CN107118219A - The method of separating-purifying gelsevirine, koumidine, koumine, gelsemine and furans koumine from elegant jessamine - Google Patents
The method of separating-purifying gelsevirine, koumidine, koumine, gelsemine and furans koumine from elegant jessamine Download PDFInfo
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- CN107118219A CN107118219A CN201710444073.3A CN201710444073A CN107118219A CN 107118219 A CN107118219 A CN 107118219A CN 201710444073 A CN201710444073 A CN 201710444073A CN 107118219 A CN107118219 A CN 107118219A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D491/00—Heterocyclic compounds containing in the condensed ring system both one or more rings having oxygen atoms as the only ring hetero atoms and one or more rings having nitrogen atoms as the only ring hetero atoms, not provided for by groups C07D451/00 - C07D459/00, C07D463/00, C07D477/00 or C07D489/00
- C07D491/12—Heterocyclic compounds containing in the condensed ring system both one or more rings having oxygen atoms as the only ring hetero atoms and one or more rings having nitrogen atoms as the only ring hetero atoms, not provided for by groups C07D451/00 - C07D459/00, C07D463/00, C07D477/00 or C07D489/00 in which the condensed system contains three hetero rings
- C07D491/18—Bridged systems
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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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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D491/00—Heterocyclic compounds containing in the condensed ring system both one or more rings having oxygen atoms as the only ring hetero atoms and one or more rings having nitrogen atoms as the only ring hetero atoms, not provided for by groups C07D451/00 - C07D459/00, C07D463/00, C07D477/00 or C07D489/00
- C07D491/22—Heterocyclic compounds containing in the condensed ring system both one or more rings having oxygen atoms as the only ring hetero atoms and one or more rings having nitrogen atoms as the only ring hetero atoms, not provided for by groups C07D451/00 - C07D459/00, C07D463/00, C07D477/00 or C07D489/00 in which the condensed system contains four or more hetero rings
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Abstract
The invention discloses a kind of method that separation gelsevirine, koumidine, koumine, gelsemine and furans koumine are extracted from elegant jessamine.This method is that elegant jessamine raw material is extracted using aqueous acid, is neutralized, it is dried under reduced pressure to obtain gelseminic acid scopoletin water extract, gelseminic acid scopoletin water extract is extracted by organic solvent, concentrated, water dissolving, after freeze-drying, obtain elegant jessamine extract powder, powder respectively obtains gelsevirine, koumidine, koumine, gelsemine and furans koumine by separation, purifying.This method can extract gelsevirine, koumidine, koumine, gelsemine and the furans koumine of separating high-purity from elegant jessamine, and simple to operate, cost is low, separated while realizing a variety of alkaloids in elegant jessamine, be conducive to the comprehensive utilization of natural resources.
Description
Technical field
The present invention relates to a kind of method that alkaloid is extracted from elegant jessamine, more particularly to from elegant jessamine (Gelsemium
Elegans Benth.) in simultaneously separating-purifying gelsevirine, koumidine, koumine, gelsemine and furans gelsemicine
The method of son, belongs to natural drug and extracts field.
Background technology
Elegant jessamine is the herb of loganiaceae plant Gelsemium el-egans, also known as gelsemium elegan, elegant jessamine, poison root, big tea medicine etc..Bitter, Xin Wei,
Property heat, it is very toxic.It is mainly distributed on the ground such as Zhejiang, Fujian, Guangdong, Guangxi, Hunan, Guizhou and Yunnan.It is conventional in traditional Chinese medicine
To treat rheumatoid arthritis pain, neuropathic pain, skin ulcer etc..At aspect for animals, few dosage elegant jessamine can be to some
Animal has somatotrophic effect.Indoles alkaloid is mainly rich in elegant jessamine.More than 120 kinds are had now been found that, it is some of biological
Alkali has been shown to have good antitumor, anti-inflammatory and antalgic, immunization isoreactivity.Clinically, also often it is used to suppress liver
Growth of tumour cell, preparation treatment medicine for treating rheumatoid arthritis, anxiety disease drug, chronic ache medicine etc..Therefore in elegant jessamine
Alkaloid be its pharmacological activity a class important component.Koumine is content highest but the relatively low class life of toxicity in elegant jessamine
Neuropathic pain, ethyl ester neuroglial cytoma U251 can be treated on alkaloids, its pharmacological activity, and with apoptosis-induced effect,
Also there is anti-stress effect etc. simultaneously.The alkaloid that gelsemine is separated in elegant jessamine is only second to sub-prime, can suppress swollen
Tumor cell growth, and show as in chronic ache strong effective analgesic activity.The preparation of presently disclosed koumine, plain first
Method is removed and prepared using high speed adverse current chromatogram from gelsemium total alkaloidses；Also extracted in elegant jessamine alcohol extract with ethyl acetate
After taking, then with silica gel column chromatography it is isolated and purified.Equipment needed for high speed adverse current chromatogram method is expensive, and yield is low, consumptive material
It is many.The a certain class or a few classes in elegant jessamine indoles alkaloid may can only be obtained by extraction in ethyl acetate method, and related alkaloids can
It can not be extracted and obtain, therefore more related alkaloids can not be separated to.Koumidine and gelsevirine are separated in elegant jessamine
Two indoles alkaloids arrived, its pharmacological action has the effects such as suppression growth of tumour cell, analgesia, calmness.At present, do not occur
The relevant report of the preparation technology of koumidine and gelsevirine.Therefore, the deficiency of its separation means is to limit its medical usage
A main cause.
Elegant jessamine complicated component, active component is separated based on gelsemine and koumine.Only have a small number of enterprises pair at present
The a certain single component of elegant jessamine is separated, and other compositions do offal treatment, causes the unreasonable of the utilization of resources, and only right
Elegant jessamine raw material carry out a certain monomer or the separation of total alkali has been reported that, but are carried out for elegant jessamine as raw material to a variety of alkaloids
While extracting and developing and purifying, also have no report.
The content of the invention
Multi-medicament composition can not be separated simultaneously by existing for prior art to the separation of the active constituents of medicine in elegant jessamine,
The waste of active ingredient is caused, and separated monomer process is had nothing in common with each other, the obtained low defect of active ingredient yield.This hair
Bright purpose is to provide one kind from elegant jessamine while extracting separating high-purity gelsevirine, koumidine, koumine, elegant jessamine
The method of plain first and furans koumine, this method is simple to operate, and cost is low, realizes the comprehensive utilization of natural resources.
In order to realize above-mentioned technical purpose, the invention provides one kind from elegant jessamine separating-purifying gelsevirine, kounidine
Pentath, the method for koumine, gelsemine and furans koumine, this method comprises the following steps：
1) after elegant jessamine is crushed, sour water extraction is carried out successively, neutralizes and dries, sour extract is obtained；The sour extract
Organic solvent extraction, sedimentation are carried out successively and is centrifuged, and obtain medicinal extract I, the medicinal extract I by hot water dissolving, freeze-drying,
Obtain powder；
2) powder is used in silica gel post separation, silica gel column separation process using dichloro methane-methanol as eluant, eluent
Carry out gradient elution, collect the cut containing identical component, and vacuum distillation respectively successively, obtain the medicinal extract II containing gelsevirine,
Medicinal extract III containing koumidine, the medicinal extract IV containing koumine, the leaching of the medicinal extract V containing gelsemine and the koumine containing furans
Cream VI；
3) the medicinal extract II is decolourized using silicagel column purifying and gel column, obtains gelsevirine；In silicagel column purge process
Using methylene chloride-methanol-ammonia spirit as eluant, eluent, gel column decolorization is using methanol as eluant, eluent；
4) the medicinal extract III is purified using silicagel column, obtains koumidine；In silicagel column purge process with dichloromethane-
Methanol-ammonia water is eluant, eluent；
5) the medicinal extract IV is purified using silicagel column, obtains koumine；With dichloromethane-first in silicagel column purge process
Alcohol-ammonia spirit is eluant, eluent；
6) the medicinal extract V is purified using silicagel column, obtains gelsemine；With dichloromethane-first in silicagel column purge process
Alcohol-ammonia spirit is eluant, eluent；
7) the medicinal extract VI is purified using silicagel column, obtains furans koumine；With dichloromethane in silicagel column purge process
Alkane-methanol-ammonia water is eluant, eluent.
It is preferred that scheme, the sour water, which was carried, takes the process to be：Solid-to-liquid ratio is 1:6~10kg/L, extract solution is that inorganic acid is molten
Liquid, extraction time is 20~28h, and extraction time is 2~3 times.The inorganic acid concentration is in the range of 0.2~0.8wt%.It is described
Inorganic acid is at least one of hydrochloric acid, sulfuric acid, phosphoric acid；Most preferably sulfuric acid solution.
It is preferred that scheme, the organic solvent extraction process is：Solid-to-liquid ratio is 1:1~2kg/L, extract solution is formic acid, second
At least one of alcohol, methanol, dichloromethane, ethylene glycol, n-hexane, petroleum ether；Extracting temperature is reflux temperature, and extraction time is
1~3h, extraction time is 2~3 times.Extract solution is preferably the ethanol that concentration is 85~95wt%；Most preferably concentration is
90wt%.
It is preferred that scheme, the medicinal extract I is freeze-dried using after 45~55 DEG C of hot water dissolvings under -20 DEG C of temperature below
24~48h obtains dried powder.
More preferably scheme, step 2) gradient elution during in methylene chloride-methanol volume ratio be 9:When 1, successively
It is collected into containing gelsevirine, koumidine, koumine and gelsemine cut, is 7 in methylene chloride-methanol volume ratio:3
When, collect the cut of the koumine containing furans.It is difficult to isolated above-mentioned contain in the methylene chloride-methanol system of other ratios
The cut of gelsevirine, koumidine, koumine and gelsemine or furans koumine.
More preferably scheme, step 3) in, the medicinal extract II first uses 40*600mm silicagel columns, using volume ratio as 95:5:
1/20~90:10:1/20 methylene chloride-methanol-ammonia spirit is that eluant, eluent is eluted, and collects evaporating containing gelsevirine
Point, vacuum distillation obtains medicinal extract II-1；The medicinal extract II-1 uses 25*500mm silicagel columns, using volume ratio as 20:0.8:1/20
Methylene chloride-methanol-ammonia spirit is that eluant, eluent is eluted, and collects the cut containing gelsevirine, vacuum distillation obtains medicinal extract
II-2；The medicinal extract II-2 uses 20*1800mm gel columns, with pure methanol eluant, eluent, collects the cut containing gelsevirine, decompression
Distillation, obtains medicinal extract II-3；The medicinal extract II-3 uses 10*400mm silicagel columns, using volume ratio as 19:0.7:1/20 dichloromethane
Alkane-methanol-ammonia water be eluant, eluent eluted, collection the cut containing gelsevirine, vacuum distillation, obtain purity 98% with
On gelsevirine.
More preferably scheme, step 4) in, the medicinal extract III first uses 40*600mm silicagel columns, using volume ratio as 95:5:
1/20~90:10:1/20 methylene chloride-methanol-ammonia spirit is that eluant, eluent is eluted, and collects evaporating containing koumidine
Point, vacuum distillation obtains medicinal extract III-1；The medicinal extract III-1 uses 25*500mm silicagel columns, using volume ratio as 20:0.8:1/20
Methylene chloride-methanol-ammonia spirit eluted for eluant, eluent, cut of the collection containing koumidine, vacuum distillation obtains purity
Koumidine more than 96%.
More preferably scheme, step 5) in, the medicinal extract IV first uses 40*600mm silicagel columns, using volume ratio as 95:5:
1/20~90:10:1/20 methylene chloride-methanol-ammonia spirit is that eluant, eluent is eluted, and collects evaporating containing koumine
Point, vacuum distillation obtains medicinal extract IV-1；The medicinal extract IV-1 uses 25*500mm silicagel columns, using volume ratio as 20:0.8:1/20
Methylene chloride-methanol-ammonia spirit is that eluant, eluent is eluted, and collects the cut containing koumine, vacuum distillation obtains purity and existed
More than 98% koumine.
More preferably scheme, step 6) in, the medicinal extract V uses 40*600mm silicagel columns, using volume ratio as 95:5:1/20
~90:10:1/20 methylene chloride-methanol-ammonia spirit is that eluant, eluent is eluted, and collects the cut containing gelsemine, subtracts
Pressure distillation, obtains gelsemine of the purity more than 92%.
More preferably scheme, step 7) in, the medicinal extract VI first uses 40*600mm silicagel columns, using volume ratio as 95:5:
1/20 methylene chloride-methanol-ammonia spirit is that eluant, eluent is eluted, and collects the cut of the koumine containing furans, and decompression is steamed
Evaporate, obtain the furans koumine of purity 93%.
N-process is used in alkali in technical scheme and sour water extraction solution is to neutrality.Alkali is sodium hydroxide
And/or potassium hydroxide.Optimal is sodium hydroxide；Concentration of sodium hydroxide solution is 8mol/L.
The process that methylene chloride-methanol system carries out gradient elution in technical scheme is dichloromethane-methanol
By volume from 100:0 to 0:100 carry out gradient elution.The dichloromethane and methanol of the present invention is by a large amount of as solvent
The optimal solvent combination that optimum experimental is obtained, if not reaching separation effect using other components replacement dichloromethane or methanol
Really.Petroleum ether and acetone as conventional can not also deploy.The eluant, eluent of the present invention is made using methylene chloride-methanol-ammonia spirit
For eluant, eluent, appropriate ammoniacal liquor can effectively solve compound tailing problem in separation process.
The gel column of the present invention uses pure methanol solvent, can ensure that recycling for gel column.
Compared with the prior art, the beneficial effect that technical scheme is brought：Elegant jessamine extraction process of the prior art
In it is general be only capable of extracting that separation is a small number of to plant active principles, cause the wasting of resources, such as gelseminic acid scopoletin water extract is industrial abstract hook
Kiss the discarded object after active principle.Technical scheme, using elegant jessamine as raw material, obtains sour water extract, and by simple
Technique isolates gelsevirine, koumidine, koumine, gelsemine and the furans koumine of high-purity simultaneously, wherein,
Gelsevirine purity reaches 98%, and the purity of other components reaches more than 92%, natural elegant jessamine resource is obtained comprehensive profit
With, and the method for extraction separation is simple to operate, cost is low.
Brief description of the drawings
【Fig. 1】HPLC collection of illustrative plates, EIC figures, the second order spectrum of respectively obtained gelsevirine；
【Fig. 2】For the HPLC collection of illustrative plates of obtained koumidine, EIC figures, second order spectrum；
【Fig. 3】For the HPLC collection of illustrative plates of obtained koumine, EIC figures, second order spectrum；
【Fig. 4】For the HPLC collection of illustrative plates of obtained gelsemine, EIC figures, second order spectrum；
【Fig. 5】For the HPLC collection of illustrative plates of obtained furans koumine, EIC figures, second order spectrum；
【Fig. 6】To do eluant, eluent, 3 using petroleum ether-acetone：1 plate design sketch；
【Fig. 7】For the process chart of the present invention.
Embodiment
Following examples are intended to further illustrate present invention, rather than limit the protection model of the claims in the present invention
Enclose.
Embodiment 1
Extract：By the 100kg elegant jessamines crushed plus 800L 0.5% sulfuric acid solution, in the acidproof extraction that capacity is 1000L
24h is extracted in stirring in tank, and decoction is filtered with 200 mesh filter screens, and the dregs of a decoction are extracted 1 time with method again, are merged extract solution twice, are used hydroxide
Sodium (8mol/L) adjusts pH to neutrality, is then put in concentration tank and is concentrated into relative density 1.2 or so, is produced after being dried under reduced pressure.Claim
Sour water extract 1kg is kissed in hook taking, puts into 5L round bottom cucurbits, adds 90% alcohol reflux and extracts 2 times, 1.5L is added every time, is carried
2h is taken, extract solution liquid collects extract solution twice after gauze simple filtration, place sedimentation 2h after merging again, then pass through centrifuge
Centrifugate is obtained after centrifugation, concentration centrifugate obtains medicinal extract, added after 45-55 DEG C of hot water dissolving, -20 DEG C of freeze-drying 48h obtain 138g
Dried powder.
Separation：By 138g dried powders, 280g 200-300 mesh silica gel mixed samples are added, addition has filled 1.5kg 200-300
In the chromatographic column of mesh silica gel.Add methylene chloride-methanol (100:0-0:100) system gradient elution.By eluent thin layer silica gel
Plate (GF254) point plate merges single identical component cut after being observed under uviol lamp 254nm.Obtain containing gelsevirine, hook successively
Kiss alkali penta, koumine, gelsemine and furans koumine eluting fraction.
Purifying：Concentration gelsevirine, koumidine, koumine, gelsemine and the elution of furans koumine evaporate respectively
Point.Contain gelsevirine cut (solvent dichloromethane：Methanol is 9:1) solvent, is recovered under reduced pressure, extractum A is obtained；Gained extractum A
From 40*600mm silicagel columns, with dichloromethane：Methanol：Ammoniacal liquor volume ratio is 95:5:1/20-90:10:1/20 enters for eluant, eluent
Row elution；After thin layer point plate, merge the cut containing gelsevirine, solvent is recovered under reduced pressure, medicinal extract B is obtained；Gained medicinal extract B is selected
25*500mm silicagel column, with dichloromethane：Methanol：Ammoniacal liquor volume ratio 20:0.8:1/20 is that eluant, eluent is eluted, through thin layer
After point plate, merge the cut containing gelsevirine, solvent is recovered under reduced pressure, medicinal extract C is obtained；Medicinal extract C obtained by (purifying of 3 gel chromatographies) is again
Decolourized with 20*1800mm gel columns, eluent is collected by solvent of pure methanol, after thin layer point plate, merging contains hook
The cut of green alkali is kissed, solvent is recovered under reduced pressure, medicinal extract D is obtained；Gained medicinal extract D selects 10*400mm silicagel column, dichloromethane：First
Alcohol：Ammoniacal liquor volume 19:0.7:1/20；Eluted for eluant, eluent, after thin layer point plate, produce the gelsevirine (purity of purifying
98%).
Cut (solvent dichloromethane containing koumidine：Methanol is 9:1) solvent, is recovered under reduced pressure, extractum A is obtained；Institute
Obtain extractum A and select 40*600mm silicagel columns, with dichloromethane：Methanol：Ammoniacal liquor volume ratio is 95:5:1/20-90:10:1/20 is
Eluant, eluent is eluted；After thin layer point plate, merge the cut containing koumidine, solvent is recovered under reduced pressure, medicinal extract B is obtained；Gained
Medicinal extract B selects 25*500mm silicagel column, with dichloromethane：Methanol：Ammoniacal liquor volume ratio 20:0.8:1/20 is that eluant, eluent is washed
It is de-, after thin layer point plate, merge the cut containing koumidine, solvent is recovered under reduced pressure, producing the koumidine of purifying, (purity is
96%).
Cut (solvent dichloromethane containing koumine：Methanol is 9:1) solvent, is recovered under reduced pressure, extractum A is obtained；Institute
Obtain extractum A and select 40*600mm silicagel columns, with dichloromethane：Methanol：Ammoniacal liquor volume ratio is 95:5:1/20-90:10:1/20 is
Eluant, eluent is eluted；After thin layer point plate, merge the cut containing koumine, solvent is recovered under reduced pressure, medicinal extract B is obtained；Gained
Medicinal extract B selects 25*500mm silicagel column, with dichloromethane：Methanol：Ammoniacal liquor volume ratio 20:0.8:1/20 is that eluant, eluent is washed
It is de-, after thin layer point plate, merge the cut containing koumine, solvent is recovered under reduced pressure, the koumine (purity of purifying is obtained
98%).
Cut (solvent dichloromethane containing gelsemine：Methanol is 9:1) solvent, is recovered under reduced pressure, extractum A is obtained；Institute
Obtain extractum A and select 40*600mm silicagel columns, with dichloromethane：Methanol：Ammoniacal liquor volume ratio is 95:5:1/20-90:10:1/20 is
Eluant, eluent is eluted；After thin layer point plate, merge the cut containing gelsemine, solvent is recovered under reduced pressure, the elegant jessamine of purifying is obtained
Plain first (purity 92%).
Cut (solvent dichloromethane containing furans koumine：Methanol is 7:3) solvent, is recovered under reduced pressure, medicinal extract is obtained
A；Gained extractum A selects 40*600mm silicagel columns, with dichloromethane：Methanol：Ammoniacal liquor volume ratio is 95:5:1/20 enters for eluant, eluent
Row elution；After thin layer point plate, merge the cut containing furans koumine, solvent is recovered under reduced pressure, the furans hook of purifying is produced
Kiss sub-prime (purity is 93%).
Comparative example 1
Extract：By the 100kg elegant jessamines crushed plus 800L 0.5% sulfuric acid solution, in the acidproof extraction that capacity is 1000L
24h is extracted in stirring in tank, and decoction is filtered with 200 mesh filter screens, and the dregs of a decoction are extracted 1 time with method again, are merged extract solution twice, are used hydroxide
Sodium (8mol/L) adjusts PH to neutrality, is then put in concentration tank and is concentrated into relative density 1.2 or so, is produced after being dried under reduced pressure.Claim
Sour water extract 1kg is kissed in hook taking, puts into 5L round bottom cucurbits, adds 90% alcohol reflux and extracts 2 times, 1.5L is added every time, is carried
Take 2h, extract solution collects extract solution twice after gauze simple filtration, place sedimentation 2h after merging again, then by centrifuge from
Centrifugate is obtained after the heart, concentration centrifugate obtains medicinal extract, added after 45-55 DEG C of hot water dissolving, -20 DEG C of freeze-drying 48h obtain 138g
Dried powder.
Separation：By 138g dried powders, 280g200-300 mesh silica gel mixed samples are added, addition has filled 1.5kg200-300 mesh
In the chromatographic column of silica gel.Add petroleum ether-acetone (4:1-1:1) system gradient elution.By eluent thin layer silica gel plate (GF254)
Point plate under uviol lamp 254nm after being observed, and each cut can not well be separated in the ratio of the eluant, eluent, fail to obtain
The consistent composition with embodiment.
Claims (10)
1. the side of separating-purifying gelsevirine, koumidine, koumine, gelsemine and furans koumine from elegant jessamine
Method, it is characterised in that：
Comprise the following steps：
1) after elegant jessamine is crushed, sour water extraction is carried out successively, neutralizes and dries, sour extract is obtained；
The sour extract carries out organic solvent extraction, sedimentation and centrifuged successively, obtains medicinal extract I, the medicinal extract I through overheat
Water dissolving, freeze-drying, obtain powder；
2) powder uses the progress by eluant, eluent of dichloro methane-methanol in silica gel post separation, silica gel column separation process
Gradient elution, collects the cut containing identical component, and vacuum distillation respectively successively, respectively obtain the medicinal extract II containing gelsevirine,
Medicinal extract III containing koumidine, the medicinal extract IV containing koumine, the leaching of the medicinal extract V containing gelsemine and the koumine containing furans
Cream VI；
3) the medicinal extract II is decolourized using silicagel column purifying and gel column, obtains gelsevirine；With two in silicagel column purge process
Chloromethanes-methanol-ammonia water is eluant, eluent, and gel column decolorization is using methanol as eluant, eluent；
4) the medicinal extract III is purified using silicagel column, obtains koumidine；In silicagel column purge process with methylene chloride-methanol-
Ammonia spirit is eluant, eluent；
5) the medicinal extract IV is purified using silicagel column, obtains koumine；In silicagel column purge process with methylene chloride-methanol-
Ammonia spirit is eluant, eluent；
6) the medicinal extract V is purified using silicagel column, obtains gelsemine；With methylene chloride-methanol-ammonia in silicagel column purge process
The aqueous solution is eluant, eluent；
7) the medicinal extract VI is purified using silicagel column, obtains furans koumine；With dichloromethane-first in silicagel column purge process
Alcohol-ammonia spirit is eluant, eluent.
2. separating-purifying gelsevirine, koumidine, koumine, gelsemine according to claim 1 from elegant jessamine
With the method for furans koumine, it is characterised in that：The sour water, which was carried, takes the process to be：Solid-to-liquid ratio is 1:6~10kg/L, is extracted
Liquid is inorganic acid solution, and extraction time is 20~28h, and extraction time is 2~3 times.
3. separating-purifying gelsevirine, koumidine, koumine, gelsemine according to claim 1 from elegant jessamine
With the method for furans koumine, it is characterised in that：The organic solvent extraction process is：Solid-to-liquid ratio is 1:1~2kg/L, is carried
It is at least one of formic acid, ethanol, methanol, dichloromethane, ethylene glycol, n-hexane, petroleum ether to take liquid, and Extracting temperature is backflow temperature
Degree, extraction time is 1~3h, and extraction time is 2~3 times.
4. separating-purifying gelsevirine, koumidine, koumine, gelsemine according to claim 1 from elegant jessamine
With the method for furans koumine, it is characterised in that：It is warm below -20 DEG C after the medicinal extract I is using 45~55 DEG C of hot water dissolvings
24~48h of the lower freeze-drying of degree obtains dried powder.
5. according to any one of Claims 1 to 4 from elegant jessamine separating-purifying gelsevirine, koumidine, koumine,
The method of gelsemine and furans koumine, it is characterised in that：Step 2) gradient elution during in methylene chloride-methanol
Volume ratio is 9:When 1, it is collected into successively containing gelsevirine, koumidine, koumine and gelsemine cut, in dichloromethane
Alkane-methanol volume ratio is 7:When 3, the cut of the koumine containing furans is collected.
6. the high-purity gelsevirine of the separating-purifying from elegant jessamine, koumidine, elegant jessamine according to any one of Claims 1 to 4
The method of sub-prime, gelsemine and furans koumine, it is characterised in that：Step 3) in, the medicinal extract II first uses 40*
600mm silicagel columns, using volume ratio as 95:5:1/20~90:10:1/20 methylene chloride-methanol-ammonia spirit enters for eluant, eluent
Row elution, collects the cut containing gelsevirine, and vacuum distillation obtains medicinal extract II-1；The medicinal extract II-1 uses 25*500mm silica gel
Post, using volume ratio as 20:0.8:1/20 methylene chloride-methanol-ammonia spirit is that eluant, eluent is eluted, and collects green containing elegant jessamine
The cut of alkali, vacuum distillation obtains medicinal extract II-2；The medicinal extract II-2 uses 20*1800mm gel columns, with pure methanol eluant, eluent,
The cut containing gelsevirine is collected, vacuum distillation obtains medicinal extract II-3；The medicinal extract II-3 uses 10*400mm silicagel columns, with body
Product is than being 19:0.7:1/20 methylene chloride-methanol-ammonia spirit is that eluant, eluent is eluted, and collects evaporating containing gelsevirine
Point, vacuum distillation obtains gelsevirine of the purity more than 98%.
7. according to any one of Claims 1 to 4 from elegant jessamine separating-purifying gelsevirine, gelsevirine, koumidine,
The method of koumine, gelsemine and furans koumine, it is characterised in that：Step 4) in, the medicinal extract III is first used
40*600mm silicagel columns, using volume ratio as 95:5:1/20~90:10:1/20 methylene chloride-methanol-ammonia spirit is elution
Agent is eluted, and collects the cut containing koumidine, and vacuum distillation obtains medicinal extract III-1；The medicinal extract III-1 uses 25*
500mm silicagel columns, using volume ratio as 20:0.8:1/20 methylene chloride-methanol-ammonia spirit is that eluant, eluent is eluted, and is received
Collect the cut containing koumidine, vacuum distillation obtains koumidine of the purity more than 96%.
8. according to any one of Claims 1 to 4 from elegant jessamine separating-purifying gelsevirine, koumidine, koumine,
The method of gelsemine and furans koumine, it is characterised in that：Step 5) in, the medicinal extract IV first uses 40*600mm silica gel
Post, using volume ratio as 95:5:1/20~90:10:1/20 methylene chloride-methanol-ammonia spirit is that eluant, eluent is eluted, and is received
Collect the cut containing koumine, vacuum distillation obtains medicinal extract IV-1；The medicinal extract IV-1 uses 25*500mm silicagel columns, with volume
Than for 20:0.8:1/20 methylene chloride-methanol-ammonia spirit is that eluant, eluent is eluted, and collects the cut containing koumine,
Vacuum distillation, obtains koumine of the purity more than 98%.
9. according to any one of Claims 1 to 4 from elegant jessamine separating-purifying gelsevirine, koumidine, koumine,
The method of gelsemine and furans koumine, it is characterised in that：Step 6) in, the medicinal extract V uses 40*600mm silicagel columns,
Using volume ratio as 95:5:1/20~90:10:1/20 methylene chloride-methanol-ammonia spirit is that eluant, eluent is eluted, and is collected
Cut containing gelsemine, vacuum distillation obtains gelsemine of the purity more than 92%.
10. separating-purifying gelsevirine, koumidine, gelsemicine from elegant jessamine according to any one of Claims 1 to 4
The method of son, gelsemine and furans koumine, it is characterised in that：Step 7) in, the medicinal extract VI first uses 40*600mm
Silicagel column, using volume ratio as 95:5:1/20 methylene chloride-methanol-ammonia spirit is that eluant, eluent is eluted, and collects and contains furans
The cut of koumine, vacuum distillation obtains more than 93% furans koumine.
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| CN107894475A (en) * | 2017-11-20 | 2018-04-10 | 湖南农业大学 | The Liquid Chromatography-Tandem Mass Spectrometry quantitative approach that plurality of active ingredients detects simultaneously in elegant jessamine |
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| CN113440482A (en) * | 2021-08-19 | 2021-09-28 | 福建中医药大学 | Evergreen gelsemine microemulsion and preparation method thereof |
| CN114246863A (en) * | 2021-03-04 | 2022-03-29 | 上海大学 | Application of gelsemine in product for inhibiting osteoporosis |
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Cited By (5)
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| CN114246863A (en) * | 2021-03-04 | 2022-03-29 | 上海大学 | Application of gelsemine in product for inhibiting osteoporosis |
| CN113440482A (en) * | 2021-08-19 | 2021-09-28 | 福建中医药大学 | Evergreen gelsemine microemulsion and preparation method thereof |
| CN113440482B (en) * | 2021-08-19 | 2022-10-11 | 福建中医药大学 | Evergreen gelsemine microemulsion and preparation method thereof |
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