CN109336943A - A kind of Bolbostemma paniculatum glucoside A purification process - Google Patents
A kind of Bolbostemma paniculatum glucoside A purification process Download PDFInfo
- Publication number
- CN109336943A CN109336943A CN201811275421.XA CN201811275421A CN109336943A CN 109336943 A CN109336943 A CN 109336943A CN 201811275421 A CN201811275421 A CN 201811275421A CN 109336943 A CN109336943 A CN 109336943A
- Authority
- CN
- China
- Prior art keywords
- methanol
- spare
- eluent
- purification process
- crystallization
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07J—STEROIDS
- C07J63/00—Steroids in which the cyclopenta(a)hydrophenanthrene skeleton has been modified by expansion of only one ring by one or two atoms
- C07J63/008—Expansion of ring D by one atom, e.g. D homo steroids
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
- C07H15/20—Carbocyclic rings
- C07H15/24—Condensed ring systems having three or more rings
- C07H15/256—Polyterpene radicals
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Saccharide Compounds (AREA)
Abstract
The invention discloses a kind of Bolbostemma paniculatum glucoside A purification process, and by rhizoma bolbostemmae root drying and crushing, refluxing extraction 3 times, combined extract, material residue is discarded；The resulting extracting solution of upper step is concentrated into no alcohol, macroreticular resin on extracting solution is eluted with the methanol of different alcoholic degrees respectively, collects the eluent of different alcoholic degrees, concentrate eluant, and with ethanol solution repeated crystallization；Compared with the prior art this technique, has the advantages that high income, purity are good, with short production cycle, technical process is simple, operation is safer and the Bolbostemma paniculatum glucoside A third of available high-purity.
Description
Technical field
The invention belongs to pharmaceutical technology field more particularly to a kind of Bolbostemma paniculatum glucoside A purification process.
Background technique
Domestic existing rhizoma bolbostemmae extraction process, main includes the big step of extracting and developing two of rhizoma bolbostemmae raw material.In the rhizoma bolbostemmae
The step of Bolbostemma paniculatum glucoside A extraction separation, is: now crushing rhizoma bolbostemmae raw material, is then extracted with water three times, extracting solution is concentrated into
Without alcohol, D101 macroreticular resin on concentrate is collected into the elution of different alcoholic degrees with the separating methanol Bolbostemma paniculatum glucoside A of different alcoholic degrees
The eluent of different alcoholic degrees is concentrated and does, methanol is added to dissolve by liquid, and ethyl acetate is added after dissolution and places crystallization, filtering for crystallizing is female
Liquid is concentrated into small size and places crystallization.
Complicated for operation with the methanol elution Fractional Collections of different alcoholic degrees in prior art, collection rate is low, is unfavorable for producing, and ties
Brilliant purity is low, and yield is low.
Summary of the invention
The present invention provides a kind of Bolbostemma paniculatum glucoside A purification process, it is intended to solve to be washed in prior art with the methanol of different alcoholic degrees
De- Fractional Collections are complicated for operation, and collection rate is low, is unfavorable for producing, and the purity of crystallization is low, the low problem of yield.
The present invention relates to a kind of Bolbostemma paniculatum glucoside A purification process, and steps are as follows:
(1) by rhizoma bolbostemmae material disintegrating, sieving is fitted into circumfluence distillation device, and pure water is added and is impregnated with raw material meal,
Refluxing extraction at a certain temperature, material residue discard, and extracting solution are collected filtrate after filter, filtrate is concentrated through tank is concentrated under reduced pressure
Afterwards, it is cooled to room temperature spare；
(2) macroreticular resin is fitted into spare in chromatographic column, macroreticular resin is activated with methanol, is washed to no alcohol with pure,
Extracting solution spare in step (1) is added on macroreticular resin pillar, is added by the 1% of adsorbance.First step pure water
Elution, eluent discards, second step with 35% methanol elution, eluent concentration and recovery methanol, third step with 60% methanol
Eluent is collected in elution, and it is spare that the eluent that third step is collected by the 4th step is concentrated under reduced pressure into no alcohol；
(3) step (2) is concentrated into non-alcoholic spare eluent to rejoin in new macroporous resin column, by adsorbance
1.5% be added.The first step is discarded with pure water elution, eluent, and second step is eluted with 35% methanol, and eluent decompression is dense
It retracts and receives methanol, third step is eluted with 95% methanol, collects eluent, and the eluent that third step is collected by the 4th step depressurizes
It is spare to be concentrated to dryness thick paste；
(4) ethyl acetate that 2 times of thick paste amounts are added in thick paste spare in step (3) stirred clockwise, be placed on 20 DEG C
At a temperature of, crystallization, filtering for crystallizing is dried for standby, and filtrated stock is concentrated into thick paste and places in the ethyl acetate that 2 times of thick paste amounts are added
At a temperature of 20 DEG C, secondary crystallization, filtering for crystallizing is dried for standby；
(5) by 50% methanol dissolution of crystal crude product twice in step (4), anhydrous second is added after the solid is completely dissolved
Alcohol places 72h crystallization, and filtering for crystallizing is spare, and mother liquor concentrations dehydrated alcohol places 72h crystallization, and filtering for crystallizing is spare；
(6) by crystal crude product was filtered while hot with dehydrated alcohol heating for dissolving 30 minutes, and crystallized twice in step (5)
The dry rhizoma bolbostemmae glycosides third for obtaining high-purity is concentrated in finished product, filtrated stock.
Preferably, 6 mesh sieve are used in step (1) in sifting step.
Preferably, reflux temperature is 97 DEG C in step (1), and reflow's cycle is that 3 each return times are 1.5 hours.
Preferably, step (2) macroreticular resin selects D101 macroreticular resin, and chromatography column size is 300 millimeters of internal diameter, length 2000
Millimeter.
Preferably, pure water and be 3 times of chromatographic column cylinder product with the dosage of 35% methanol in step (2), 60%
The dosage of methanol is 3 times of chromatographic column cylinder product.
Preferably, pure water and be 3 times of chromatographic column cylinder product with the dosage of 35% methanol in step (3), 95%
The dosage of methanol is 2 times of chromatographic column cylinder product.
Preferably, the dosage of ethyl acetate is spare 2 times of thick paste in step (4), the mixing time 30 minutes, temperature
Degree is 20 DEG C, and crystallization time is 48 hours.
Compared with prior art, the beneficial effects of the present invention are: a kind of Bolbostemma paniculatum glucoside A purification process of the invention, has
High income, purity are good, with short production cycle, technical process is simple, operation is safer and the rhizoma bolbostemmae of available high-purity
The advantages of glycosides first third.
Specific embodiment
Embodiment 1
A kind of Bolbostemma paniculatum glucoside A purification process,
(1) by rhizoma bolbostemmae material disintegrating, sieving is fitted into circumfluence distillation device, and pure water is added and is impregnated with raw material meal,
Refluxing extraction at a certain temperature, material residue discard, and extracting solution is collected filtrate, the pressurized concentration tank concentration of filtrate after filter
Afterwards, it is cooled to room temperature spare；
(2) macroreticular resin is fitted into spare in chromatographic column, macroreticular resin is activated with methanol, is washed to no alcohol with pure,
Extracting solution spare in step (1) is added on macroreticular resin pillar, the first step is discarded with pure water elution, eluent, the
Two steps are eluted with 35% methanol, eluent concentration and recovery methanol, and third step is eluted with 60% methanol, collect eluent, the
It is spare that the eluent that third step is collected by four steps is concentrated under reduced pressure into no alcohol；
(3) step (2) is concentrated into non-alcoholic spare eluent to rejoin in new macroporous resin column, the first step is used
Pure water elution, eluent discard, and second step is eluted with 35% methanol, and recycling methanol is concentrated under reduced pressure in eluent, and third step is used
95% methanol elution, collects eluent, it is spare that the eluent that third step is collected by the 4th step is concentrated to dryness thick paste；
(4) by spare thick paste in step (3) be added ethyl acetate stir clockwise, place at a certain temperature, crystallize,
Filtering for crystallizing is dried for standby, filtrated stock be concentrated into thick paste be added ethyl acetate place at a certain temperature, crystallization, filtering knot
Crystalline substance is dried for standby；
(5) by 50% methanol dissolution of crystal crude product twice in step (4), anhydrous second is added after the solid is completely dissolved
Alcohol places 72h crystallization, and filtering for crystallizing is spare, and mother liquor concentrations dehydrated alcohol places 72h crystallization, and filtering for crystallizing is spare；
(6) it by crystal crude product is dissolved with 1 dehydrated alcohol repeatedly twice in step (5), filters while hot, obtains crystal product,
The dry rhizoma bolbostemmae glycosides third for obtaining high-purity is concentrated in filtrated stock.
6 mesh sieve are used in step (1) in sifting step.
Reflux temperature is 97 DEG C in step (1), and reflow's cycle is that 3 each return times are 1.5 hours.
The optional D101 macroreticular resin of step (2) macroreticular resin, chromatography column size are 300 millimeters of internal diameter, 2000 millimeters of length.
In step (2) pure water and with the dosage of 35% methanol be chromatographic column cylinder product 3 times.
In step (3) pure water and with the dosage of 35% methanol be chromatographic column cylinder product 3 times.
The dosage of ethyl acetate is spare 2 times of thick paste in step (4), and the mixing time 30 minutes, temperature is 20 DEG C,
Crystallization time is 48 hours.
Embodiment 2
A kind of Bolbostemma paniculatum glucoside A purification process,
1, rhizoma bolbostemmae raw material 50kg crushed 6 mesh sieve, and the pure water for being fitted into addition 250L in circumfluence distillation device will be former
Material coarse powder is impregnated with, and refluxing extraction 3 times 1.5 hours every time at a temperature of 97 DEG C, material residue discards, and obtains 750L extracting solution, will extract
Liquid collects filtrate after filter, and the pressurized concentration tank of filtrate is concentrated into 300L, is cooled to room temperature spare.
2, it is standby the preliminary purification of Bolbostemma paniculatum glucoside A: to prepare 100kgD101 macroreticular resin, 300 millimeters of * 2000 millimeters of chromatographic columns
With macroreticular resin being fitted into spare in chromatographic column, resin is activated with methanol, no alcohol is washed to pure, by the extract of 1000L
On on ready D101 macroreticular resin pillar, the first step pure water elution of 450L, eluent discards, and second step is used
35% methanol elutes 450L-500L, eluent concentration and recovery methanol, and third step elutes 450L with 60% methanol, and collection is washed
De- liquid, it is spare that the 4th eluent for being collected into third step is concentrated under reduced pressure into no alcohol.
3, rhizoma bolbostemmae elution fluid dewatering and secondarily purified: a non-alcoholic eluent upper D101 again is concentrated by above-mentioned
Macroporous resin column, the first step pure water elution of 450L, eluent discard, and second step elutes 450L-500L with 35% methanol,
Recycling methanol is concentrated under reduced pressure in eluent, and 95% methanol of third step elutes 300L, and collection eluent, the 4th by third step
It is spare that the eluent being collected into is concentrated to dryness thick paste about 20L.
4, the purifying three times of Bolbostemma paniculatum glucoside A: thick paste obtained above about 20L addition 40L ethyl acetate is stirred clockwise
30min places 20 DEG C of crystallization 48h.Filtering for crystallizing is dried for standby, and obtains 30% or so Bolbostemma paniculatum glucoside A 1.35kg of coarse crystallization content
Left and right.Filtrated stock is concentrated into thick paste and places 20 DEG C of crystallization 48h secondary crystallizations in addition 40L ethyl acetate, and filtering for crystallizing obtains
To 30% or so Bolbostemma paniculatum glucoside A 700g of content or so, filtrated stock concentration is dry, contains Bolbostemma paniculatum glucoside A 12% or so.
5, four purifying of Bolbostemma paniculatum glucoside A: by above-mentioned Bolbostemma paniculatum glucoside A, crystal crude product is molten with the methanol of 20L50% twice
50L-60L dehydrated alcohol is added after the solid is completely dissolved and places 72h crystallization for solution, and filtering for crystallizing obtains 75% Bolbostemma paniculatum glucoside A
410g or so, mother liquor concentrations to 5L or so are added 25L dehydrated alcohol and place 72h crystallization, and filtering for crystallizing obtains 75% rhizoma bolbostemmae glycosides
First 160g or so, filtrated stock concentration are dry.
6, four times of Bolbostemma paniculatum glucoside A purifying: by above-mentioned Bolbostemma paniculatum glucoside A crystal crude product 18000L dehydrated alcohol 60 twice
DEG C dissolve 1h repeatedly, filter while hot, the rhizoma bolbostemmae to crystallization 95% crystallize 450g, yield 95%.Filtrated stock concentration is done
To the rhizoma bolbostemmae glycosides third of high-purity.
Embodiment 3
1, rhizoma bolbostemmae raw material 50kg crushed 6 mesh sieve, and the pure water for being fitted into addition 250L in circumfluence distillation device will be former
Material coarse powder is impregnated with, and refluxing extraction 3 times 1.5 hours every time at a temperature of 97 DEG C, material residue discards, and obtains 750L extracting solution, will extract
Liquid collects filtrate after filter, and the pressurized concentration tank of filtrate is concentrated into 300L, is cooled to room temperature spare.
2, it is standby the preliminary purification of Bolbostemma paniculatum glucoside A: to prepare 100kgAB-8 macroreticular resin, 300 millimeters of * 2000 millimeters of chromatographic columns
With macroreticular resin being fitted into spare in chromatographic column, resin is activated with methanol, no alcohol is washed to pure, by the extract of 1000L
On on ready AB-8 macroreticular resin pillar, the first step pure water elution of 450L, eluent discards, and second step is used
35% methanol elutes 450L-500L, eluent concentration and recovery methanol, and third step elutes 450L with 60% methanol, and collection is washed
De- liquid, it is spare that the 4th eluent for being collected into third step is concentrated under reduced pressure into no alcohol.
3, rhizoma bolbostemmae elution fluid dewatering and secondarily purified: a non-alcoholic eluent upper AB-8 again is concentrated by above-mentioned
Macroporous resin column, the first step pure water elution of 450L, eluent discard, and second step elutes 450L-500L with 35% methanol,
Recycling methanol is concentrated under reduced pressure in eluent, and 95% methanol of third step elutes 300L, and collection eluent, the 4th by third step
It is spare that the eluent being collected into is concentrated to dryness thick paste about 20L.
4, the purifying three times of Bolbostemma paniculatum glucoside A: thick paste obtained above about 20L addition 40L ethyl acetate is stirred clockwise
30min places 20 DEG C of crystallization 48h.Filtering for crystallizing is dried for standby, and obtains 30% or so Bolbostemma paniculatum glucoside A 1.35kg of coarse crystallization content
Left and right.Filtrated stock is concentrated into thick paste and places 20 DEG C of crystallization 48h secondary crystallizations in addition 40L ethyl acetate, and filtering for crystallizing obtains
To 30% or so Bolbostemma paniculatum glucoside A 700g of content or so, filtrated stock concentration is dry, contains Bolbostemma paniculatum glucoside A 12% or so.
5, four purifying of Bolbostemma paniculatum glucoside A: by above-mentioned Bolbostemma paniculatum glucoside A, crystal crude product is molten with the methanol of 20L50% twice
50L-60L dehydrated alcohol is added after the solid is completely dissolved and places 72h crystallization for solution, and filtering for crystallizing obtains 75% Bolbostemma paniculatum glucoside A
410g or so, mother liquor concentrations to 5L or so are added 25L dehydrated alcohol and place 72h crystallization, and filtering for crystallizing obtains 75% rhizoma bolbostemmae glycosides
First 160g or so, filtrated stock concentration are dry.
6, four times of Bolbostemma paniculatum glucoside A purifying: by above-mentioned Bolbostemma paniculatum glucoside A crystal crude product 18000L dehydrated alcohol 60 twice
DEG C dissolve 1h repeatedly, filter while hot, the rhizoma bolbostemmae to crystallization 95% crystallize 450g, yield 85%.Filtrated stock concentration is done
To the rhizoma bolbostemmae glycosides third of high-purity.
Embodiment 4
1, rhizoma bolbostemmae raw material 50kg crushed 6 mesh sieve, and the pure water for being fitted into addition 250L in circumfluence distillation device will be former
Material coarse powder is impregnated with, and refluxing extraction 3 times 1.5 hours every time at a temperature of 97 DEG C, material residue discards, and obtains 750L extracting solution, will extract
Liquid collects filtrate after filter, and the pressurized concentration tank of filtrate is concentrated into 300L, is cooled to room temperature spare.
2, it is standby the preliminary purification of Bolbostemma paniculatum glucoside A: to prepare 100kgD301 macroreticular resin, 300 millimeters of * 2000 millimeters of chromatographic columns
With macroreticular resin being fitted into spare in chromatographic column, resin is activated with methanol, no alcohol is washed to pure, by the extract of 1000L
On on ready D301 macroreticular resin pillar, the first step pure water elution of 450L, eluent discards, and second step is used
35% methanol elutes 450L-500L, eluent concentration and recovery methanol, and third step elutes 450L with 60% methanol, and collection is washed
De- liquid, it is spare that the 4th eluent for being collected into third step is concentrated under reduced pressure into no alcohol.
3, rhizoma bolbostemmae elution fluid dewatering and secondarily purified: a non-alcoholic eluent upper D301 again is concentrated by above-mentioned
Macroporous resin column, the first step pure water elution of 450L, eluent discard, and second step elutes 450L-500L with 35% methanol,
Recycling methanol is concentrated under reduced pressure in eluent, and 95% methanol of third step elutes 300L, and collection eluent, the 4th by third step
It is spare that the eluent being collected into is concentrated to dryness thick paste about 20L.
4, the purifying three times of Bolbostemma paniculatum glucoside A: thick paste obtained above about 20L addition 40L ethyl acetate is stirred clockwise
30min places 20 DEG C of crystallization 48h.Filtering for crystallizing is dried for standby, and obtains 30% or so Bolbostemma paniculatum glucoside A 1.35kg of coarse crystallization content
Left and right.Filtrated stock is concentrated into thick paste and places 20 DEG C of crystallization 48h secondary crystallizations in addition 40L ethyl acetate, and filtering for crystallizing obtains
To 30% or so Bolbostemma paniculatum glucoside A 700g of content or so, filtrated stock concentration is dry, contains Bolbostemma paniculatum glucoside A 12% or so.
5, four purifying of Bolbostemma paniculatum glucoside A: by above-mentioned Bolbostemma paniculatum glucoside A, crystal crude product is molten with the methanol of 20L50% twice
50L-60L dehydrated alcohol is added after the solid is completely dissolved and places 72h crystallization for solution, and filtering for crystallizing obtains 75% Bolbostemma paniculatum glucoside A
410g or so, mother liquor concentrations to 5L or so are added 25L dehydrated alcohol and place 72h crystallization, and filtering for crystallizing obtains 75% rhizoma bolbostemmae glycosides
First 160g or so, filtrated stock concentration are dry.
6, four times of Bolbostemma paniculatum glucoside A purifying: by above-mentioned Bolbostemma paniculatum glucoside A crystal crude product 18000L dehydrated alcohol 60 twice
DEG C dissolve 1h repeatedly, filter while hot, the rhizoma bolbostemmae to crystallization 95% crystallize 450g, yield 80%.Filtrated stock concentration is done
To the rhizoma bolbostemmae glycosides third of high-purity.
Through the foregoing embodiment, can finally obtain using D101 macroreticular resin is selected is most suitable, purifying as separation resin
Effect is most obvious.
Claims (7)
1. a kind of Bolbostemma paniculatum glucoside A purification process, which is characterized in that
(1) by rhizoma bolbostemmae material disintegrating, sieving is fitted into circumfluence distillation device, and pure water is added and is impregnated with raw material meal, one
Determine refluxing extraction at temperature, material residue discards, extracting solution is collected into filtrate after filter, after the pressurized concentration tank concentration of filtrate,
It is cooled to room temperature spare；
(2) macroreticular resin is fitted into spare in chromatographic column, macroreticular resin is activated with methanol, no alcohol is washed to pure, will walk
Suddenly extracting solution spare in (1) is added on macroreticular resin pillar, and the first step is discarded with pure water elution, eluent, second step
It is eluted with 35% methanol, eluent concentration and recovery methanol, third step is eluted with 60% methanol, collects eluent, the 4th step
It is spare that the eluent that third step is collected into is concentrated under reduced pressure into no alcohol；
(3) step (2) is concentrated into non-alcoholic spare eluent to rejoin in new macroporous resin column, the first step is with pure
Water elution, eluent discard, and second step is eluted with 35% methanol, and recycling methanol is concentrated under reduced pressure in eluent, and third step is with 95%
Methanol elution, collect eluent, it is spare that the eluent that third step is collected by the 4th step is concentrated to dryness thick paste；
(4) by spare thick paste in step (3) be added ethyl acetate stir clockwise, places at a certain temperature, crystallize, filter
Crystallization is dried for standby, filtrated stock be concentrated into thick paste be added ethyl acetate place at a certain temperature, crystallization, filtering for crystallizing dry
It does spare；
(5) by 50% methanol dissolution of crystal crude product twice in step (4), dehydrated alcohol is added after the solid is completely dissolved and puts
72h crystallization is set, filtering for crystallizing is spare, and mother liquor concentrations dehydrated alcohol places 72h crystallization, and filtering for crystallizing is spare；
(6) it by crystal crude product is dissolved with dehydrated alcohol repeatedly twice in step (5), filters while hot, obtains crystal product, filtering is female
The dry rhizoma bolbostemmae glycosides third for obtaining high-purity is concentrated in liquid.
2. a kind of Bolbostemma paniculatum glucoside A purification process according to claim 1, which is characterized in that adopted in sifting step in step (1)
With 6 mesh sieve.
3. a kind of Bolbostemma paniculatum glucoside A purification process according to claim 1, which is characterized in that reflux temperature in step (1)
It is 97 DEG C, reflow's cycle is that 3 each return times are 1.5 hours.
4. a kind of Bolbostemma paniculatum glucoside A purification process according to claim 1, which is characterized in that step (2) macroreticular resin is excellent
Selecting D101 macroreticular resin chromatography column size is internal diameter 300Millimeter, 2000 millimeters of length.
5. a kind of Bolbostemma paniculatum glucoside A purification process according to claim 1, which is characterized in that pure in the step (2)
Water and with the dosage of 35% methanol be chromatographic column cylinder product 3 times.The dosage of 60% methanol is the 3 of chromatographic column cylinder product Times.
6. a kind of Bolbostemma paniculatum glucoside A purification process according to claim 1, which is characterized in that pure in the step (3)
Water and with the dosage of 35% methanol be chromatographic column cylinder product 3 times.The dosage of 95% methanol is the 2 of chromatographic column cylinder product Times.
7. a kind of Bolbostemma paniculatum glucoside A purification process according to claim 1, which is characterized in that acetic acid in the step (4)
The dosage of ethyl ester is spare 2 times of thick paste, the mixing time 30 minutes, and temperature is 20 degrees Celsius, and crystallization time is 48 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811275421.XA CN109336943A (en) | 2018-10-26 | 2018-10-26 | A kind of Bolbostemma paniculatum glucoside A purification process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811275421.XA CN109336943A (en) | 2018-10-26 | 2018-10-26 | A kind of Bolbostemma paniculatum glucoside A purification process |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109336943A true CN109336943A (en) | 2019-02-15 |
Family
ID=65311001
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811275421.XA Pending CN109336943A (en) | 2018-10-26 | 2018-10-26 | A kind of Bolbostemma paniculatum glucoside A purification process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109336943A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113912664A (en) * | 2021-11-12 | 2022-01-11 | 浙江大学 | Preparation method and application of tubeimoside A |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1093272A (en) * | 1993-04-07 | 1994-10-12 | 山东新华制药厂 | The preparation method of tubeimoside first element |
| CN102180934A (en) * | 2011-01-24 | 2011-09-14 | 南京泽朗医药科技有限公司 | Preparation method of tubeimoside I |
| CN102603853A (en) * | 2011-01-25 | 2012-07-25 | 苏州宝泽堂医药科技有限公司 | Efficient separation and purification method of tubeimoside |
| CN106420433A (en) * | 2015-08-08 | 2017-02-22 | 于立坚 | Uses of new cosmetic raw material bolbostemma paniculatum total saponin in elimination of bromhidrosis odor |
-
2018
- 2018-10-26 CN CN201811275421.XA patent/CN109336943A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1093272A (en) * | 1993-04-07 | 1994-10-12 | 山东新华制药厂 | The preparation method of tubeimoside first element |
| CN102180934A (en) * | 2011-01-24 | 2011-09-14 | 南京泽朗医药科技有限公司 | Preparation method of tubeimoside I |
| CN102603853A (en) * | 2011-01-25 | 2012-07-25 | 苏州宝泽堂医药科技有限公司 | Efficient separation and purification method of tubeimoside |
| CN106420433A (en) * | 2015-08-08 | 2017-02-22 | 于立坚 | Uses of new cosmetic raw material bolbostemma paniculatum total saponin in elimination of bromhidrosis odor |
Non-Patent Citations (2)
| Title |
|---|
| RYOJI KASAI等: "TUBEIMOSIDE I, A NEW CYCLIC BISDESMOSIDE FROM CHINESE CUCURBITACEOUS FOLK MEDICINE "TU BEI MU"", 《CHEM.PHARM.BULL.》 * |
| 马挺军: "土贝母化学成分及抗肿瘤活性研究", 《中国博士学位论文全文数据库 医药卫生科技辑》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113912664A (en) * | 2021-11-12 | 2022-01-11 | 浙江大学 | Preparation method and application of tubeimoside A |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104086425B (en) | A kind of method simultaneously extracting also separate tobacco chlorogenic acid, Salanesol, alkaloid, violaguercitrin | |
| CN108752231B (en) | Method for extracting theanine from sweet tea and simultaneously extracting rubusoside and tea polyphenol | |
| CN104177370B (en) | A kind of method preparing high-load sesamin from sesame seed meal | |
| CN101787060A (en) | Method for extracting and separating stilbene glucoside from polygonum multiflorum | |
| CN101143887B (en) | Method for separating and preparing corosolicacid in loquat leaf | |
| CN101407535A (en) | Preparation of high-purity Momordica grosvenori mogroside V | |
| CN112266399B (en) | High-purity separation and extraction method of epimedium extract | |
| CN106589020A (en) | Method for extracting icariin from epimedium | |
| CN109336943A (en) | A kind of Bolbostemma paniculatum glucoside A purification process | |
| CN103450000B (en) | Method for extracting hypericin from hyperforin perforatum | |
| CN111018940A (en) | Method for extracting oil saponin from oil-tea camellia cakes | |
| CN110922413A (en) | Extraction and separation method of glabridin | |
| CN108586440A (en) | The purification process of Puerarin | |
| CN102199159A (en) | Method for separating and purifying ginkgolide C in ginkgo root bark | |
| CN101955503A (en) | Preparation method of oleuropein | |
| CN112939761B (en) | Method for extracting nervonic acid | |
| CN102372606A (en) | Method for extracting kirenol from glandularstalk st.paulswort herb | |
| CN107235988A (en) | A kind of extracting method of qinghaosu and Artemisitene | |
| CN106905339A (en) | A kind of method that capsule of weeping forsythia aglycon is purified from Folium Forsythia | |
| CN109970838B (en) | Preparation method of pedunculoside | |
| CN105085587A (en) | Extraction and purification process method for forsythiaside A in fructus forsythiae leaves | |
| CN106336390A (en) | Method for extracting flavone from banana leaves | |
| CN109134562A (en) | A kind of aesculin purification process | |
| CN107602642B (en) | Method for extracting and purifying trachelospermin from safflower seed | |
| CN102675142B (en) | Method for purifying capsicine in hot pepper |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20190215 |