106220598A
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- CN
- China
- Prior art keywords
- extracts
- aesculetin
- semen euphorbiae
- ethyl acetate
- methanol
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/06—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 2
- C07D311/08—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 2 not hydrogenated in the hetero ring
- C07D311/16—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 2 not hydrogenated in the hetero ring substituted in position 7
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a kind of method that Semen Euphorbiae extracts aesculetin, belong to medicine, chemical technology field, aesculetin comparision contents in natural plants Cortex Fraxini is low, the content of the raw materials used Semen Euphorbiae of the present invention is higher, because aesculetin content in Cortex Fraxini is low, use traditional separation and extraction technology, quickly speed difficulty carries out high yield industrialized production while reaching purity more than 98%, the present invention develops a kind of separation and Extraction aesculetin from Semen Euphorbiae, it is not only the problem that industrialized production reduces cost, also make purity reach crude drug rank simultaneously, improve production efficiency, technical process environmental protection, to environment without serious harm.
Description
Technical field
The present invention relates to a kind of method that Semen Euphorbiae extracts aesculetin, belong to medicine, chemical technology field.
Background technology
Aesculetin is derived from Hippocastanaceae plant Aesculus hippocastanum L. bark, and feverfew Herba Cichorii herb, Rubiaceae is planted
Thing, belongs to Coumarins.Most domestic is reported as separation and Extraction from Cortex Fraxini, and comparision contents is low in Cortex Fraxini, and difficulty is relatively
Greatly.And aesculetin content about 0.6%-2% in Semen Euphorbiae, the raw material that the present invention uses is Semen Euphorbiae, solves raw material
The problem that content is low, and technique is simple, solves industrialized production problem, purity reaches the crude drug level of more than 98% simultaneously
Not.Aesculetin is a kind of antimicrobial drug, and dysentery bacterium is had inhibitory action, can be used for treating acute bacillary dysentery, and has and relieving asthma, eliminate the phlegm
Effect, it is possible to be used for treating chronic tracheitis.
Summary of the invention
It is an object of the invention to provide a kind of method that Semen Euphorbiae extracts aesculetin, so that solve cannot industrialization and pure
Spend higher problem.To achieve these goals, the present invention uses Semen Euphorbiae to be raw material, obtains filtering residue after oil expression, uses plastid ratio
Methanol eddy for 1:5 extracts 3 times, united extraction liquid, after concentration, and petroleum ether extraction 1 time, abandon upper strata, lower floor's sodium hydroxide
Solution regulation pH is 9, is extracted with ethyl acetate 3 times, then is 7 with dilute hydrochloric acid regulation pH, and ethyl acetate extracts 1 time, merges acetic acid
Ethyl ester, is evaporated to without ethyl acetate.Again with methanol recrystallization obtains sterling.
Above-mentioned a kind of Semen Euphorbiae extracts the method for aesculetin, it is characterised in that: obtain filtering residue after described oil expression, its filtering residue
Clean with a small amount of methanol.
Above-mentioned a kind of Semen Euphorbiae extracts the method for aesculetin, it is characterised in that: described plastid returns than the methanol being 1:5
Stream extracts 3 times, and its plastid ratio may range from 1:3 to 1:8.
Above-mentioned a kind of Semen Euphorbiae extracts the method for aesculetin, it is characterised in that: described petroleum ether extraction, its petroleum ether is used
Measure and extract concentrated solution ratio for 1:3.
Above-mentioned a kind of Semen Euphorbiae extracts the method for aesculetin, it is characterised in that: described sodium hydroxide solution regulates pH
Being 9 to make all to dissolve, its PH scope is 8-9, is allowed to all dissolve
Above-mentioned a kind of Semen Euphorbiae extracts the method for aesculetin, it is characterised in that be extracted with ethyl acetate described in:, its acetic acid
Ethyl ester consumption is 3 times of liquid to be extracted.
Above-mentioned a kind of Semen Euphorbiae extracts the method for aesculetin, it is characterised in that: described recrystallizing methanol, its plastid ratio
For 1:15
Aesculetin structural formula is as follows:
Accompanying drawing explanation
Fig. 1 is the present invention final sterling HPLC collection of illustrative plates.
Fig. 2 is the present invention final sterling MS collection of illustrative plates.
Detailed description of the invention
Embodiment:
Described a kind of Semen Euphorbiae extracts the method for aesculetin: takes 3Kg Semen Euphorbiae, obtains filtering residue after oil expression, uses 0.5L first
Alcohol filter wash slag, adds 30L methanol, refluxes 3 hours, extract 3 times, after merging, reduce pressure 85 DEG C after being concentrated into without alcohol, obtain concentrated solution
1L, with 2.2L petroleum ether extraction 1 time, abandons upper strata, and lower floor's aqueous phase has a small amount of precipitation, is 9 with sodium hydroxide solution regulation pH, is allowed to
All dissolve, extract 3 times by 6L ethyl acetate, then with dilute hydrochloric acid regulation to neutral, 0.8L ethyl acetate extracts 1 time, merges second
Acetoacetic ester, is evaporated to obtain 36g yellow powder without ethyl acetate, then obtains 27.5g sterling Cortex Fraxini by 700mL recrystallizing methanol
B prime content is 98%.
Claims (7)
1. the method that Semen Euphorbiae extracts aesculetin, the present invention uses Semen Euphorbiae to be raw material, obtains filtering residue, use matter after oil expression
Body extracts 3 times than the methanol eddy for 1:5, united extraction liquid, after concentration, and petroleum ether extraction 1 time, abandon upper strata, lower floor's hydrogen-oxygen
Changing sodium solution regulation pH is 9, is extracted with ethyl acetate 3 times, then is 7 with dilute hydrochloric acid regulation pH, and ethyl acetate extracts 1 time, merges
Ethyl acetate, is evaporated to without ethyl acetate.Again with methanol recrystallization obtains sterling.
A kind of Semen Euphorbiae the most as claimed in claim extracts the method for aesculetin, it is characterised in that: filtered after described oil expression
Slag, its filtering residue cleans with a small amount of methanol.
A kind of Semen Euphorbiae the most as claimed in claim extracts the method for aesculetin, it is characterised in that: it is characterized in that: described stone
Oil ether extraction, its petroleum ether consumption with extract concentrated solution ratio for 1:3.
A kind of Semen Euphorbiae the most as claimed in claim extracts the method for aesculetin, it is characterised in that: described sodium hydroxide is molten
Liquid regulation pH is 9 to make all to dissolve, and its pH scope is 8-9, is allowed to all dissolve.
A kind of Semen Euphorbiae the most as claimed in claim extracts the method for aesculetin, it is characterised in that: described ethyl acetate extracts
Taking, its ethyl acetate consumption is 3 times of liquid to be extracted.
A kind of Semen Euphorbiae the most as claimed in claim extracts the method for aesculetin, it is characterised in that: described recrystallizing methanol,
Its plastid is than for 1:15.
A kind of Semen Euphorbiae the most as claimed in claim extracts the method for aesculetin: takes 3Kg Semen Euphorbiae, obtains filtering residue after oil expression,
With 0.5L methanol filter wash slag, add 30L methanol, reflux 3 hours, extract 3 times, after merging, reduce pressure 85 DEG C after being concentrated into without alcohol,
Concentrated solution 1L, with 2.2L petroleum ether extraction 1 time, abandons upper strata, and lower floor's aqueous phase has a small amount of precipitation, with sodium hydroxide solution regulation pH is
9, it is allowed to all dissolve, extracts 3 times by 6L ethyl acetate, then with dilute hydrochloric acid regulation to neutral, 0.8L ethyl acetate extracts 1 time,
Combined ethyl acetate, is evaporated to obtain yellow powder without ethyl acetate, and again with methanol recrystallization obtains sterling.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610590812.5A CN106220598A (en) | 2016-07-25 | 2016-07-25 | A kind of Semen Euphorbiae extracts the method for aesculetin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610590812.5A CN106220598A (en) | 2016-07-25 | 2016-07-25 | A kind of Semen Euphorbiae extracts the method for aesculetin |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106220598A true CN106220598A (en) | 2016-12-14 |
Family
ID=57532912
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610590812.5A Pending CN106220598A (en) | 2016-07-25 | 2016-07-25 | A kind of Semen Euphorbiae extracts the method for aesculetin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106220598A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115996738A (en) * | 2020-05-18 | 2023-04-21 | 塞尔比泰克有限责任公司 | Drug delivery system based on bioactive compound functionalized calcium phosphate nanoparticles from euphorbia pekinensis extract and uses thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103408522A (en) * | 2013-08-22 | 2013-11-27 | 乐山师范学院 | Method for extracting high-purity aesculetin from euphorbia lathyris fruit |
-
2016
- 2016-07-25 CN CN201610590812.5A patent/CN106220598A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103408522A (en) * | 2013-08-22 | 2013-11-27 | 乐山师范学院 | Method for extracting high-purity aesculetin from euphorbia lathyris fruit |
Non-Patent Citations (4)
| Title |
|---|
| 于玲等: "秦皮中秦皮乙素的提取纯化工艺研究", 《安徽农业科学》 * |
| 孙国君等: "千金子化学成分和药理活性研究进展", 《中药材》 * |
| 封家福等: "千金子中6，7-二羟基香豆素的分离鉴定及抗氧化活性研究", 《油脂加工》 * |
| 张建业等: "千金子的乙酸乙醋萃取物抗肿瘤活性部位研究", 《内蒙古中医药》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115996738A (en) * | 2020-05-18 | 2023-04-21 | 塞尔比泰克有限责任公司 | Drug delivery system based on bioactive compound functionalized calcium phosphate nanoparticles from euphorbia pekinensis extract and uses thereof |
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| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20161214 |
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| WD01 | Invention patent application deemed withdrawn after publication |