CN103254045A - Preparation method of high-purity Erianin - Google Patents
Preparation method of high-purity Erianin Download PDFInfo
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- CN103254045A CN103254045A CN2013101943624A CN201310194362A CN103254045A CN 103254045 A CN103254045 A CN 103254045A CN 2013101943624 A CN2013101943624 A CN 2013101943624A CN 201310194362 A CN201310194362 A CN 201310194362A CN 103254045 A CN103254045 A CN 103254045A
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- China
- Prior art keywords
- preparation
- solution
- erianin
- hair orchid
- chloroform
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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)
Abstract
The invention discloses a preparation method of high-purity Erianin, which is simple to operate and causes less pollution. The preparation method comprises the following process steps: pulverizing a dendrobe raw material by using a drumstick, adding 5-10 times of 70-100% methanol solution, performing ultrasonic extraction 2-3 times, concentrating the extracting solution, extracting with a chloroform solution, collecting the extract, recovering the reagent, separating the concentrated solution by using a high-speed counter-current chromatograph, performing on-line monitoring by using an ultraviolet detector, collecting the fraction, and performing reduced pressure drying. By using the preparation method to prepare Erianin, the product purity is high, and the large-scale industrialization can be easily realized.
Description
Technical field
The invention belongs to the Natural Medicine Chemistry field, particularly a kind of preparation method of high purity hair orchid element.
Background technology
Hair orchid element (Erianin), Chinese information processing system name: 3-hydroxyl-4,3 ', 4 ', 5 '-tetramethoxy bibenzyl; Molecular formula: C
18H
22O
5Molecular structural formula is as follows:
。
The hair orchid element is the bibenzyl compound, is soluble in organic solvents such as ethanol, chloroform, acetone, methyl alcohol, and is atomic water-soluble.Found through experiments the hair orchid element and can obviously suppress stomach cancer cell SGC-7901 propagation, show as concentration dependent, 48 hours IC
50Be 0.056 μ g/ml, discover that the hair orchid element can suppress the telomerase activation of stomach cancer cell SGC-7901 fast, just visible telomerase activation suppressed in 8 hours, just can suppress 80% of telomerase activation in 48 hours.
Nineteen nineties Chinese scholar separation and Extraction from the stem of noble dendrobium goes out the hair orchid element, its extracting method is to be the extraction solvent and to extract in 30 minutes with supersound process with chloroform or benzene, and extract gets the plain crystalline powder of white atypic hair orchid through the silicagel column column chromatography for separation again.Chinese patent application (03115752.1) discloses the method for extracting the hair orchid element from the stem of noble dendrobium, comprises the application supercritical CO
2Extraction and column chromatography are entrainment agent with dehydrated alcohol, methyl alcohol, acetone etc., with CO
2Equipotential extracts medium and extracts antineoplastic component hair orchid element from the orchid stem of noble dendrobium, to the crude extract of gained again with sherwood oil: vinyl acetic monomer solution is that eluent carries out steps acquisition extracts such as silicagel column column chromatography for separation and recrystallization.The tradition silicagel column prepares high purity hair orchid element, the separating step complexity, and solvent load is big, and sepn process sample yield is low, and is seriously polluted, is not suitable for suitability for industrialized production.
Summary of the invention
The objective of the invention is to solve the deficiencies in the prior art and defective, provide a kind of efficient, the preparation method of easy high purity hair orchid element.
To achieve these goals, the present invention is by the following technical solutions:
A kind of preparation method of high purity hair orchid element, it is characterized in that: get the Dendrobium chrysotoxum raw material pulverizing, add 5 ~ 10 times of amount 70 ~ 100% methanol solution supersound extraction 2-3 time, extracting solution concentrates the back and extracts with chloroformic solution, collect extraction liquid and reclaim reagent, concentrated solution separates with high-speed counter-current chromatograph again, and the UV-detector on-line monitoring is collected the flow point drying under reduced pressure namely.
Described high-speed counter-current chromatograph separation condition is: get chloroform, methyl alcohol, water, mix by 5 ~ 10:2 ~ 4:3 ~ 9, get the phase that fixes mutually, be moving phase mutually down, engine speed 700 ~ 1000rpm, flow velocity are 1 ~ 4ml/min.
Positively effect of the present invention is: adopt high-speed countercurrent chromatography to separate, preparation cycle is short, and simple to operate, preparation amount is big, and sample do not lose, and is environmentally friendly, is fit to suitability for industrialized production.
Further specify the present invention below in conjunction with embodiment, but the scope of protection of present invention is not limited to following embodiment.
Embodiment:
Embodiment 1:
The Dendrobium chrysotoxum raw material pulverizing claims 3kg, uses 15L80% methanol solution supersound extraction 30 minutes at every turn, extracts 3 times, and extracting solution is evaporated to 500ml, adds the equal-volume chloroform extraction 3 times, and combining extraction liquid reclaims chloroform and gets extract.Get chloroform, methyl alcohol, water, press 5:2:3 and mix, fully after the layering, get and fill with the high speed adverse current chromatogram pipe phase that fixes mutually, drive alternation of hosts's machine, rotating speed 800rpm pumps into down and do the stream phasing mutually simultaneously, after setting up running balance, flow rate regulation is 2ml/min, with moving phase dissolution extraction thing, by the sampling valve sample introduction, the UV-detector on-line monitoring is collected target component, preparation continuously, flow point reclaims reagent, gets the plain 4.2g of white powder hair orchid, detect through HPLC, content 98.8%, through UV, IR, MS,
2HNMR,
13The data of its physical behavior of sign such as CNMR are consistent with prior art.
Embodiment 2:
The Dendrobium chrysotoxum raw material pulverizing claims 3kg, uses 30L90% methanol solution supersound extraction 30 minutes at every turn, extracts 2 times, and extracting solution is evaporated to 800ml, adds the equal-volume chloroform extraction 2 times, and combining extraction liquid reclaims chloroform and gets extract.Get chloroform, methyl alcohol, water, press 10:4:7 and mix, fully after the layering, get and fill with the high speed adverse current chromatogram pipe phase that fixes mutually, drive alternation of hosts's machine, rotating speed 900rpm pumps into down and do the stream phasing mutually simultaneously, after setting up running balance, flow rate regulation is 3ml/min, with moving phase dissolution extraction thing, by the sampling valve sample introduction, the UV-detector on-line monitoring is collected target component, preparation continuously, flow point reclaims reagent, gets the plain 4.8g of white powder hair orchid, detect through HPLC, content 98.1%, through UV, IR, MS,
2HNMR,
13The data of its physical behavior of sign such as CNMR are consistent with prior art.
Claims (2)
1. the preparation method of a high purity hair orchid element, it is characterized in that: get the Dendrobium chrysotoxum raw material pulverizing, add 5 ~ 10 times of amount 7 ~ 100% methanol solution supersound extraction 2 ~ 3 times, extracting solution concentrates the back and extracts with chloroformic solution, collect extraction liquid and reclaim reagent, concentrated solution separates with high-speed counter-current chromatograph again, and the UV-detector on-line monitoring is collected the flow point drying under reduced pressure namely.
2. the preparation method of high purity hair orchid element according to claim 1, it is characterized in that described high-speed counter-current chromatograph separation condition is: get chloroform, methyl alcohol, water, mix by 5 ~ 10:2 ~ 4:3 ~ 9, get the phase that fixes mutually, descend to be mutually moving phase, engine speed 700 ~ 1000rpm, flow velocity are 1 ~ 4ml/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013101943624A CN103254045A (en) | 2013-05-23 | 2013-05-23 | Preparation method of high-purity Erianin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013101943624A CN103254045A (en) | 2013-05-23 | 2013-05-23 | Preparation method of high-purity Erianin |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103254045A true CN103254045A (en) | 2013-08-21 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
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| CN2013101943624A Pending CN103254045A (en) | 2013-05-23 | 2013-05-23 | Preparation method of high-purity Erianin |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103980099A (en) * | 2014-05-29 | 2014-08-13 | 云南金九地生物科技有限公司 | Method for extracting erianin from dendrobe |
| CN111929396A (en) * | 2020-07-24 | 2020-11-13 | 杭州师范大学 | On-line enrichment method of dendrobium |
-
2013
- 2013-05-23 CN CN2013101943624A patent/CN103254045A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103980099A (en) * | 2014-05-29 | 2014-08-13 | 云南金九地生物科技有限公司 | Method for extracting erianin from dendrobe |
| CN103980099B (en) * | 2014-05-29 | 2016-01-13 | 云南金九地生物科技有限公司 | A kind of method extracting EN from the stem of noble dendrobium |
| CN111929396A (en) * | 2020-07-24 | 2020-11-13 | 杭州师范大学 | On-line enrichment method of dendrobium |
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| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20130821 |