CN102329311A - Method for purifying cheliensisin A - Google Patents
Method for purifying cheliensisin A Download PDFInfo
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- CN102329311A CN102329311A CN201110210627A CN201110210627A CN102329311A CN 102329311 A CN102329311 A CN 102329311A CN 201110210627 A CN201110210627 A CN 201110210627A CN 201110210627 A CN201110210627 A CN 201110210627A CN 102329311 A CN102329311 A CN 102329311A
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- goniothalamicin
- jinghong
- extraction
- purifying
- pressure
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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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- 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
- Y02P20/582—Recycling of unreacted starting or intermediate materials
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Abstract
The invention provides a method for purifying cheliensisin A. The method is characterized by comprising the following steps: taking leaves of goniothalamus cheliensis as raw materials, grinding the leaves to 60-80 meshes, adding the ground leaves to an extraction kettle, extracting the leaves by adopting supercritical CO2, collecting the extracts, adopting a high-speed counter-current chromatography for separation and drying stream under reduced pressure by taking n-hexane-ethyl acetate-methanol-water as a solvent system, thus obtaining cheliensisin A. The method has the advantages of high efficiency, environment friendliness and the like.
Description
Technical field
The present invention relates to a kind of method of purifying Jinghong goniothalamicin A, particularly relate to a kind of application supercritical CO
2The method of extraction and high speed adverse current chromatogram purifying Jinghong goniothalamicin A.
Background technology
Jinghong goniothalamicin A (Cheliensisin A), chemical name 6 (7,8-epoxy-styryl)-5-acetoxyl group-5,6-dihydro-2-pyrone, molecular weight 274, white crystals, fusing point 152-153 ℃.
Jinghong goniothalamicin A is from annonaceae plant Goniothalamus cheliensis Hu. leaf, to extract to get, and has very strong antitumor action.Document " Jinghong goniothalamicin A is induced the research of human promyelocytic leukemia apoptosis and signal transduction pathway thereof " and patent " Jinghong goniothalamicin A " have all been reported the remarkable antitumor action of Jinghong goniothalamicin A.
The method of existing purifying Jinghong goniothalamicin A is: Goniothalamus cheliensis Hu. leaf or stem stalk, extract decompression recycling ethanol with the ethanol cold soaking; Liquid concentrator adds water to be mixed well, and uses chloroform extraction, reclaims chloroform; Get chloroform extract, this extract carries out column chromatography through silica gel, uses sherwood oil successively; ETHYLE ACETATE-sherwood oil gradient elution gets Jinghong goniothalamicin A (cheliensisin A).Document " new anticancer active constituent in the Goniothalamus cheliensis Hu. " and patent " Jinghong goniothalamicin A " disclosed method all are this kind methods.But this traditional technology, extraction efficiency and yield are all lower, and environmental pollution is serious.
Summary of the invention
The objective of the invention is to overcome the deficiency in the existing purifying process, a kind of method of purifying Jinghong goniothalamicin A is provided, this method can improve product yield, and pollution-free.
To achieve these goals, technical scheme of the present invention is following:
A kind of method of purifying Jinghong goniothalamicin A is characterized in that: with the Goniothalamus cheliensis Hu. leaf is raw material, pulverizes the 60-80 order, adds in the extraction kettle, adopts supercritical CO
2Extract is collected in extraction, is solvent systems with normal hexane-ETHYLE ACETATE-methanol-water, adopts high-speed counter-current chromatograph to separate, and the flow point drying under reduced pressure promptly gets Jinghong goniothalamicin A.
Said supercritical CO
2Extraction conditions is: extraction temperature is 50-55 ℃, and extracting pressure is 20-25MPa, and separating still I temperature is 50-55 ℃, and pressure is 8-10MPa, and separating still II temperature is 45-50 ℃, and pressure is 5-6MPa.
Described normal hexane-ETHYLE ACETATE-methanol-water solvent systems ratio is 3: (3-5): (4-5): 4.
Positively effect of the present invention is:
1) adopts supercritical CO
2Extraction, extraction time is short, and efficient is high, and energy consumption is lower, CO
2Recycling, environmental protection.
2) adopt high speed adverse current chromatogram to separate, the product free of losses is a kind of efficient separation method, and preparation cycle is short, and reagent can reuse, and preparation amount is big, no generation of waste materials.
To combine embodiment to further specify the present invention below, but the scope that the present invention requires to protect is not limited to following embodiment.
Embodiment
Embodiment 1:
The big vast brother that finds a view receives the spiceleaf medicinal material, pulverizes 60 orders, gets the 500g raw material and adds supercritical CO
2In the extraction kettle, the opening device adjusting parameter: extraction temperature is 50 ℃, and extracting pressure is 25MPa, and separating still I temperature is 55 ℃, and pressure is 10MPa, and separating still II temperature is 45 ℃, and pressure is 5MPa.After reaching above-mentioned parameter,, resolve extract with 20L/h flow extraction 4h.Getting normal hexane, ETHYLE ACETATE, methyl alcohol, water, be that in proportion 3:3:5:4 mixes, below is stationary phase mutually, on be moving phase mutually; Open high-speed counter-current chromatograph, get acetic acid ethyl dissolution extract injecting chromatograph, regulate rotating speed 900r/min; Flow velocity 2ml/min, separate the red brother of scape to receive fragrant first plain, collect the red brother of scape and receive the plain flow point of fragrant first; Drying under reduced pressure gets the red brother of scape and receives the plain 650mg of fragrant first, and performance liquid detects, content 98.7%.
Embodiment 2:
The red brother that finds a view receives the spiceleaf medicinal material, pulverizes 60 orders, gets the 500g raw material and adds CO
2In the extraction kettle, the opening device adjusting parameter: extraction temperature is 50 ℃, and extracting pressure is 20MPa, and separating still I temperature is 50 ℃, and pressure is 8MPa, and separating still II temperature is 45 ℃, and pressure is 6MPa.After reaching above-mentioned parameter,, collect extract with 30L/h flow extraction 2h.Getting normal hexane, ETHYLE ACETATE, methyl alcohol, water, be that in proportion 3:5:4:4 mixes, below is stationary phase mutually, on be moving phase mutually; Open high-speed counter-current chromatograph, get acetic acid ethyl dissolution extract injecting chromatograph, regulate rotating speed 850r/min; Flow velocity 2ml/min, separating the red brother of scape, to receive fragrant first plain, collects the red brother of scape and receive the plain flow point of fragrant first; Drying under reduced pressure gets the red brother of scape and receives the plain 671mg of fragrant first, and performance liquid detects, content 98.1%.
Embodiment 3:
The red brother that finds a view receives the spiceleaf medicinal material, pulverizes 80 orders, gets the 1kg raw material and adds CO
2In the extraction kettle, the opening device adjusting parameter: extraction temperature is 55 ℃, and extracting pressure is 22MPa, and separating still I temperature is 50 ℃, and pressure is 8MPa, and separating still II temperature is 45 ℃, and pressure is 6MPa.After reaching above-mentioned parameter,, collect extract with 30L/h flow extraction 2h.Getting normal hexane, ETHYLE ACETATE, methyl alcohol, water, be that in proportion 3:4:5:4 mixes, below is stationary phase mutually, on be moving phase mutually; Open high-speed counter-current chromatograph, acetic acid ethyl dissolution extract injecting chromatograph is regulated rotating speed 850r/min; Flow velocity 2ml/min, separating the red brother of scape, to receive fragrant first plain, collects the red brother of scape and receive the plain flow point of fragrant first; Drying under reduced pressure gets the red brother of scape and receives the plain 1.31g of fragrant first, and performance liquid detects, content 98.5%.
Embodiment 4:
The red brother that finds a view receives the spiceleaf medicinal material, pulverizes 80 orders, gets the 2kg raw material and adds CO
2In the extraction kettle, the opening device adjusting parameter: extraction temperature is 50 ℃, and extracting pressure is 25MPa, and separating still I temperature is 55 ℃, and pressure is 9MPa, and separating still II temperature is 50 ℃, and pressure is 5MPa.After reaching above-mentioned parameter,, collect extract with 30L/h flow extraction 3h.Getting normal hexane, ETHYLE ACETATE, methyl alcohol, water, be that in proportion 3:5:5:4 mixes, below is stationary phase mutually, on be moving phase mutually; Open high-speed counter-current chromatograph, acetic acid ethyl dissolution extract injecting chromatograph is regulated rotating speed 900r/min; Flow velocity 3ml/min, separating the red brother of scape, to receive fragrant first plain, collects the red brother of scape and receive the plain flow point of fragrant first; Drying under reduced pressure gets the red brother of scape and receives the plain 2.7g of fragrant first, and performance liquid detects, content 98.2%.
Claims (3)
1. the method for a purifying Jinghong goniothalamicin A, it is characterized in that: with the Goniothalamus cheliensis Hu. leaf is raw material, pulverizes the 60-80 order, adds in the extraction kettle, adopts supercritical CO
2Extract is collected in extraction, is solvent systems with normal hexane-ETHYLE ACETATE-methanol-water, adopts high-speed counter-current chromatograph to separate, and the flow point drying under reduced pressure promptly gets Jinghong goniothalamicin A.
2. according to the method for the said a kind of purifying Jinghong goniothalamicin A of claim 1, it is characterized in that said supercritical CO
2Extraction conditions is: extraction temperature is 50-55 ℃, and extracting pressure is 20-25MPa, and separating still I temperature is 50-55 ℃, and pressure is 8-10MPa, and separating still II temperature is 45-50 ℃, and pressure is 5-6MPa.
3. according to the method for the said a kind of purifying Jinghong goniothalamicin A of claim 1, it is characterized in that described normal hexane-ETHYLE ACETATE-methanol-water solvent systems ratio is 3: (3-5): (4-5): 4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110210627A CN102329311A (en) | 2011-07-26 | 2011-07-26 | Method for purifying cheliensisin A |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110210627A CN102329311A (en) | 2011-07-26 | 2011-07-26 | Method for purifying cheliensisin A |
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| CN102329311A true CN102329311A (en) | 2012-01-25 |
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| CN201110210627A Pending CN102329311A (en) | 2011-07-26 | 2011-07-26 | Method for purifying cheliensisin A |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05255295A (en) * | 1992-03-10 | 1993-10-05 | Nippon Zeon Co Ltd | Production of gamma-alkylidene-gamma-butylolactone |
| CN1144221A (en) * | 1995-09-01 | 1997-03-05 | 中国科学院昆明植物研究所 | Jinghong goniothalamicin A and its preparation method and use |
| CN101759687A (en) * | 2009-10-20 | 2010-06-30 | 苏州派腾生物医药科技有限公司 | Method for preparing Silymarin |
-
2011
- 2011-07-26 CN CN201110210627A patent/CN102329311A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05255295A (en) * | 1992-03-10 | 1993-10-05 | Nippon Zeon Co Ltd | Production of gamma-alkylidene-gamma-butylolactone |
| CN1144221A (en) * | 1995-09-01 | 1997-03-05 | 中国科学院昆明植物研究所 | Jinghong goniothalamicin A and its preparation method and use |
| CN101759687A (en) * | 2009-10-20 | 2010-06-30 | 苏州派腾生物医药科技有限公司 | Method for preparing Silymarin |
Non-Patent Citations (3)
| Title |
|---|
| T. W. SAM，等: "Goniothalamin oxide: An embryotoxic compound from goniothalamusmacrophyllus (annonaceae)", 《TETRAHEDRON LETTERS》 * |
| 曹学丽: "《高速逆流色谱分离技术及应用》", 31 March 2005, 化学工业出版社 * |
| 缪勇，等: "《中草药植物提取与深加工新技术实用手册》", 31 December 2004, 天津电子出版社 * |
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Application publication date: 20120125 |