CN106749247A - Method for extracting and purifying sophoramine from subprostrate sophora - Google Patents
Method for extracting and purifying sophoramine from subprostrate sophora Download PDFInfo
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- CN106749247A CN106749247A CN201611268254.7A CN201611268254A CN106749247A CN 106749247 A CN106749247 A CN 106749247A CN 201611268254 A CN201611268254 A CN 201611268254A CN 106749247 A CN106749247 A CN 106749247A
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- subprostrate sophora
- sophoramine
- extraction
- extraction purification
- dichloromethane
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D471/00—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, at least one ring being a six-membered ring with one nitrogen atom, not provided for by groups C07D451/00 - C07D463/00
- C07D471/22—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, at least one ring being a six-membered ring with one nitrogen atom, not provided for by groups C07D451/00 - C07D463/00 in which the condensed systems contains four or more hetero rings
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- Medicines Containing Plant Substances (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses a method for extracting and purifying sophoramine from subprostrate sophora, which comprises the following steps: extraction: pulverizing radix Sophorae Tonkinensis, ultrasonically extracting with organic solvent water solution, extracting the extractive solution with diethyl ether, adjusting pH to alkaline, extracting with dichloromethane, and concentrating to obtain radix Sophorae Tonkinensis alkaloid extract; separation: dissolving the alkaloid extract in acid water, extracting with dichloromethane, and recrystallizing. The method has simple process, simple operation, low cost, and high purity of the obtained sophoramine, and is suitable for industrial production.
Description
Technical field
The present invention relates to Chemistry for Chinese Traditional Medicine field, and in particular to a kind of method of the extraction purification sophoramine from subprostrate sophora.
Background technology
Subprostrate sophora, alias root of subprostrate sophora is the dry root of legume sophora tonkinensis Gapnep Sophora tonkinensis Gagnep.
And rhizome, it is China's traditional Chinese medicine.The effect of with clearing heat and detoxicating, reducing pharyngeal swelling, pented up for treating fiery poison, abscess of throat,
Gingivitis, the disease such as jaundice with damp-heat pathogen and arrhythmia cordis, hepatitis, liver cancer.Contain abundant alkaloid, flavones, three in subprostrate sophora
The various active composition such as terpene.
Sophoramine is a kind of alkaloid component in subprostrate sophora, and its molecular formula is C15H20N2O, molecular weight is 244.3321.It is existing
Show for pharmacological research, sophoramine step-down, anti-arrhythmia, improve vessel retraction and immunosupress, reduce miocardial infarction
Etc. aspect suffer from more obvious action.
Yet there are no the relevant report of the extraction purification sophoramine from subprostrate sophora.
The disclosure of background above technology contents is only used for auxiliary and understands inventive concept of the invention and technical scheme, and it is not
Necessarily belong in the prior art of present patent application, the applying date of the above in present patent application is being shown without tangible proof
In the case of disclosed, above-mentioned background technology should not be taken to evaluate the novelty and creativeness of the application.
The content of the invention
It is high it is an object of the invention to provide a kind of purity, it is adaptable to the extraction purification Chinese scholartree from subprostrate sophora of industrialized production
The method of amine.
The technical solution adopted in the present invention is as follows：
A kind of method of the extraction purification sophoramine from subprostrate sophora, comprises the following steps：
(1) in subprostrate sophora alkaloid extraction：Subprostrate sophora medicinal material, plus aqueous solutions of organic solvent ultrasonic extraction are weighed, are filtered,
Merging filtrate, is concentrated under reduced pressure and reclaims organic solvent, and after the aqueous solution extracts 3 times with ether, aqueous alkali lye adjusts PH to alkalescence, with two
Chloromethanes is extracted 3-5 times, combined dichloromethane extract, is reclaimed dichloromethane and is concentrated to dryness, and obtains subprostrate sophora biology alkali carries
Take thing；
(2) separate：The extract obtained by (1) is taken, acid liquid makes dissolving, add methylene chloride extraction 5 times, combined dichloromethane
Extract, reclaims dichloromethane and is concentrated under reduced pressure into dry, obtains solid；
(3) recrystallize：Take the solid solvent that (2) obtain to recrystallize repeatedly, obtain final product.
Subprostrate sophora pulverizing medicinal materials described in the method for the above extraction purification sophoramine from subprostrate sophora, wherein step (1)
Cross 40-60 mesh sieves；The aqueous solutions of organic solvent is 30-50% ethanol solutions, and consumption is measured for 10-20 times；The ultrasonic extraction
Number of times is 2-3 times, 1-1.5h/ times；The alkali lye is 3-5mol/LNaOH solution；The regulation pH value is 10-12.
Acid solution described in the method for the above extraction purification sophoramine from subprostrate sophora, wherein step (2) be 5% hydrochloric acid or
5% sulfuric acid solution.
Solvent described in the method for the above extraction purification sophoramine from subprostrate sophora, wherein step (3) is ethanol or second
Ether；Solid is 1g with the amount ratio of solvent:(1-10)ml.
Beneficial effects of the present invention：
1st, the method process is simple of extraction purification sophoramine, easy to operate, with low cost from subprostrate sophora that the present invention is provided,
It is adapted to industrialized production.
2nd, the sophoramine purity obtained by the inventive method extraction purification is high, more than 98.0%.
Specific embodiment
With reference to specific embodiment, the invention will be further described, but do not limit the scope of the invention and apply
Scope：
Embodiment 1
Subprostrate sophora medicinal material 50g is weighed, 40 mesh sieves were crushed, plus 10 times of 30% ethanol solutions of amount, ultrasonic extraction 2 times, every time
1.5h, filtration, merging filtrate is concentrated under reduced pressure and reclaims organic solvent, after the aqueous solution extracts 3 times with ether, aqueous 5mol/
LNaOH solution adjusts pH value to 10, is extracted 3 times with dichloromethane, combined dichloromethane extract, reclaims dichloromethane and is concentrated into
It is dry, obtain subprostrate sophora alkaloid extract；The extract of gained is taken, plus 5% hydrochloric acid solution makes dissolving, add methylene chloride extraction 5
Secondary, combined dichloromethane extract reclaims dichloromethane and is concentrated under reduced pressure into dry, obtains solid, is dissolved with ethanol, solid and ethanol
Amount ratio be 1g:1ml, recrystallizes to sophoramine crystallization completely repeatedly, obtains sophoramine 0.41g, and content is 99.81%.
Embodiment 2
Subprostrate sophora medicinal material 100g is weighed, 60 mesh sieves were crushed, plus 15 times of 40% ethanol solutions of amount, ultrasonic extraction 3 times, every time
1h, filtration, merging filtrate is concentrated under reduced pressure and reclaims organic solvent, after the aqueous solution extracts 3 times with ether, aqueous 5mol/LNaOH
Solution adjusts pH value to 11, is extracted 4 times with dichloromethane, combined dichloromethane extract, reclaims dichloromethane and is concentrated to dryness, and obtains
To subprostrate sophora alkaloid extract；The extract of gained is taken, plus 5% hydrochloric acid solution makes dissolving, add methylene chloride extraction 5 times, closes
And dichloromethane extract, reclaim dichloromethane and be concentrated under reduced pressure into dry, solid is obtained, dissolved with ethanol, the use of solid and ethanol
Amount is than being 1g:5ml, recrystallizes to sophoramine crystallization completely repeatedly, obtains sophoramine 0.81g, and content is 99.83%.
Embodiment 3
Subprostrate sophora medicinal material 200g is weighed, 60 mesh sieves were crushed, plus 20 times of 50% ethanol solutions of amount, ultrasonic extraction 3 times, every time
1.5h, filtration, merging filtrate is concentrated under reduced pressure and reclaims organic solvent, after the aqueous solution extracts 3 times with ether, aqueous 5mol/
LNaOH solution adjusts pH value to 12, is extracted 5 times with dichloromethane, combined dichloromethane extract, reclaims dichloromethane and is concentrated into
It is dry, obtain subprostrate sophora alkaloid extract；The extract of gained is taken, plus 5% sulfuric acid solution makes dissolving, add methylene chloride extraction 5
Secondary, combined dichloromethane extract reclaims dichloromethane and is concentrated under reduced pressure into dry, obtains solid, with ether dissolution, solid and ether
Amount ratio be 1g:10ml, recrystallizes to sophoramine crystallization completely repeatedly, obtains sophoramine 0.1.59g, and content is 99.84%.
Above content is to combine specific/preferred embodiment further description made for the present invention, it is impossible to
Assert that specific implementation of the invention is confined to these explanations.Come for general technical staff of the technical field of the invention
Say, without departing from the inventive concept of the premise, its embodiment that can also have been described to these makes some replacements or modification,
And these are substituted or variant should all be considered as belonging to protection scope of the present invention.
Claims (10)
1. a kind of method of the extraction purification sophoramine from subprostrate sophora, it is characterised in that comprise the following steps：
(1) in subprostrate sophora alkaloid extraction：Subprostrate sophora medicinal material, plus aqueous solutions of organic solvent ultrasonic extraction are weighed, is filtered, merged
Filtrate, is concentrated under reduced pressure and reclaims organic solvent, and after the aqueous solution extracts 3 times with ether, aqueous alkali lye adjusts PH to alkalescence, uses dichloromethane
Alkane is extracted 3-5 times, combined dichloromethane extract, is reclaimed dichloromethane and is concentrated to dryness, and obtains subprostrate sophora alkaloid extract；
(2) separate：The extract obtained by (1) is taken, acid liquid makes dissolving, add methylene chloride extraction 5 times, combined dichloromethane extraction
Liquid, reclaims dichloromethane and is concentrated under reduced pressure into dry, obtains solid；
(3) recrystallize：Take the solid solvent that (2) obtain to recrystallize repeatedly, obtain final product.
2. a kind of method of the extraction purification sophoramine from subprostrate sophora according to claim 1, it is characterised in that in step (1)
The subprostrate sophora pulverizing medicinal materials cross 40-60 mesh sieves.
3. a kind of method of the extraction purification sophoramine from subprostrate sophora according to claim 1, it is characterised in that in step (1)
The aqueous solutions of organic solvent is 30%-50% ethanol solutions.
4. a kind of method of the extraction purification sophoramine from subprostrate sophora according to claim 1, it is characterised in that in step (1)
The consumption of the aqueous solutions of organic solvent is measured for 10-20 times.
5. a kind of method of the extraction purification sophoramine from subprostrate sophora according to claim 1, it is characterised in that in step (1)
The ultrasonic extraction number of times is 2-3 times.
6. a kind of method of the extraction purification sophoramine from subprostrate sophora according to claim 1, it is characterised in that in step (1)
The ultrasonic extraction time is 1-1.5h/ times.
7. a kind of method of the extraction purification sophoramine from subprostrate sophora according to claim 1, it is characterised in that in step (1)
The alkali lye is 3-5mol/LNaOH solution.
8. a kind of method of the extraction purification sophoramine from subprostrate sophora according to claim 1, it is characterised in that in step (1)
The regulation pH value is 10-12.
9. a kind of method of the extraction purification sophoramine from subprostrate sophora according to claim 1, it is characterised in that in step (2)
The acid solution is 5% hydrochloric acid or 5% sulfuric acid solution.
10. a kind of method of the extraction purification sophoramine from subprostrate sophora according to claim 1, it is characterised in that in step (3)
The solvent is ethanol or ether；Solid is 1g with the amount ratio of solvent：(1-10)ml.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611268254.7A CN106749247A (en) | 2016-12-31 | 2016-12-31 | Method for extracting and purifying sophoramine from subprostrate sophora |
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| CN201611268254.7A CN106749247A (en) | 2016-12-31 | 2016-12-31 | Method for extracting and purifying sophoramine from subprostrate sophora |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101084989A (en) * | 2007-07-11 | 2007-12-12 | 石任兵 | Method for preparing general flavone and total alkaloid of sophora flavescens simultaneously |
| CN101921272A (en) * | 2009-07-02 | 2010-12-22 | 陕西嘉禾植物化工有限责任公司 | Method for extracting and separating laburnine |
| CN103059021A (en) * | 2013-01-24 | 2013-04-24 | 宁夏紫荆花制药有限公司 | Preparation process of high-purity sophoramine |
-
2016
- 2016-12-31 CN CN201611268254.7A patent/CN106749247A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101084989A (en) * | 2007-07-11 | 2007-12-12 | 石任兵 | Method for preparing general flavone and total alkaloid of sophora flavescens simultaneously |
| CN101921272A (en) * | 2009-07-02 | 2010-12-22 | 陕西嘉禾植物化工有限责任公司 | Method for extracting and separating laburnine |
| CN103059021A (en) * | 2013-01-24 | 2013-04-24 | 宁夏紫荆花制药有限公司 | Preparation process of high-purity sophoramine |
Non-Patent Citations (3)
| Title |
|---|
| 张士舜 主编: "《肠癌中医研究》", 31 May 2015 * |
| 王秀坤 等: "白刺花种子生物碱成分的研究", 《中国中药杂志》 * |
| 窦金辉: "山豆根生物碱成分的研究", 《中国中药杂志》 * |
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