CN102850305A - Preparation process of Forrestiin A - Google Patents
Preparation process of Forrestiin A Download PDFInfo
- Publication number
- CN102850305A CN102850305A CN2012103666640A CN201210366664A CN102850305A CN 102850305 A CN102850305 A CN 102850305A CN 2012103666640 A CN2012103666640 A CN 2012103666640A CN 201210366664 A CN201210366664 A CN 201210366664A CN 102850305 A CN102850305 A CN 102850305A
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- ether
- extract
- ginger
- extraction
- lobe
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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)
- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
Abstract
The invention provides a preparation process of Forrestiin A. The process comprises the following steps of: smashing dry roots of Hedychium forrestii until the particle size is 20-40 meshes, feeding the smashed dry root into an extraction kettle, introducing liquid CO2 and an entrainer, and performing supercritical extraction so as to obtain an oily extract; extracting the extract with ether for multiple times; concentrating obtained extract liquor to obtain an ether extract; carrying out column chromatography on silica gel and normal hexane-ether gradient elution on the ether extract; performing rotary evaporation and concentration on an eluent; and drying to obtain a Forrestiin A product. The method has the advantages of high efficiency and low pollution, and is suitable for industrial production.
Description
Technical field
The invention belongs to the extract Technique of Chinese Medicine Efficacious Ingredient field, relate to a kind of preparation technology who justifies lobe ginger florigen A.
Background technology
Circle lobe ginger florigen A(Forrestiin A), molecular formula is C
20H
26O
4, molecular weight is 330.42, derives from Zingiber (Zingiberaceae) circle lobe ginger
Hedychium forrestiiThe Diels root is a kind of diterpene-kind compound.Circle lobe ginger florigen A has cytotoxic activity, to the IC of KB cell
50Be 18.96 μ g/ml, be used for antitumor, human body nasopharyngeal carcinoma etc. on the modern medicine.
At present, the domestic extracting method of round lobe ginger florigen A and the Patents of technique of there is no.
Summary of the invention
The purpose of this invention is to provide a kind of preparation technology who justifies lobe ginger florigen A.
To achieve these goals, the present invention is by the following technical solutions:
A kind of preparation technology who justifies lobe ginger florigen A is characterized in that may further comprise the steps: the dry root of circle lobe ginger, be crushed to the 20-40 order, and drop into extraction kettle, pass into liquid CO
2Carry out supercritical extraction with entrainment agent, obtain the oily extract, with extract with extracted with diethyl ether repeatedly, get ether medicinal extract after the gained extraction liquid is concentrated, ether medicinal extract is by silica gel column chromatography, normal hexane-ether gradient elution, the elutriant rotary evaporation is concentrated, is drying to obtain round lobe ginger florigen A product.
Described supercritical CO
2Extraction conditions is: extraction temperature is that 35 ~ 50 ℃, pressure are that 25 ~ 30MPa, time are 2 ~ 4h, CO
2Flow is 15 ~ 25L/h, and take ethanol as entrainment agent, the consumption of entrainment agent is 10 ~ 30% of material quantity, 30 ~ 40 ℃ of resolution temperatures, pressure 8 ~ 10MPa.
Described silicagel column blade diameter length ratio is 1:10-15, and normal hexane-ether mixed solvent by volume 1:1,1:3,1:7 carries out gradient elution.
Advantage of the present invention is: the present invention adopts supercritical CO
2Extraction, cleanliness without any pollution, silica gel column chromatography, separation efficiency is high, can improve product purity.
Embodiment:
Embodiment 1:
The dry root of circle lobe ginger is pulverized, crossed 20 mesh sieves, get 5kg and drop in the extraction kettle, pass into the CO that is in supercritical state
2Extract, set the extraction kettle parameter: 38 ℃ of extraction temperature, pressure is 25MPa, passes into CO
2Flow is 15L/h, after the extractor homeostasis, pass into 1500ml ethanol and participate in extraction as entrainment agent, behind the extraction 2h, resolve 35 ℃ of resolution temperatures, pressure 8.5MPa, from separating still, collect the oily extract, extract is extracted 4 times repeatedly with ether, merge ether extraction liquid, obtain ether medicinal extract after concentrating.Ether medicinal extract mixed with proper silica gel mix thoroughly, silica gel dress post (post blade diameter length ratio 1:10) with 5 times of amounts of medicinal extract, to mix sample silica gel and place capital, 1:1,1:3,1:7 carry out gradient elution by volume with normal hexane-ether, the thin layer tracking monitor, the flow point of collection circle lobe ginger florigen A, rotary evaporation concentrates, is drying to obtain round lobe ginger florigen A product, HPLC detects, and purity is 67.3%.
Embodiment 2:
The dry root of circle lobe ginger is pulverized, crossed 40 mesh sieves, get 5kg and drop in the extraction kettle, pass into the CO that is in supercritical state
2Extract, set the extraction kettle parameter: 35 ℃ of extraction temperature, pressure is 28MPa, passes into CO
2Flow is 20L/h, after the extractor homeostasis, pass into 500ml ethanol and participate in extraction as entrainment agent, behind the extraction 4h, resolve 35 ℃ of resolution temperatures, pressure 9.5MPa, from separating still, collect the oily extract, extract is extracted 5 times repeatedly with ether, merge ether extraction liquid, obtain ether medicinal extract after concentrating.Ether medicinal extract mixed with proper silica gel mix thoroughly, silica gel dress post (post blade diameter length ratio 1:8) with 4 times of amounts of medicinal extract, to mix sample silica gel and place capital, 1:1,1:3,1:7 carry out gradient elution by volume with normal hexane-ether, the thin layer tracking monitor, the flow point of collection circle lobe ginger florigen A, rotary evaporation concentrates, is drying to obtain round lobe ginger florigen A product, HPLC detects, and purity is 67.2%.
Embodiment 3:
The dry root of circle lobe ginger is pulverized, crossed 40 mesh sieves, get 5kg and drop in the extraction kettle, pass into the CO that is in supercritical state
2Extract, set the extraction kettle parameter: 53 ℃ of extraction temperature, pressure is 29MPa, passes into CO
2Flow is 22L/h, after the extractor homeostasis, pass into 1000ml ethanol and participate in extraction as entrainment agent, behind the extraction 2h, resolve 40 ℃ of resolution temperatures, pressure 10MPa, from separating still, collect the oily extract, extract is extracted 6 times repeatedly with ether, merge ether extraction liquid, obtain ether medicinal extract after concentrating.Ether medicinal extract mixed with proper silica gel mix thoroughly, silica gel dress post (post blade diameter length ratio 1:15) with 6 times of amounts of medicinal extract, to mix sample silica gel and place capital, 1:1,1:3,1:7 carry out gradient elution by volume with normal hexane-ether, the thin layer tracking monitor, the flow point of collection circle lobe ginger florigen A, rotary evaporation concentrates, is drying to obtain round lobe ginger florigen A product, HPLC detects, and purity is 69.0%.
Embodiment 4:
The dry root of circle lobe ginger is pulverized, crossed 20 mesh sieves, get 5kg and drop in the extraction kettle, pass into the CO that is in supercritical state
2Extract, set the extraction kettle parameter: 60 ℃ of extraction temperature, pressure is 30MPa, passes into CO
2Flow is 25L/h, after the extractor homeostasis, pass into 750ml ethanol and participate in extraction as entrainment agent, behind the extraction 3h, resolve 30 ℃ of resolution temperatures, pressure 8MPa, from separating still, collect the oily extract, extract is extracted 4 times repeatedly with ether, merge ether extraction liquid, obtain ether medicinal extract after concentrating.Ether medicinal extract mixed with proper silica gel mix thoroughly, silica gel dress post (post blade diameter length ratio 1:15) with 5 times of amounts of medicinal extract, to mix sample silica gel and place capital, 1:1,1:3,1:7 carry out gradient elution by volume with normal hexane-ether, the thin layer tracking monitor, the flow point of collection circle lobe ginger florigen A, rotary evaporation concentrates, is drying to obtain round lobe ginger florigen A product, HPLC detects, and purity is 67.9%.
Claims (3)
1. a preparation technology who justifies lobe ginger florigen A is characterized in that may further comprise the steps: justify the dry root of lobe ginger, be crushed to the 20-40 order, drop into extraction kettle, pass into liquid CO
2Carry out supercritical extraction with entrainment agent, obtain the oily extract, with extract with extracted with diethyl ether repeatedly, get ether medicinal extract after the gained extraction liquid is concentrated, ether medicinal extract is by silica gel column chromatography, normal hexane-ether gradient elution, the elutriant rotary evaporation is concentrated, is drying to obtain round lobe ginger florigen A product.
2. a kind of preparation technology who justifies lobe ginger florigen A according to claim 1 is characterized in that described supercritical CO
2Extraction conditions is: extraction temperature is that 35 ~ 50 ℃, pressure are that 25 ~ 30MPa, time are 2 ~ 4h, CO
2Flow is 15 ~ 25L/h, and take ethanol as entrainment agent, the consumption of entrainment agent is 10 ~ 30% of material quantity, 30 ~ 40 ℃ of resolution temperatures, pressure 8 ~ 10MPa.
3. a kind of preparation technology who justifies lobe ginger florigen A according to claim 1 is characterized in that described silicagel column blade diameter length ratio is 1:10-15, and normal hexane-ether mixed solvent by volume 1:1,1:3,1:7 carries out gradient elution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012103666640A CN102850305A (en) | 2012-09-28 | 2012-09-28 | Preparation process of Forrestiin A |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012103666640A CN102850305A (en) | 2012-09-28 | 2012-09-28 | Preparation process of Forrestiin A |
Publications (1)
| Publication Number | Publication Date |
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| CN102850305A true CN102850305A (en) | 2013-01-02 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012103666640A Pending CN102850305A (en) | 2012-09-28 | 2012-09-28 | Preparation process of Forrestiin A |
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| CN (1) | CN102850305A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113730522A (en) * | 2021-09-28 | 2021-12-03 | 贵州大学 | Application of Pu' er ginger flower volatile oil in preparation of antibacterial or anti-inflammatory drugs |
-
2012
- 2012-09-28 CN CN2012103666640A patent/CN102850305A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113730522A (en) * | 2021-09-28 | 2021-12-03 | 贵州大学 | Application of Pu' er ginger flower volatile oil in preparation of antibacterial or anti-inflammatory drugs |
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| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20130102 |