CN103694212B - A kind of purification process of Tridemethylsciadopitysin - Google Patents
A kind of purification process of Tridemethylsciadopitysin Download PDFInfo
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- CN103694212B CN103694212B CN201310617378.1A CN201310617378A CN103694212B CN 103694212 B CN103694212 B CN 103694212B CN 201310617378 A CN201310617378 A CN 201310617378A CN 103694212 B CN103694212 B CN 103694212B
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- tridemethylsciadopitysin
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- selaginella tamariscina
- general flavone
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/22—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
- C07D311/26—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
- C07D311/28—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only
- C07D311/30—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only not hydrogenated in the hetero ring, e.g. flavones
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/22—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
- C07D311/26—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
- C07D311/40—Separation, e.g. from natural material; Purification
Abstract
The invention discloses a kind of purification process of Tridemethylsciadopitysin, comprise the following steps: 1) obtain Selaginella tamariscina extractive of general flavone, Tridemethylsciadopitysin content >=30% in this Selaginella tamariscina extractive of general flavone; 2) by Selaginella tamariscina extractive of general flavone methyl alcohol or dissolve with ethanol, upper ADS-7 macroporous resin column, washed resin post is clarified to effluent liquid, then uses the hydrochloric acid wash-out of 0.5 ~ 2v/v%, collects elutriant; 3) pH to 4 ~ 6 adjusted by elutriant, concentrated, leave standstill crystallization, and collect crystal, gained crystal carries out recrystallization with methyl alcohol or ethanol again, filter, and collect crystal, dry, to obtain final product.The present invention adopts the ADS-7 macroporous resin with ion exchanging function while of both having had adsorption function to carry out chromatography to Selaginella tamariscina extractive of general flavone, while Tridemethylsciadopitysin is adsorbed on macroporous resin, serve extraordinary removal of impurities effect, make the purity of products obtained therefrom reach the product of more than 95%, and product yield is more than 71%.
Description
Technical field
The present invention relates to the extracting method of activeconstituents in plant, be specifically related to a kind of purification process of Tridemethylsciadopitysin.
Background technology
In China's coastal port, regulation Selaginella tamariscina is the dry herb of Spikemoss plant Selaginella tamariscina Selaginellatamariscina (Beauv.) Spring or Selaginella pulvinata Selaginella pulvinata (Hook.etGrev.) Maxim..Selaginella tamariscina is ornamental both, also pharmaceutically acceptable, and herb has the usefulness of hemostasis, convergence.Among the people its complete stool to be incinerated, for oral administrationly can treat various hemorrhage, and external application mixed by rape oil, can treat various knife wound.Modern medicine prove its have clearing heat and detoxicating, promoting blood circulation and removing blood stasis, stop blooding anticancer, cancer preventing and treating, anti-inflammatory, antiviral, anti-infective, antianaphylaxis, analgesia, hypnosis, hypotensive, hypoglycemic, strengthen the effects such as immune function of human body.Clinically Selaginella tamariscina be mainly used in treatment amenorrhoea, haematemesis, hematuria, have blood in stool, uterine bleeding, prolapse of the anus, wound, stomachache, asthma etc.
Functional component in Selaginella tamariscina mainly flavonoid, and be mainly biflavone.Herb is containing sotetsuflavone (sotetsuflavone), Tridemethylsciadopitysin (amentoflavone), hinokiflavone (hinokiflavone), isocryptomerin (isocryptomerin), cryptomeria biflavone (cryptomerin) B, apigenin (apigenin) and trehalose (trehalose).
The quality of chromatogram of Herba Selaginellae mainly with the content of Tridemethylsciadopitysin for standard, and in Herba Selaginellae extract also with Tridemethylsciadopitysin be major objective composition, its molecular formula is C
30h
180
10, molecular weight is 538.46.Fusing point is 256 " C.Pale yellow powder, is soluble in methyl alcohol, ethanol and acetone, and its structural formula is as follows:
Publication number is the patent of invention of CN101585825A, disclose a kind of preparation method of Tridemethylsciadopitysin, take Selaginella tamariscina as raw material, after the different concns mixing solutions of organic solvent and water extracts, concentrate and obtain medicinal extract, collecting precipitation thing, with organic solvent dissolution, enter silica gel column chromatography, with the organic solvent wash-out of different gradient, again through Sephadex LH-20 column chromatography after concentrated, finally use the organic solvent wash-out of different gradient again, use TLC tracing detection, after Fractional Collections concentrates, obtain the Tridemethylsciadopitysin highly finished product of more than 95%.The method needs through silica gel column chromatography and Sephadex LH-20 column chromatography, and technique is comparatively loaded down with trivial details on the one hand, and the cycle is longer; Will use silicagel column and Sephadex LH-20 post on the other hand, not only production cost is higher, and is not easy to realize industrialization.Publication number is the patent of invention of CN102178703A, disclose a kind of method extracting selaginella tamariscina biflavone, take Selaginella tamariscina as raw material, through sherwood oil and acetone extraction, inorganic salt and polyoxyethylene glycol is added in acetone extract, extract after stirring, taking polyethylene glycol carries out ultrafiltration and nanofiltration mutually, and reconcentration obtains selaginella tamariscina biflavone product.The method operation is comparatively simple, and can obtain the Tridemethylsciadopitysin product of content higher (more than 65%), but owing to using the polyoxyethylene glycol of high molecular, makes the more difficult control of technique; In addition, in extraction step, the grease in extracting solution can be dissolved in extraction agent, causes impurity in product more, and not easily dry; Moreover the ultrafiltration used in the method and nanofiltration equipment cost higher, during operation, energy consumption is also higher, and early investment is large.
Summary of the invention
The technical problem to be solved in the present invention is to provide the purification process of the Tridemethylsciadopitysin that a kind of cost is low, technique is simple and easy to control.In product obtained by this method, Tridemethylsciadopitysin content can reach more than 95% (HPLC method).
The purification process of Tridemethylsciadopitysin of the present invention, comprises the following steps:
1) Selaginella tamariscina extractive of general flavone is obtained, Tridemethylsciadopitysin content >=30% in this Selaginella tamariscina extractive of general flavone;
2) by Selaginella tamariscina extractive of general flavone methyl alcohol or dissolve with ethanol, upper ADS-7 macroporous resin column, washed resin post is clarified to effluent liquid, then uses the hydrochloric acid wash-out of 0.5 ~ 2v/v%, collects elutriant;
3) pH to 4 ~ 6 adjusted by elutriant, concentrated, leave standstill crystallization, and collect crystal, gained crystal carries out recrystallization with methyl alcohol or ethanol again, filter, and collect crystal, dry, obtain Tridemethylsciadopitysin.
The step 1 of above-mentioned purification process) in, described Selaginella tamariscina extractive of general flavone can directly commercially, also can prepare by existing ordinary method, preferably prepares by the following method:
A) take Selaginella tamariscina as raw material, the heating that adds water is extracted, and discards aqueous extract, collects chromatogram of Herba Selaginellae;
B) by step 1) chromatogram of Herba Selaginellae of gained adds methyl alcohol or ethanol, refluxing extraction, and collect alcohol eluen, concentrating under reduced pressure, concentrated solution is centrifugal, collecting precipitation thing;
Throw out No. 6 solvent oils or the petroleum ether and stirring degreasing of c) will collect, filter, and collects filter cake, dry, obtains Selaginella tamariscina extractive of general flavone.
Above-mentioned steps a) in, be preferably heated to 60 ~ 100 DEG C after addition of water and extract, be more preferably to 70 ~ 80 DEG C and extract; The number of times extracted is generally 1 ~ 3 time, extracts 0.5 ~ 2h at every turn, and during each extraction, the add-on of water is 5 ~ 12 times of raw material weight.Step b) in, the concentration of methyl alcohol is preferably 90 ~ 100v/v%, and the concentration of ethanol is preferably 70 ~ 100v/v%; The number of times extracted is generally 1 ~ 3 time, extracts 1 ~ 2h at every turn, and during each extraction, the add-on of methyl alcohol or ethanol is preferably 8 ~ 12 times of raw material weight; In this step, concentrated solution can be centrifugal while hot, also centrifugal again after can leaving standstill cooling, adopt and obtain relatively high Tridemethylsciadopitysin content in the centrifugal Selaginella tamariscina extractive of general flavone that can make to obtain while hot, adopt mode centrifugal again after leaving standstill cooling then can make to obtain relatively high Tridemethylsciadopitysin yield in the Selaginella tamariscina extractive of general flavone obtained.Step c) in, the time of described stirring degreasing, at more than 30min, is preferably 30 ~ 60min.In this step, the consumption of described No. 6 solvent oils or sherwood oil is 5 ~ 10 times of weight of precipitate.
Containing a large amount of water-soluble substanceses in Selaginella tamariscina, these water-soluble substanceses also can be extracted when direct methyl alcohol or extraction using alcohol, and Tridemethylsciadopitysin itself is water-soluble very poor, water-soluble hardly, so the very large burden of postorder purification procedures (as crossed the operation such as resin column, extraction) can be caused when direct methyl alcohol or extraction using alcohol extract Selaginella tamariscina, present method by first by water extraction and the operation discarding Aqueous extracts to remove water-soluble substanceses (being equivalent to impurity) a large amount of in Selaginella tamariscina, greatly reduce the burden of postorder purification procedures; In addition, usually adopt in prior art and add extraction agent extracting solution is extracted, conventional extraction agent is the organic solvents such as ethyl acetate, but the fat impurity such as the grease in extracting solution and other apolar substances also have certain solubleness in ethyl acetate, thus with a certain amount of fat impurity, the reduction of product purity can be caused in the organic phase of extracting operation collection; And the present invention stirs the operation of de-ester to the throw out collected, be the equal of that the fat impurity such as the grease in throw out and other apolar substances are dissolved in the de-ester solvent (No. 6 solvent oils or sherwood oil) added, by the mode of filtering, these impurity are separated with flavonoid extracts, effectively prevent because impurity is dissolved in extraction agent the phenomenon causing product purity to reduce, and being conducive to the drying of product, the proterties of products obtained therefrom is good.In the Selaginella tamariscina extractive of general flavone adopting aforesaid method to obtain, the content of Tridemethylsciadopitysin is 30 ~ 41%, and general flavone content is 62 ~ 70%.
The step 2 of above-mentioned purification process) in, for the consumption of the methyl alcohol or ethanol that dissolve Selaginella tamariscina extractive of general flavone and concentration same as the prior art, the concentration of particular methanol is 60 ~ 80v/v%, and the concentration of ethanol is 30 ~ 60v/v%; The consumption of particular methanol or ethanol is 8 ~ 20 times that dissolve Selaginella tamariscina extractive of general flavone weight.In this step, the hydrochloric acid soln of 1 ~ 2v/v% is preferably adopted to be used for wash-out.Thin-layer chromatography (TLC) tracing detection is adopted in the process of wash-out.
The step 3 of above-mentioned purification process) in, elutriant regulates its pH value with alkali lye such as sodium hydroxide solution, sodium carbonate solution or sodium hydrogen carbonate solutions usually, and the concentration of above-mentioned alkali lye is generally 5 ~ 20w/w%.Described for the methyl alcohol of recrystallization or the concentration of ethanol same as the prior art, the concentration of particular methanol is 60 ~ 80v/v%, and the concentration of ethanol is 30 ~ 60v/v%.In this step, normally the elutriant after adjust pH is concentrated into 2 ~ 4 times of raw material weight, the time leaving standstill crystallization crystallization is generally 24 ~ 72h.
Compared with prior art, the present invention adopts the ADS-7 macroporous resin with ion exchanging function while of both having had adsorption function to carry out chromatography to Selaginella tamariscina extractive of general flavone, while Tridemethylsciadopitysin is adsorbed on macroporous resin, serve extraordinary removal of impurities effect, make after resolving with hydrochloric acid soln, elutriant is through pH regulator, twice crystallization operation, the Tridemethylsciadopitysin product that purity reaches more than 95% (HPLC method) can be obtained, and the yield of Tridemethylsciadopitysin product (with content of Tridemethylsciadopitysin in Selaginella tamariscina extractive of general flavone for benchmark) more than 71%.
Embodiment
With specific embodiment, the invention will be further described below, but the present invention is not limited to these embodiments.
Embodiment 1
1) by Selaginella tamariscina raw material pulverizing to 20 ~ 40 order, get 100kg, the water adding 8 times of raw material weights is heated to 80 DEG C and extracts 1.5h, filters, discards filtrate, leave chromatogram of Herba Selaginellae;
2) chromatogram of Herba Selaginellae after water extraction adds the 80%(v/v of 10 times of raw material weights) ethanol, heating and refluxing extraction 1.5h, filters, and collects filtrate; Filter residue adds the 80%(v/v of 7 times of raw material weights again) ethanol, heating and refluxing extraction 1.5h, filters, and collects filtrate; Merging filtrate, obtains extracting solution, extracting solution concentration and recovery ethanol, and reconcentration is to the medicinal extract of raw material weight 1.5 times;
3) medicinal extract cooling leaves standstill 12 hours, centrifugal, collects filter cake;
4) smashed to pieces by filter cake, add No. 6 solvent oil degreasings (degreasing time is 60min, does not stop to stir in whole de-ester process) of filter cake weight 7 times amount, collecting by filtration filter cake, filter cake vacuum-drying, pulverizes, obtains 2.1kg Selaginella tamariscina extractive of general flavone; Products obtained therefrom outward appearance is chocolate brown powder, and it is 64.24% that ultraviolet spectrophotometry detects general flavone content, and wherein Tridemethylsciadopitysin is 32.16% through HPLC method detection level;
5) the Selaginella tamariscina extractive of general flavone 40%(v/v being equivalent to its weight 14 times of above-mentioned gained) ethanol heating for dissolving, cool the strong polar macroporous resin of laggard ADS-7, be washed to effluent liquid and become clear; Then use 1%(v/v) hydrochloric acid soln wash-out, collect elutriant; Elutriant 10% (w/w) sodium hydroxide solution adjusts it to pH=5 ~ 6, is then concentrated into 3 times of raw material weight, and cooling leaves standstill 30 hours, crystallization, and collecting by filtration crystal, obtains coarse crystal; Coarse crystal 30%(v/v) ethanol heating for dissolving, letting cool abundant crystallization, the crystal of collecting by filtration recrystallization, vacuum-drying, obtain Tridemethylsciadopitysin purified product 0.52kg, is 96.21% through HPLC detection level.
Embodiment 2
1) by Selaginella tamariscina raw material pulverizing to 20 order, get 200kg, the water adding 5 times of raw material weights is heated to 100 DEG C and extracts 0.5h, filters, discards filtrate, leave chromatogram of Herba Selaginellae;
2) chromatogram of Herba Selaginellae after water extraction adds the 95%(v/v of 10 times of raw material weights) ethanol, heating and refluxing extraction 1h, filters, and collects filtrate; Filter residue adds the 95%(v/v of 6 times of raw material weights again) ethanol, heating and refluxing extraction 1h, filters, and collects filtrate; Merging filtrate, obtains extracting solution, extracting solution concentration and recovery ethanol, and reconcentration is to the medicinal extract of raw material weight 2 times;
3) medicinal extract cooling leaves standstill 4 hours, centrifugal, collects filter cake;
4) smashed to pieces by filter cake, add the petroleum ether degreasing (degreasing time is 30min, does not stop to stir in whole de-ester process) of filter cake weight 5 times amount, collecting by filtration filter cake, filter cake vacuum-drying, pulverizes, obtains 4.6kg Selaginella tamariscina extractive of general flavone; Products obtained therefrom outward appearance is chocolate brown powder, and it is 63.47% that ultraviolet spectrophotometry detects general flavone content, and wherein Tridemethylsciadopitysin is 31.66% through HPLC method detection level;
5) the Selaginella tamariscina extractive of general flavone 30%(v/v being equivalent to its weight 20 times of above-mentioned gained) ethanol heating for dissolving, cool the strong polar macroporous resin of laggard ADS-7, be washed to effluent liquid and become clear; With 0.5%(v/v) hydrochloric acid soln wash-out, collect elutriant; Elutriant sodium hydroxide solution is neutralized to pH=4 ~ 5, is concentrated into 2 times of raw material weight, and cooling leaves standstill 72 hours, crystallization, and collecting by filtration crystal, obtains coarse crystal; Coarse crystal 30%(v/v) ethanol heating for dissolving, letting cool abundant crystallization, the crystal of collecting by filtration recrystallization, vacuum-drying, obtain Tridemethylsciadopitysin purified product 1.21kg, is 95.72% through HPLC detection level.
Embodiment 3
1) by Selaginella tamariscina raw material pulverizing to 10 ~ 20 order, get 150kg, the water adding 10 times of raw material weights is heated to 60 DEG C and extracts 2h, filters, discards filtrate, leave chromatogram of Herba Selaginellae;
2) chromatogram of Herba Selaginellae after water extraction adds the 70%(v/v of 12 times of raw material weights) ethanol, heating and refluxing extraction 2h, filters, and collects filtrate; Filter residue adds the 75%(v/v of 9 times of raw material weights again) ethanol, heating and refluxing extraction 2h, filters, and collects filtrate; Merging filtrate, obtains extracting solution, extracting solution concentration and recovery ethanol, and reconcentration is to the medicinal extract of material quantity 1 times;
3) medicinal extract cooling leaves standstill 4 hours, centrifugal, collects filter cake;
4) smashed to pieces by filter cake, add No. 6 solvent oil degreasings (degreasing time is 50min, does not stop to stir in whole de-ester process) of filter cake weight 10 times amount, collecting by filtration filter cake, filter cake vacuum-drying, pulverizes, obtains 3.2kg Selaginella tamariscina extractive of general flavone; Products obtained therefrom outward appearance is chocolate brown powder, and it is 62.7% that ultraviolet spectrophotometry detects general flavone content, and wherein Tridemethylsciadopitysin is 30.46% through HPLC method detection level;
5) the Selaginella tamariscina extractive of general flavone 50%(v/v being equivalent to its weight 8 times of above-mentioned gained) ethanol heating for dissolving, cool the strong polar macroporous resin of laggard ADS-7, be washed to effluent liquid and become clear; With 2%(v/v) hydrochloric acid soln wash-out, collect elutriant; Elutriant sodium hydroxide solution is neutralized to pH=5 ~ 5.5, is concentrated into 4 times amount of material quantity, and cooling leaves standstill 45 hours, crystallization, and collecting by filtration crystal, obtains coarse crystal; Coarse crystal 30%(v/v) ethanol heating for dissolving, letting cool abundant crystallization, the crystal of collecting by filtration recrystallization, vacuum-drying, obtain Tridemethylsciadopitysin purified product 0.73kg, is 95.83% through HPLC detection level.
Embodiment 4
1) by Selaginella tamariscina raw material pulverizing to 10 ~ 20 order, get 150kg, the water adding 10 times of raw material weights is heated to 100 DEG C and extracts 2h, filters, discards filtrate, leave chromatogram of Herba Selaginellae;
2) chromatogram of Herba Selaginellae after water extraction adds the 95%(v/v of 10 times of raw material weights) methyl alcohol, heating and refluxing extraction 2h, filters, and collects filtrate; Filter residue adds the 95%(v/v of 8 times of raw material weights again) methyl alcohol, heating and refluxing extraction 1.5h, filters, and collects filtrate; Filter residue adds the 95%(v/v of 8 times of raw material weights again) methyl alcohol, heating and refluxing extraction 1h, filters, and collects filtrate; Merging filtrate, obtains extracting solution, extracting solution concentration and recovery methyl alcohol, and reconcentration is to the medicinal extract of material quantity 1.5 times;
3) medicinal extract cooling leaves standstill 4 hours, centrifugal, collects filter cake;
4) smashed to pieces by filter cake, add the petroleum ether degreasing (degreasing time is 50min, does not stop to stir in whole de-ester process) of filter cake weight 8 times amount, collecting by filtration filter cake, filter cake vacuum-drying, pulverizes, obtains 3.4kg Selaginella tamariscina extractive of general flavone; Products obtained therefrom outward appearance is chocolate brown powder, and it is 61.94% that ultraviolet spectrophotometry detects general flavone content, and wherein Tridemethylsciadopitysin is 30.21% through HPLC method detection level;
5) the Selaginella tamariscina extractive of general flavone 60%(v/v being equivalent to its weight 8 times of above-mentioned gained) methyl alcohol heating for dissolving, cool the strong polar macroporous resin of laggard ADS-7, be washed to effluent liquid and become clear; With 1.5%(v/v) hydrochloric acid soln wash-out, collect elutriant; Elutriant sodium hydroxide solution is neutralized to pH=4, is concentrated into 2 times amount of material quantity, and cooling leaves standstill 60 hours, crystallization, and collecting by filtration crystal, obtains coarse crystal; Coarse crystal 70%(v/v) methyl alcohol heating for dissolving, letting cool abundant crystallization, the crystal of collecting by filtration recrystallization, vacuum-drying, obtain Tridemethylsciadopitysin purified product 0.77kg, is 95.37% through HPLC detection level.
Embodiment 5
Get Selaginella tamariscina extractive of general flavone 7.5kg (being purchased from Kang Lu bio tech ltd, Hunan), wherein general flavone content is 62.56%, Tridemethylsciadopitysin content is 30.16%), 40%(v/v with being equivalent to its weight 8 times) ethanol heating for dissolving, cool the strong polar macroporous resin of laggard ADS-7, be washed to effluent liquid and become clear; With 1.5%(v/v) hydrochloric acid soln wash-out, collect elutriant; Elutriant sodium hydroxide solution is neutralized to pH=4.5, is concentrated into 3 times amount of material quantity, and cooling leaves standstill 30 hours, crystallization, and collecting by filtration crystal, obtains coarse crystal; Coarse crystal 40%(v/v) ethanol heating for dissolving, letting cool abundant crystallization, the crystal of collecting by filtration recrystallization, vacuum-drying, obtain Tridemethylsciadopitysin purified product 1.68kg, is 96.76% through HPLC detection level.
Claims (7)
1. a purification process for Tridemethylsciadopitysin, comprises the following steps:
1) Selaginella tamariscina extractive of general flavone is obtained, Tridemethylsciadopitysin content >=30% in this Selaginella tamariscina extractive of general flavone; The step of described acquisition Selaginella tamariscina extractive of general flavone comprises the following steps:
A) take Selaginella tamariscina as raw material, the heating that adds water is extracted, and discards aqueous extract, collects chromatogram of Herba Selaginellae;
B) by step 1) chromatogram of Herba Selaginellae of gained adds methyl alcohol or ethanol, refluxing extraction, and collect alcohol eluen, concentrating under reduced pressure, concentrated solution is centrifugal, collecting precipitation thing;
Throw out No. 6 solvent oils or the petroleum ether and stirring degreasing of c) will collect, filter, and collects filter cake, dry, obtains Selaginella tamariscina extractive of general flavone;
2) by Selaginella tamariscina extractive of general flavone methyl alcohol or dissolve with ethanol, upper ADS-7 macroporous resin column, washed resin post is clarified to effluent liquid, then uses the hydrochloric acid wash-out of 0.5 ~ 2v/v%, collects elutriant;
3) pH to 4 ~ 6 adjusted by elutriant, concentrated, leave standstill crystallization, and collect crystal, gained crystal carries out recrystallization with methyl alcohol or ethanol again, filter, and collect crystal, dry, obtain Tridemethylsciadopitysin.
2. the purification process of Tridemethylsciadopitysin according to claim 1, is characterized in that: step 2) in, be 60 ~ 80v/v% for dissolving the concentration of the methyl alcohol of Selaginella tamariscina extractive of general flavone, the concentration of ethanol is 30 ~ 60v/v%.
3. the purification process of Tridemethylsciadopitysin according to claim 1, is characterized in that: step 3) in, the concentration for the methyl alcohol of recrystallization is 60 ~ 80v/v%, and the concentration of ethanol is 30 ~ 60v/v%.
4. the purification process of the Tridemethylsciadopitysin according to any one of claims 1 to 3, is characterized in that: step c) in, the time of described stirring degreasing is 30 ~ 60min.
5. the purification process of the Tridemethylsciadopitysin according to any one of claims 1 to 3, is characterized in that: step c) in, the consumption of described No. 6 solvent oils or sherwood oil is 5 ~ 10 times of weight of precipitate.
6. the purification process of the Tridemethylsciadopitysin according to any one of claims 1 to 3, is characterized in that: step a) in, post-heating to 60 ~ 100 DEG C that add water are extracted.
7. the purification process of the Tridemethylsciadopitysin according to any one of claims 1 to 3, is characterized in that: step b) in, the concentration of methyl alcohol is 90 ~ 100v/v%, and the concentration of ethanol is 70 ~ 100v/v%.
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| CN106872611A (en) * | 2017-04-17 | 2017-06-20 | 广西壮族自治区梧州食品药品检验所 | A kind of method that ASE HPLC methods determine amentoflavone content in Selaginella tamariscina |
| CN109400566B (en) * | 2018-10-19 | 2021-06-08 | 中国药科大学 | Method for extracting and separating high-purity amentoflavone from Selaginella plant |
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| CN100451013C (en) * | 2004-04-21 | 2009-01-14 | 徐州技源天然保健品有限公司 | Producing technique for extracting extract products of amentoflavone |
| KR100623164B1 (en) * | 2004-07-22 | 2006-09-19 | 재단법인서울대학교산학협력재단 | A method for preparing purified extract for the prevention and treatment of stroke and ischemia from ginkgo biloba leaves extract and the composition containing the same |
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| CN107382939A (en) * | 2017-07-31 | 2017-11-24 | 天津市泰通农业科技有限公司 | The method of flavone compound in supercritical carbon dioxide extracting selaginella doederleinii |
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