CN107496508A - A kind of preparation method of Fourstamen Stephania Root alkaloid - Google Patents
A kind of preparation method of Fourstamen Stephania Root alkaloid Download PDFInfo
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- CN107496508A CN107496508A CN201710713252.2A CN201710713252A CN107496508A CN 107496508 A CN107496508 A CN 107496508A CN 201710713252 A CN201710713252 A CN 201710713252A CN 107496508 A CN107496508 A CN 107496508A
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- alkaloid
- stephania root
- fourstamen stephania
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/59—Menispermaceae (Moonseed family), e.g. hyperbaena or coralbead
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07G—COMPOUNDS OF UNKNOWN CONSTITUTION
- C07G5/00—Alkaloids
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/35—Extraction with lipophilic solvents, e.g. Hexane or petrol ether
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
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Abstract
The invention discloses a kind of preparation method of Fourstamen Stephania Root alkaloid, former material is handled by way of acid solution diacolation, can remove in advance more non-needs alkaloid substance, such as Cyclanoline, the process for simplifying later separation, and the method separated by low pressure column chromatography efficiently, rapidly by Tetrandrine and B prime can be kept completely separate separation, mutually undope, purity is very high, quality better.
Description
Technical field
The present invention relates to biological technical field, specifically a kind of preparation method of Fourstamen Stephania Root alkaloid.
Background technology
Fourstamen Stephania Root is the root tuber of Menispermaceae stephania plant Fourstamen Stephania Root, is that China is often removed with one of Chinese herbal medicine, tool wind-dispelling
The effect of wet, inducing diuresis to remove edema, promoting qi circulation and relieving pain.The main active of Fourstamen Stephania Root is alkaloid, such as Tet, root of fangji promise woods
Alkali etc..Fourstamen Stephania Root alkaloid, there is anti-hypertension, resist myocardial ischemia and reperfusion injury, anti-arrhythmia, anti-inflammatory and immune suppression
System, antitumor extensive physiological activity.
Although there is research report and patent document in terms of Fourstamen Stephania Root alkaloid extraction in recent years, chromatogram is mostly based on
Method separation, the purification of post, use substantial amounts of auxiliary agent, such as high concentration ethanol therebetween, and process is complex, purifies work
There is many disturbing factors in sequence, constrain the preparation purity of Fourstamen Stephania Root alkaloid.
The content of the invention
It is an object of the invention to provide a kind of preparation method of Fourstamen Stephania Root alkaloid, to solve to carry in above-mentioned background technology
The problem of going out.
To achieve the above object, the present invention provides following technical scheme：
A kind of preparation method of Fourstamen Stephania Root alkaloid, is realized by following steps：
S1, the Fourstamen Stephania Root medicinal material of 100 parts by weight is taken, is ground by grinder, obtains coarse powder；
S2,0.5%H2SO4 solution is added into coarse powder, is sufficiently stirred, obtains sour water percolate；
S3, fresh milk of lime is slowly added into sour water percolate, regulation pH value to 9-10, is filtered after standing 15 minutes, is removed
Alkaline solution obtains mud yellow mercury oxide；
S4, net sand is added into mud yellow mercury oxide, and stirred to being sufficiently mixed, be placed into 80 DEG C of drying bakers and dry, then divided
Criticize to be introduced into apparatus,Soxhlet's repeatedly to be extracted to biological alkali carries with ether and use up, reclaim ether, obtain ether extract；
S5, with 95%, 40-60ml ethanol solutions backflow thermosol, pour into 500ml water, the NaCl solution for adding 30 parts by weight is entered
Row is saltoutd, and is subsequently heated to condensation, is stood until precipitating completely, is filtered, obtained containing Tetrandrine and Fourstamen Stephania Root second
The white precipitate of element；
S6, low pressure column chromatography separation, specific method are：
S61, using decompression dry method dress method dress post, fill silica gel at least 30 parts by weight；
S62, add a small amount of acetone thermosol, be added on 1.5g silica gel with dropper, carefully mixed thoroughly, is evaporated in water-bath, it is fine ground, it is rear to add in vain
Color precipitates, and keeps its surfacing；
S63, elution, dropper carefully adds a small amount of eluant, eluent along chromatographic column post jamb, when liquid level reach a certain height, adds again
Enter remaining eluant, eluent, about 250ml, pressure needed for transfer, 0.6-1.2kg/cm2, flows out, coutroi velocity 1ml/ after about 40 minutes altogether
Point, manage within every 10 minutes or so one, receive 12-15 parts, elution overall process about 3 hours；
S64, each fraction move into small glass evaporators respectively, in being concentrated in water-bath, using Tetrandrine, B prime as standard items pair
According to merging same composition, acquisition first, B prime crude product, with acetone recrystallization, obtains alkaloid sterling respectively.
As the further scheme of the present invention：In step S2, the amount of added 0.5%H2SO4 solution is can moisten crude drug powder
It is wet to be defined, and fully mix thoroughly, place half an hour.
As the further scheme of the present invention：In step S4, net sand must clean drying in advance, and the amount of mixing and stirring is preferably shorter than
120 parts by weight.
As the further scheme of the present invention：In step S4, check whether alkaloid puies forward most method and be：Take last time
About few drops of ether extracted liquid, ether is flung to, after residue adds 5%HCl 0.5ml to dissolve, add improvement Dragendorff's reagent one to drip, without heavy
When shallow lake folds or be obvious muddy, show that alkaloid has been carried to the greatest extent, conversely, should continue to extract.
As the further scheme of the present invention：The eluant, eluent is preferably thiacyclohexane-ashamed acetoacetic ester-diethylamine by 6：2：
0.8 ratio mixed solution.
Compared with prior art, the beneficial effects of the invention are as follows：The present invention is carried out by way of acid solution diacolation to former material
Processing, can remove in advance it is more it is non-need alkaloid substance, such as Cyclanoline, simplify the process of later separation, and pass through
Tetrandrine and B prime efficiently, rapidly can be kept completely separate separation by the method for low pressure column chromatography separation, mutually be undoped, purity
It is very high, quality better.
Embodiment
The technical scheme in the embodiment of the present invention is clearly and completely described below, it is clear that described embodiment
Only part of the embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, the common skill in this area
The every other embodiment that art personnel are obtained under the premise of creative work is not made, belong to the model that the present invention protects
Enclose.
In the embodiment of the present invention, a kind of preparation method of Fourstamen Stephania Root alkaloid, realized by following steps：
S1, the Fourstamen Stephania Root medicinal material of 100 parts by weight is taken, is ground by grinder, obtains coarse powder；
S2,0.5%H2SO4 solution is added into coarse powder, is sufficiently stirred, obtains sour water percolate；
S3, fresh milk of lime is slowly added into sour water percolate, regulation pH value to 9-10, is filtered after standing 15 minutes, is removed
Alkaline solution obtains mud yellow mercury oxide；
S4, net sand is added into mud yellow mercury oxide, and stirred to being sufficiently mixed, be placed into 80 DEG C of drying bakers and dry, then divided
Criticize to be introduced into apparatus,Soxhlet's repeatedly to be extracted to biological alkali carries with ether and use up, reclaim ether, obtain ether extract；
S5, with 95%, 40-60ml ethanol solutions backflow thermosol, pour into 500ml water, the NaCl solution for adding 30 parts by weight is entered
Row is saltoutd, and is subsequently heated to condensation, is stood until precipitating completely, is filtered, obtained containing Tetrandrine and Fourstamen Stephania Root second
The white precipitate of element；
S6, low pressure column chromatography separation, specific method are：
S61, using decompression dry method dress method dress post, fill silica gel at least 30 parts by weight；
S62, add a small amount of acetone thermosol, be added on 1.5g silica gel with dropper, carefully mixed thoroughly, is evaporated in water-bath, it is fine ground, it is rear to add in vain
Color precipitates, and keeps its surfacing；
S63, elution, dropper carefully adds a small amount of eluant, eluent along chromatographic column post jamb, when liquid level reach a certain height, adds again
Enter remaining eluant, eluent, about 250ml, pressure needed for transfer, 0.6-1.2kg/cm2, flows out, coutroi velocity 1ml/ after about 40 minutes altogether
Point, manage within every 10 minutes or so one, receive 12-15 parts, elution overall process about 3 hours；
S64, each fraction move into small glass evaporators respectively, in being concentrated in water-bath, using Tetrandrine, B prime as standard items pair
According to merging same composition, acquisition first, B prime crude product, with acetone recrystallization, obtains alkaloid sterling respectively.
In step S2, the amount of added 0.5%H2SO4 solution is defined by that can soak crude drug powder, and is fully mixed thoroughly, is placed
Half an hour.
In step S4, net sand must clean drying in advance, and the amount of mixing and stirring is preferably shorter than 120 parts by weight.
In step S4, check whether alkaloid puies forward most method and be：Take last time ether extracted liquid about few drops, fling to second
Ether, after residue adds 5%HCl 0.5ml to dissolve, add improvement Dragendorff's reagent one to drip, when no precipitation folds or be obvious muddy, show
Alkaloid has been carried to the greatest extent, conversely, should continue to extract.
The eluant, eluent is preferably thiacyclohexane-ashamed acetoacetic ester-diethylamine by 6：2：0.8 ratio mixed solution.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie
In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit requires rather than described above limits, it is intended that all in the implication and scope of the equivalency of claim by falling
Change is included in the present invention.
Moreover, it will be appreciated that although the present specification is described in terms of embodiments, not each embodiment is only wrapped
Containing an independent technical scheme, this narrating mode of specification is only that those skilled in the art should for clarity
Using specification as an entirety, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
It is appreciated that other embodiment.
Claims (5)
- A kind of 1. preparation method of Fourstamen Stephania Root alkaloid, it is characterised in that：Realized by following steps：S1, the Fourstamen Stephania Root medicinal material of 100 parts by weight is taken, is ground by grinder, obtains coarse powder；S2,0.5%H2SO4 solution is added into coarse powder, is sufficiently stirred, obtains sour water percolate；S3, fresh milk of lime is slowly added into sour water percolate, regulation pH value to 9-10, is filtered after standing 15 minutes, is removed Alkaline solution obtains mud yellow mercury oxide；S4, net sand is added into mud yellow mercury oxide, and stirred to being sufficiently mixed, be placed into 80 DEG C of drying bakers and dry, then divided Criticize to be introduced into apparatus,Soxhlet's repeatedly to be extracted to biological alkali carries with ether and use up, reclaim ether, obtain ether extract；S5, with 95%, 40-60ml ethanol solutions backflow thermosol, pour into 500ml water, the NaCl solution for adding 30 parts by weight is entered Row is saltoutd, and is subsequently heated to condensation, is stood until precipitating completely, is filtered, obtained containing Tetrandrine and Fourstamen Stephania Root second The white precipitate of element；S6, low pressure column chromatography separation, specific method are：S61, using decompression dry method dress method dress post, fill silica gel at least 30 parts by weight；S62, add a small amount of acetone thermosol, be added on 1.5g silica gel with dropper, carefully mixed thoroughly, is evaporated in water-bath, it is fine ground, it is rear to add in vain Color precipitates, and keeps its surfacing；S63, elution, dropper carefully adds a small amount of eluant, eluent along chromatographic column post jamb, when liquid level reach a certain height, adds again Enter remaining eluant, eluent, about 250ml, pressure needed for transfer, 0.6-1.2kg/cm2, flows out, coutroi velocity 1ml/ after about 40 minutes altogether Point, manage within every 10 minutes or so one, receive 12-15 parts, elution overall process about 3 hours；S64, each fraction move into small glass evaporators respectively, in being concentrated in water-bath, using Tetrandrine, B prime as standard items pair According to merging same composition, acquisition first, B prime crude product, with acetone recrystallization, obtains alkaloid sterling respectively.
- A kind of 2. preparation method of Fourstamen Stephania Root alkaloid according to claim 1, it is characterised in that：It is added in step S2 The amount of 0.5%H2SO4 solution is defined by that can soak crude drug powder, and is fully mixed thoroughly, places half an hour.
- A kind of 3. preparation method of Fourstamen Stephania Root alkaloid according to claim 1, it is characterised in that：It is net husky in step S4 Drying must be cleaned in advance, and the amount of mixing and stirring is preferably shorter than 120 parts by weight.
- A kind of 4. preparation method of Fourstamen Stephania Root alkaloid according to claim 1, it is characterised in that：In step S4, check Whether alkaloid puies forward most method：Take last time ether extracted liquid about few drops, fling to ether, residue adds 5%HCl 0.5ml After dissolving, add improvement Dragendorff's reagent one to drip, when no precipitation folds or be obvious muddy, show that alkaloid has carried to the greatest extent, conversely, should Continue to extract.
- A kind of 5. preparation method of Fourstamen Stephania Root alkaloid according to claim 1, it is characterised in that：The eluant, eluent is preferred 6 are pressed for thiacyclohexane-ashamed acetoacetic ester-diethylamine：2：0.8 ratio mixed solution.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710713252.2A CN107496508A (en) | 2017-08-18 | 2017-08-18 | A kind of preparation method of Fourstamen Stephania Root alkaloid |
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| CN201710713252.2A CN107496508A (en) | 2017-08-18 | 2017-08-18 | A kind of preparation method of Fourstamen Stephania Root alkaloid |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110179799A (en) * | 2019-06-20 | 2019-08-30 | 中国人民解放军军事科学院军事医学研究院 | The application of tetrandrine and the extracting method of tetrandrine |
| CN111153909A (en) * | 2020-01-17 | 2020-05-15 | 石药集团江西金芙蓉药业股份有限公司 | A double-template molecular imprinting purification method for alpha-and beta-carotene in Stephania tetrandra |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102285994A (en) * | 2011-08-30 | 2011-12-21 | 聊城大学 | Method for separating and purifying fangchinoline and tetrandrine from stephania tetrandra |
-
2017
- 2017-08-18 CN CN201710713252.2A patent/CN107496508A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102285994A (en) * | 2011-08-30 | 2011-12-21 | 聊城大学 | Method for separating and purifying fangchinoline and tetrandrine from stephania tetrandra |
Non-Patent Citations (1)
| Title |
|---|
| 杨玉红等: "《生命科学综合实验指导》", 31 July 2016 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110179799A (en) * | 2019-06-20 | 2019-08-30 | 中国人民解放军军事科学院军事医学研究院 | The application of tetrandrine and the extracting method of tetrandrine |
| CN111153909A (en) * | 2020-01-17 | 2020-05-15 | 石药集团江西金芙蓉药业股份有限公司 | A double-template molecular imprinting purification method for alpha-and beta-carotene in Stephania tetrandra |
| CN111153909B (en) * | 2020-01-17 | 2022-05-17 | 石药集团江西金芙蓉药业股份有限公司 | A double-template molecular imprinting purification method for alpha-and beta-carotene in Stephania tetrandra |
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