CN102659804A - Preparation method of dehydrodeguelin - Google Patents
Preparation method of dehydrodeguelin Download PDFInfo
- Publication number
- CN102659804A CN102659804A CN2012101208686A CN201210120868A CN102659804A CN 102659804 A CN102659804 A CN 102659804A CN 2012101208686 A CN2012101208686 A CN 2012101208686A CN 201210120868 A CN201210120868 A CN 201210120868A CN 102659804 A CN102659804 A CN 102659804A
- Authority
- CN
- China
- Prior art keywords
- dehydrodeguelin
- extraction
- preparation
- polyamide resin
- liquid concentrator
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to the technical field of extraction of active ingredients of plants and relates to a preparation method of dehydrodeguelin. The method comprises enabling Tephrosia vogelii Hook. to serve as a raw material, and enabling the technologies including continuous countercurrent ultrasonic extraction, adsorption separation through polyamide resin and high-speed counter-current chromatography purification and the like to be organically combined. The method ensures coordination in the process of extraction, purification and the like of the dehydrodeguelin, and meets the requirements for preparing the high-purity dehydrodeguelin. The method is low in cost, the preparation quantity is large, the extraction rate is high, and continuous production can be carried out.
Description
Technical field
The invention belongs to the Natural Medicine Chemistry field, relate to a kind of preparation method of dehydrodeguelin.
Background technology
Dehydrodeguelin (Dehydrodeguelin), molecular formula are C
23H
20O
6, molecular weight is 392.41, is from leguminous plants square leaf trifoliate jewelvine
Derris oblongaBenth. root, wood are blue
Indigofera tinctoriaL. complete stool, Herba Tephrosiae purpureae
Tephrosia purpureaPers. herb and Ao Shi Herba Tephrosiae purpureae
Tephrosia vogeliiHook. separate a kind of xanthone compounds that obtains in.Pharmacological research shows that dehydrodeguelin has nematocidal effect, can suppress the activity of rat heart cAMP phosphodiesterase, in addition, also has effects such as anti-young mosquito, anti-beans beetle.
At present, less to the research of dehydrodeguelin both at home and abroad, do not retrieve the method report for preparing dehydrodeguelin as yet.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of dehydrodeguelin; This method organically combines through technology such as continuous countercurrent ultrasonic extraction, polyamide resin absorption and high speed adverse current chromatogram separation and purification; Solve the Harmony of the operations such as extraction, purifying of dehydrodeguelin, reached the requirement of preparation high purity dehydrodeguelin.The inventive method cost is low, preparation amount is big, but and the high continuous production of extraction yield.
The objective of the invention is to realize through following technical scheme:
A kind of preparation method of dehydrodeguelin is characterized in that may further comprise the steps:
(1) extract: with the pulverizing of Ao Shi Herba Tephrosiae purpureae herb, add 70-85% ethanol, adopt the continuous countercurrent supersound extraction, under the UW effect of Vltrasonic device, extraction time is 40-120min, extracts 2-4 time, extracts 40-55 ℃ of temperature, filters, and gets extracting solution;
(2) extraction: said extracted liquid concentrating under reduced pressure is got liquid concentrator, with water-saturated n-butanol liquid concentrator is extracted, reclaim under reduced pressure reagent must extract liquid concentrator;
(3) polyamide resin column absorption: will extract liquid concentrator and mix appearance, volatilize reagent with a small amount of polyamide resin, last polyamide resin column, extremely colourless with 10% ethanol elution earlier, again with the 70-85% ethanol elution, the TLC tracking monitor is collected the dehydrodeguelin elutriant;
(4) high speed adverse current chromatogram purifying: elutriant is concentrated after the high speed adverse current chromatogram separation and purification, and chloroform-methanol-water is solvent systems, and UV-detector detects, and collects flow point, reclaims reagent, is drying to obtain.
Ultrasonic frequency is 20-50KHz in the said step (1).
In the said step (4), the high-speed countercurrent chromatography solvent systems is chloroform-methanol-water, and volume ratio is (4-10): (5-13): (2-5), below be stationary phase mutually, on be moving phase mutually.
Advantage of the present invention is: the present invention adopts the continuous countercurrent supersound extraction, has realized that not only serialization operation, dynamic countercurrent extract, and has cooperated Vltrasonic device, has shortened extraction time, has improved extraction ratio of effective constituents; Earlier effective constituent is carried out enrichment, reduced the treatment capacity of subsequent handling with polyamide resin.
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:
Get Ao Shi Herba Tephrosiae purpureae herb, pulverize, the 1kg powder is added 70% ethanol, adopt the continuous countercurrent supersound extraction, temperature is 40 ℃; Extraction time is 50min, and ultrasonic frequency is 40KHz, extracts 3 times, filters; United extraction liquid, concentrating under reduced pressure, the gained liquid concentrator is used the water saturation n-butanol extraction, extraction liquid reclaim under reduced pressure reagent; To extract liquid concentrator and mix appearance with a small amount of polyamide resin, and add polyamide resin column after volatilizing reagent, first water flushing is washed till colourless with 10% ethanol again; Use 75% ethanol elution then, the TLC tracking monitor is collected the dehydrodeguelin elutriant, injects high-speed counter-current chromatograph behind the concentrating under reduced pressure; With chloroform-methanol-water (4:5:2) is solvent systems, and UV-detector detects, and is stationary phase mutually down, on be moving phase mutually; Flow rate of mobile phase is 2ml/min, collects the dehydrodeguelin flow point according to the detector spectrogram, concentrated, the dry dehydrodeguelin that gets, and the HPLC detection level is 97%.
Embodiment 2:
Get Ao Shi Herba Tephrosiae purpureae herb, pulverize, the 1kg powder is added 75% ethanol, adopt the continuous countercurrent supersound extraction, temperature is 55 ℃; Extraction time is 40min, and ultrasonic frequency is 30KHz, extracts 4 times, filters; United extraction liquid, concentrating under reduced pressure, the gained liquid concentrator is used the water saturation n-butanol extraction, extraction liquid reclaim under reduced pressure reagent; To extract liquid concentrator and mix appearance with a small amount of polyamide resin, and add polyamide resin column after volatilizing reagent, first water flushing is washed till colourless with 10% ethanol again; Use 80% ethanol elution then, the TLC tracking monitor is collected the dehydrodeguelin elutriant, injects high-speed counter-current chromatograph behind the concentrating under reduced pressure; With chloroform-methanol-water (9:13:4) is solvent systems, and UV-detector detects, and is stationary phase mutually down, on be moving phase mutually; Flow rate of mobile phase is 2ml/min, collects the dehydrodeguelin flow point according to the detector spectrogram, concentrated, the dry dehydrodeguelin that gets, and the HPLC detection level is 98%.
Embodiment 3:
Get Ao Shi Herba Tephrosiae purpureae herb, pulverize, the 1kg powder is added 80% ethanol, adopt the continuous countercurrent supersound extraction, temperature is 50 ℃; Extraction time is 90min, and ultrasonic frequency is 50KHz, extracts 2 times, filters; United extraction liquid, concentrating under reduced pressure, the gained liquid concentrator is used the water saturation n-butanol extraction, extraction liquid reclaim under reduced pressure reagent; To extract liquid concentrator and mix appearance with a small amount of polyamide resin, and add polyamide resin column after volatilizing reagent, first water flushing is washed till colourless with 10% ethanol again; Use 85% ethanol elution then, the TLC tracking monitor is collected the dehydrodeguelin elutriant, injects high-speed counter-current chromatograph behind the concentrating under reduced pressure; With chloroform-methanol-water (8:9:5) is solvent systems, and UV-detector detects, and is stationary phase mutually down, on be moving phase mutually; Flow rate of mobile phase is 2ml/min, collects the dehydrodeguelin flow point according to the detector spectrogram, concentrated, the dry dehydrodeguelin that gets, and the HPLC detection level is 95%.
Embodiment 4:
Get Ao Shi Herba Tephrosiae purpureae herb, pulverize, the 1kg powder is added 85% ethanol, adopt the continuous countercurrent supersound extraction, temperature is 45 ℃; Extraction time is 120min, and ultrasonic frequency is 20KHz, extracts 2 times, filters; United extraction liquid, concentrating under reduced pressure, the gained liquid concentrator is used the water saturation n-butanol extraction, extraction liquid reclaim under reduced pressure reagent; To extract liquid concentrator and mix appearance with a small amount of polyamide resin, and add polyamide resin column after volatilizing reagent, first water flushing is washed till colourless with 10% ethanol again; Use 80% ethanol elution then, the TLC tracking monitor is collected the dehydrodeguelin elutriant, injects high-speed counter-current chromatograph behind the concentrating under reduced pressure; With chloroform-methanol-water (10:7:3) is solvent systems, and UV-detector detects, and is stationary phase mutually down, on be moving phase mutually; Flow rate of mobile phase is 2ml/min, collects the dehydrodeguelin flow point according to the detector spectrogram, concentrated, the dry dehydrodeguelin that gets, and the HPLC detection level is 96%.
Claims (3)
1. the preparation method of a dehydrodeguelin is characterized in that may further comprise the steps:
(1) extract: with the pulverizing of Ao Shi Herba Tephrosiae purpureae herb, add 70-85% ethanol, adopt the continuous countercurrent supersound extraction, under the UW effect of Vltrasonic device, extraction time is 40-120min, extracts 2-4 time, extracts 40-55 ℃ of temperature, filters, and gets extracting solution;
(2) extraction: said extracted liquid concentrating under reduced pressure is got liquid concentrator, with water-saturated n-butanol liquid concentrator is extracted, reclaim under reduced pressure reagent must extract liquid concentrator;
(3) polyamide resin column absorption: will extract liquid concentrator and mix appearance, volatilize reagent with a small amount of polyamide resin, last polyamide resin column, extremely colourless with 10% ethanol elution earlier, again with the 70-85% ethanol elution, the TLC tracking monitor is collected the dehydrodeguelin elutriant;
(4) high speed adverse current chromatogram purifying: elutriant is concentrated after the high speed adverse current chromatogram separation and purification, and chloroform-methanol-water is solvent systems, and UV-detector detects, and collects flow point, reclaims reagent, is drying to obtain.
2. the preparation method of a kind of dehydrodeguelin as claimed in claim 1 is characterized in that ultrasonic frequency is 20-50KHz in the said step (1).
3. the preparation method of a kind of dehydrodeguelin as claimed in claim 1; It is characterized in that in the said step (4), the high-speed countercurrent chromatography solvent systems is chloroform-methanol-water, volume ratio is (4-10): (5-13): (2-5); Below be stationary phase mutually, on be moving phase mutually.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101208686A CN102659804A (en) | 2012-04-24 | 2012-04-24 | Preparation method of dehydrodeguelin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101208686A CN102659804A (en) | 2012-04-24 | 2012-04-24 | Preparation method of dehydrodeguelin |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102659804A true CN102659804A (en) | 2012-09-12 |
Family
ID=46769412
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012101208686A Pending CN102659804A (en) | 2012-04-24 | 2012-04-24 | Preparation method of dehydrodeguelin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102659804A (en) |
-
2012
- 2012-04-24 CN CN2012101208686A patent/CN102659804A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102451235B (en) | Preparation method of olive leaf extract | |
| CN101260131A (en) | Method for extracting iridoid active site and monomer from eucommia bark | |
| CN102924416B (en) | Method for separating and purifying monomeric compounds from ash bark | |
| CN103694364A (en) | Method for synchronously extracting, separating and purifying polysaccharides and flavones of cyclocarya paliurus | |
| CN103623034B (en) | The preparation method of Daxing'an Mountainrange wild euphorbia helioscopia general flavone | |
| CN101838299B (en) | Method for separating and purifying natural acteoside | |
| CN109879919B (en) | Method for separating and preparing three flavonoid glycosides from spina date seeds | |
| CN104418743A (en) | Method for refining chlorogenic acid from honeysuckle crude extract | |
| CN102250164A (en) | Purification method of gastrodin | |
| CN103665065B (en) | A kind of method of preparing fast ponticin and rhapontigenin | |
| CN107722080A (en) | A kind of method that ursin is extracted in the leaf from purple bergenia herb | |
| CN104788527B (en) | Method for extracting tripterine efficiently with ionic liquid | |
| CN105175426B (en) | A kind of method of the extraction purification Bergenin from treebine stem | |
| CN106916162B (en) | A kind of preparation method of jolkinolide B bulk pharmaceutical chemicals | |
| CN104231011B (en) | Preparation method of verbascoside | |
| CN103524578B (en) | A kind of method of extraction and isolation paeoniflorin compound from tree peony stamen | |
| CN107245046B (en) | A method of extracting separating pepper total alkaloids and capsicum red pigment from capsicum | |
| CN105646638B (en) | The preparation method of pedunculoside | |
| CN102659804A (en) | Preparation method of dehydrodeguelin | |
| CN102432521A (en) | Method for extracting abrine from Abrus cantoniensis | |
| CN105859700B (en) | A method of extraction prepares Saponaretin from Patrinia villosa Juss | |
| CN108727441A (en) | A kind of extracting method of rhodioside | |
| CN103739649A (en) | Preparation method for mussaendoside G | |
| CN102911239A (en) | Preparation method of picfeltrarraenin IA | |
| CN102911146A (en) | Method for extracting tricin from alfalfa |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20120912 |