CN101851219A - Method for preparing isofraxidin from acanthopanax senticosus rhizomes - Google Patents
Method for preparing isofraxidin from acanthopanax senticosus rhizomes Download PDFInfo
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- CN101851219A CN101851219A CN 201010184243 CN201010184243A CN101851219A CN 101851219 A CN101851219 A CN 101851219A CN 201010184243 CN201010184243 CN 201010184243 CN 201010184243 A CN201010184243 A CN 201010184243A CN 101851219 A CN101851219 A CN 101851219A
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- isofraxidin
- radix
- acanthopanacis senticosi
- caulis acanthopanacis
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Abstract
The invention relates to a method for preparing isofraxidin from acanthopanax senticosus rhizomes, which is characterized by comprising the following steps: extracting crushed acanthopanax senticosus rhizomes and an ethanol solution in a certain feed liquid ratio; filtering an obtained mixture; carrying out decompression concentration on a filtrate to 1/2 volume to obtain a concentrated solution; then adding an acid aqueous solution and a given volume of 1,1-dichloroethane; separating out a 1,1-dichloroethane phase after hydrolysis extraction is carried out under the heating condition; carrying out the decompression concentration until dryness to obtain the product of the isofraxidin. The operation process hs the main characteristics of rich and available raw materials, simple operation and process, strong practicability and easy industrial operation, and high-yield products can be obtained by single extraction.
Description
Affiliated technical field
The present invention relates to the natural product chemistry field, particularly a kind of method that from the Radix Et Caulis Acanthopanacis Senticosi rhizome, prepares isofraxidin.
Background technology
Radix Et Caulis Acanthopanacis Senticosi (Acanthopanax senticosus (Rupr.et Maxim.) Harms.Syn.Eleutherococccus Senticosus (Rupr.et Maxim.) Maxim) mainly is distributed in ground such as the northeast of Russia, Korea, Japan and China and Hebei.Be a kind of scattered or grow thickly in mountain region broad-leaved mixed forest down and the common shrub on border or the cutover, root and rhizome is main medicinal part.Be called in Russia " siberian ginseng (Siberian ginseng), Japan is called " Ezo-ukogi ", and the U.S. is called " Adatogen ".The Radix Et Caulis Acanthopanacis Senticosi complete stool contains multiple secondary metabolite with physiologically active, is the famous plant amedica with long applicating history.Compendium of Material Medica record " Radix Et Caulis Acanthopanacis Senticosi is can benefit power benefit smart, and the therapeutic method to keep the adverse qi flowing downward makes eye bright ", " can mend five kinds of strain and seven kinds of impairment, clothes are made light of one's life by commiting suicide anti-old for a long time "; Has the merit that replenishes qi to invigorate the spleen, tonifies the kidney to relieve mental strain.Modern clinical neurosis, hypoadrenocorticism disease, diabetes, the tumour patient of being used for the treatment of is because of multiple diseases such as radiotherapy, leukopenia caused by cancer chemotherapy, rheumatic and rheumatoid arthritis, chronic bronchitis, pulmonary heart disease, stenocardia, hypertension, hyperlipemia disease, local anemia, cerebral thrombosis, ypotension and diabetes.
In recent years, extensive studies has been carried out in the chemical ingredients and the pharmacological action thereof of Radix Et Caulis Acanthopanacis Senticosi both at home and abroad, proved that they have higher pharmaceutical use.Isofraxidin is one of important secondary metabolite of containing of Radix Et Caulis Acanthopanacis Senticosi, and Chinese scholar Zhao Yuqings in 1991 etc. are isolation identification first.Isofraxidin has tangible tranquilizing effect, and isofraxidin not only makes time for falling asleep obviously shorten, and also significant prolongation of sleep time, effectively improves sleep quality.Isofraxidin has tangible anti-inflammatory action, has weak antitumor action, to S
180Inhibiting rate be 37%～38%, to Lymphocytic leukemia P
388Effectively, its ED
50Be 1.7 μ g/ml, the Korea S scholar treats hepatitis with isofraxidin.In China usually the inspecting standard of isofraxidin as the Radix Et Caulis Acanthopanacis Senticosi preparation.Isofraxidin exists with the form of free type and mating type in the Radix Et Caulis Acanthopanacis Senticosi medicinal material, and mating type is mainly Radix Et Caulis Acanthopanacis Senticosi glucoside B
1Convert it into isofraxidin, significant to improving drug effect.
Generally be to adopt acid hydrolysis-organic solvent extractionprocess conversion and separate isofraxidin at present both at home and abroad, the promptly direct combined isofraxidin that the Radix Et Caulis Acanthopanacis Senticosi extract acid hydrolysis is wherein contained is used organic solvent extraction then.This technological operation is loaded down with trivial details, repeatedly extraction and easily emulsification, and yield is low.So the present invention has considered above situation and has developed hydrolysis and extracted the method for preparing isofraxidin from the Radix Et Caulis Acanthopanacis Senticosi rhizome simultaneously.
Summary of the invention
The purpose of content of the present invention is to provide a kind of method for preparing isofraxidin from the Radix Et Caulis Acanthopanacis Senticosi rhizome, it is characterized in that: Radix Et Caulis Acanthopanacis Senticosi rhizome and the ethanolic soln pulverized are extracted by certain solid-liquid ratio, the gained mixture is filtered, filtrate decompression is concentrated into 1/2nd volumes, get concentrated solution, add aqueous acid and certain volume 1 then, the 1-ethylene dichloride is after hydrolysis extracts under heating condition, tell 1,1-ethylene dichloride phase, be evaporated to dried, the thick product of isofraxidin.
The volume fraction of used ethanolic soln is 30%～80%; The mass ratio of Radix Et Caulis Acanthopanacis Senticosi rhizome and ethanolic soln is 1: 5～1: 10; Extracting temperature is 70～90 ℃, and extraction time is 2～4 hours.
Aqueous acid is aqueous hydrochloric acid or the aqueous sulfuric acid of 0.6mol/l～1.8mol/l, and consumption is 0.3～1.2 times of concentrated solution volume, 1, and 1-ethylene dichloride consumption is 0.3～3 times of concentrated solution volume, 70～90 ℃ of hydrolysis extraction temperature, 3～8 hours time.
Advantage of the present invention is:
Raw material resources is rich and easy to get, and the single extraction can obtain the product of high yield, and technology is simple, and is practical, is easy to the industrialization operation.
Specific embodiments
Below, the present invention will be further detailed with embodiment, but it is not limited to any or the similar example of these embodiment.
Embodiment 1
The Radix Acanthopanacis Senticosi root of 500g drying and crushing is pulverized the back with 50% ethanolic soln 3000ml, in 80 ℃ of refluxing extraction 3 hours, mixture filters, filtrate decompression is concentrated into 1/2nd volumes, adds the aqueous hydrochloric acid of 0.6mol/l, and consumption is 0.5 times of concentrated solution volume, 1,1-ethylene dichloride consumption is 2 times of concentrated solution volume, 85 ℃ of hydrolysis extraction temperature, 5 hours time.Tell 1,1-ethylene dichloride phase, be evaporated to dried, the thick product of isofraxidin, extraction yield be the tradition acid-hydrolyzed 1.25 times.
Embodiment 2
The Radix Acanthopanacis Senticosi root of 500g drying and crushing is pulverized the back with 60% ethanolic soln 3500ml, in 80 ℃ of refluxing extraction 3 hours, mixture filters, filtrate decompression is concentrated into 1/2nd volumes, adds the aqueous hydrochloric acid of 0.6mol/l, and consumption is 0.8 times of concentrated solution volume, 1,1-ethylene dichloride consumption is 1.5 times of concentrated solution volume, 85 ℃ of hydrolysis extraction temperature, 4 hours time.Tell 1,1-ethylene dichloride phase, be evaporated to dried, the thick product of isofraxidin, extraction yield be the tradition acid-hydrolyzed 1.23 times.
Claims (7)
1. method that from the Radix Et Caulis Acanthopanacis Senticosi rhizome, prepares isofraxidin, it is characterized in that: Radix Et Caulis Acanthopanacis Senticosi rhizome and the ethanolic soln pulverized are extracted by certain solid-liquid ratio, the gained mixture is filtered, filtrate decompression is concentrated into 1/2nd volumes, get concentrated solution, add aqueous acid and certain volume 1 then, the 1-ethylene dichloride is after hydrolysis extracts under heating condition, tell 1,1-ethylene dichloride phase, be evaporated to dried, the thick product of isofraxidin.
2. according to the described a kind of method for preparing isofraxidin from the Radix Et Caulis Acanthopanacis Senticosi rhizome of claim 1, it is characterized in that: the volume fraction of ethanolic soln is 30%～80%.
3. according to the described a kind of method for preparing isofraxidin from the Radix Et Caulis Acanthopanacis Senticosi rhizome of claim 1, it is characterized in that: the mass ratio of Radix Et Caulis Acanthopanacis Senticosi rhizome and ethanolic soln is 1: 5～1: 10.
4. according to the described a kind of method for preparing isofraxidin from the Radix Et Caulis Acanthopanacis Senticosi rhizome of claim 1, it is characterized in that: extracting temperature is 70～90 ℃, and extraction time is 2～4 hours.
5. according to the described a kind of method for preparing isofraxidin from the Radix Et Caulis Acanthopanacis Senticosi rhizome of claim 1, it is characterized in that: aqueous acid is aqueous hydrochloric acid or the aqueous sulfuric acid of 0.6mol/l～1.8mol/l, and consumption is 0.3～1.2 times of concentrated solution volume.
6. according to the described a kind of method that from the Radix Et Caulis Acanthopanacis Senticosi rhizome, prepares isofraxidin of claim 1, it is characterized in that: 1,1-ethylene dichloride consumption is 0.8～3 times of concentrated solution volume.
7. according to the described a kind of method that from the Radix Et Caulis Acanthopanacis Senticosi rhizome, prepares isofraxidin of claim 1, it is characterized in that: 70～90 ℃ of hydrolysis extraction temperature, 3～8 hours time.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201010184243 CN101851219A (en) | 2010-05-27 | 2010-05-27 | Method for preparing isofraxidin from acanthopanax senticosus rhizomes |
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| CN 201010184243 CN101851219A (en) | 2010-05-27 | 2010-05-27 | Method for preparing isofraxidin from acanthopanax senticosus rhizomes |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102676404A (en) * | 2012-05-29 | 2012-09-19 | 黑龙江大学 | Endophytic fungi capable of improving content of isofraxidin in Radix Acanthopanacis Semticosi through fermenting Radix Acanthopanacis Semticosi |
| CN108484557A (en) * | 2018-06-15 | 2018-09-04 | 东北林业大学 | A method of extracting isofraxidin from wilsonii |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1450061A (en) * | 2002-04-10 | 2003-10-22 | 东北林业大学 | Process for extracting Isofraxidin |
-
2010
- 2010-05-27 CN CN 201010184243 patent/CN101851219A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1450061A (en) * | 2002-04-10 | 2003-10-22 | 东北林业大学 | Process for extracting Isofraxidin |
Non-Patent Citations (2)
| Title |
|---|
| 《南京中医药大学学报》 20060731 马新飞等 刺五加药材中异秦皮啶提取方法的研究 246-247 1-7 第22卷, 第4期 2 * |
| 《黑龙江医药》 20011231 孙华芳等 刺五加中异秦皮定甙水解的最优条件研究 445-447 1-7 第14卷, 第6期 2 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102676404A (en) * | 2012-05-29 | 2012-09-19 | 黑龙江大学 | Endophytic fungi capable of improving content of isofraxidin in Radix Acanthopanacis Semticosi through fermenting Radix Acanthopanacis Semticosi |
| CN108484557A (en) * | 2018-06-15 | 2018-09-04 | 东北林业大学 | A method of extracting isofraxidin from wilsonii |
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Application publication date: 20101006 |