CN107286211A - A kind of preparation method of morroniside - Google Patents
A kind of preparation method of morroniside Download PDFInfo
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- CN107286211A CN107286211A CN201710094742.9A CN201710094742A CN107286211A CN 107286211 A CN107286211 A CN 107286211A CN 201710094742 A CN201710094742 A CN 201710094742A CN 107286211 A CN107286211 A CN 107286211A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
- C07H17/04—Heterocyclic radicals containing only oxygen as ring hetero atoms
-
- 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
Abstract
The present invention discloses a kind of preparation method of morroniside, processing step adds ethanol including raw material, extracted by microwave, ultrasonic synergistic, extract solution reclaims ethanol, is adsorbed by polar macroporous resin, then water alcohol gradient elution, film purifying concentration is carried out using filtering again, then concentrate is extracted with water-saturated n-butanol, is finally crystallized again by ethyl acetate dichloromethane mixed solution, product is can obtain by being dried under reduced pressure.The present invention is using microwave, ultrasonic synergistic extraction method, and extraction rate is fast, and impurity dissolution is few, and energy consumption is low, has the advantages that efficiently without industrial pollution.Macroreticular resin and filter membrane are used in combination, and good impurity removing effect, energy consumption are low, with single use filter membrane be separated by filtration comparing, extend the service life of filter membrane.This invention simplifies technological process, it is more convenient in operation, products obtained therefrom content is high, this method is adapted to amplification production, cost is low, and energy consumption is small.
Description
Technical field
The present invention relates to raw material medicine preparation field, specifically a kind of preparation method of morroniside.
Background technology
Morroniside molecular formula：C17H26011.Molecular weight：402.38.Molecular structure：
Compositional classification：Iridoid glycosides.Physical property：The larger solvent of ethanol, water isopolarity is dissolved in, in certain bar
Facile hydrolysis under part.Pharmacological action：Research shows that the iridoid glycoside in Fructus Corni can improve diabetic vascular complications, can use
In the exploitation for the treatment of diabetes medicament.Morroniside has protection cell from the H202 cytotoxicities induced and the work of Apoptosis
With, therefore a kind of neuroprotection class medicine can be used as.Morroniside also has effects that bitter benefit stomach invigorating.Fructus Corni is planted for Cornaceae
The drying and ripening pulp of thing Fructus Corni.Its slightly warm in nature, it is sour, puckery, return liver and kidney channel, with tonifying the liver and kidney, the work(of arresting collape syndrome by astringents
Effect.For dizziness and tinnitus, soreness of waist and knee joint, impotence and seminal emission, enuresis frequent micturition, under uterine bleeding band, profuse sweating collapse, Heat Diabetes.Modern times grind
Study carefully the main active component for showing that iridoid is Fructus Corni.Morroniside particularly therein has improvement diabetic vascular concurrent
The pharmacological actions such as disease, anti-oxidant, anti-apoptotic, increase neurotrophy, promotion nerve growth, to cerebral apoplexy, cerebral ischemia, Reperfu- sion
There are the brain major disease such as damage, dementia, Parkinson's significant treatment and prevention to act on.Morroniside also has prevention and treated
Acute and chronic liver injury and the effect of liver fibrosis.Morroniside is a kind of small molecule, the iridoid of big polarity, chemistry
Property less stable, extracts separating difficulty greatly, and separation morroniside is extracted at present to be prepared on a small scale in laboratory, and technique is multiple
Miscellaneous, cost is high.Therefore, Monot's glycoside extraction separation technique of the industrialized production value of developing low-cost has realistic meaning.
The Chinese patent of Application No. 201510438773.2 discloses a kind of method for preparing morroniside, the invention, including
Following steps：Fructus Corni is subjected to seepage pressure effects, Fructus Corni extract solution is obtained；By the concentration of obtained Fructus Corni extract solution, obtain
Fructus Corni medicinal extract；Obtain the Fructus Corni medicinal extract, with silica gel mix, it is dry, finely ground after, be loaded in chromatographic column；The chromatogram
Column chromatography blank silica gel is had been loaded with post；The chromatographic column is eluted with eluent and flow point is collected, then is removed described
Eluent in the flow point being collected into, uses methanol dissolution residual substance, recrystallization, obtains the morroniside.Such a method is to mountain Zhu
The extraction efficiency of cornel obtains morroniside content relatively low than relatively low.
The Chinese patent of Application No. 200510041480 discloses a kind of cornel extractive and its preparation technology, the invention
Middle Fructus Corni is extracted with ethanol, extract solution concentration after stand at low temperature, upper strata solid handled with soda acid after extract
A, the subnatant isolated extract B of macroporous resin column, the cornel extractive that extract A and B are mixed, such a method
Extraction efficiency to Fructus Corni is equally very low, product content also than relatively low.
The content of the invention
It is an object of the invention to provide a kind of preparation method of morroniside, with asking for solving to propose in above-mentioned background technology
Topic.
To achieve the above object, the present invention provides following technical scheme：
A kind of preparation method of morroniside, it is characterised in that including following steps：
(1) raw material add ethanol to be extracted using microwave, ultrasonic synergistic extraction method：Fructus Corni raw material is crushed plus 5-
10 times of amount ethanol, are extracted 40-60 minutes by microwave, Ultrasound-assisted, extracted 2-3 times；
(2) macroporous resin adsorption extract solution is used：The ethanol in extract solution is reclaimed, macroporous resin column is added after filtering and is carried out
Absorption, then using water-alcohol gradient elution, finally collects morroniside flow point；
(3) morroniside flow point carries out filter operation by filter membrane：Morroniside flow point is added into milipore filter and carries out ultrafiltration, is surpassed
NF membrane is added after the completion of filter to be filtered, and then collects concentrate；
(4) extraction behaviour and crystallization operation are carried out to the concentrate being collected into：Water-saturated n-butanol is added to extract above-mentioned concentrate
Take 2-4 times, then merge extract, then be concentrated under reduced pressure, concentrated extract is can obtain after concentration, concentrated extract is dissolved in second
Acetoacetic ester removes insoluble matter and water layer, adds anhydrous sodium sulfate and reclaims ethyl acetate, solution adds dichloro after filtering
Methane, then it can be seen that there is white precipitate precipitation, finally places crystallization, repeats crystallization 3-4 times, taking can obtain after being dried under reduced pressure
To Monot's glycoside product.
1. middle concentration of alcohol is 20-60% to step.
1. middle supersonic frequency is 20-80kHz to step, and power is 1000-3000W.
1. middle microwave frequency is 2500kHz, power 10kW to step.
2. middle macroreticular resin can be chosen step from HPD850, S-8, NAK-II, LAS-7, ADS-17.
2. middle water-alcohol gradient elution is 6-10BV water -4-6BV10-30% ethanol solution -6-9BV50-80% ethanol to step
Solution.
Step 3. middle filter membrane species and filter condition：Milipore filter is molecular cut off 3000-7000 hollow composite membrane,
NF membrane is the hollow composite membrane of molecular cut off 150.Filter pressure 0.2-0.7MPa.
Compared with prior art, the beneficial effects of the invention are as follows：The present invention uses microwave ultrasound ultrasonic synergistic extraction method,
Microwave is a kind of non-ionized electromagnetic radiation, the polar molecule of irradiated material fast steering and orientation row in microwave electromagnetic field
Row, the method that selective extraction is carried out to target component in material using microwave plus thermal property, by adjusting the parameter of microwave,
Target component can be effectively heated, the judder produced in favor of the extraction of target component with separating using ultrasonic wave and cavitation
Effect accelerates the release of material in plant cell, spreads and dissolve into solvent, while the knot of material can be kept being extracted
Structure and bioactivity do not change, and extraction rate is fast, and impurity dissolution is few, and energy consumption is low, with excellent efficiently without industrial pollution etc.
Point.Macroreticular resin and filter membrane are used in combination, and good impurity removing effect, energy consumption are low, and single use filter membrane carries out being separated by filtration phase
Than extending the service life of filter membrane, simplification of flowsheet is more convenient in operation, products obtained therefrom content is high, and this method is adapted to
Amplification production, cost is low, and energy consumption is small.
Embodiment
The present invention is further illustrated below in conjunction with embodiment, the technical scheme in inventive embodiments is carried out clear
Chu, it is fully described by, but the scope of protection of present invention is not limited to following embodiments, it is clear that described implementation
Example only a part of embodiment of the invention, rather than whole embodiments.Based on the embodiment in the present invention, this area is common
The every other embodiment that technical staff is obtained under the premise of creative work is not made, belongs to the model that the present invention is protected
Enclose.
A kind of preparation method of morroniside, it is characterised in that including following steps：
(1) raw material add ethanol to be extracted using microwave, ultrasonic synergistic extraction method：Fructus Corni raw material is crushed plus 5-
10 times of amount ethanol, are extracted 40-60 minutes by microwave, Ultrasound-assisted, extracted 2-3 times；
(2) macroporous resin adsorption extract solution is used：The ethanol in extract solution is reclaimed, macroporous resin column is added after filtering and is carried out
Absorption, then using water-alcohol gradient elution, finally collects morroniside flow point；
(3) morroniside flow point carries out filter operation by filter membrane：Morroniside flow point is added into milipore filter and carries out ultrafiltration, is surpassed
NF membrane is added after the completion of filter to be filtered, and then collects concentrate；
(4) extraction behaviour and crystallization operation are carried out to the concentrate being collected into：Water-saturated n-butanol is added to extract above-mentioned concentrate
Take 2-4 times, then merge extract, then be concentrated under reduced pressure, concentrated extract is can obtain after concentration, concentrated extract is dissolved in second
Acetoacetic ester removes insoluble matter and water layer, adds anhydrous sodium sulfate and reclaims ethyl acetate, solution adds dichloro after filtering
Methane, then it can be seen that there is white precipitate precipitation, finally places crystallization, repeats crystallization 3-4 times, taking can obtain after being dried under reduced pressure
To Monot's glycoside product.
1. middle concentration of alcohol is 20-60% to step.
1. middle supersonic frequency is 20-80kHz to step, and power is 1000-3000W.
1. middle microwave frequency is 2500kHz, power 10kW to step.
2. middle macroreticular resin can be chosen step from HPD850, S-8, NAK-II, LAS-7, ADS-17.
2. middle water-alcohol gradient elution is 6-10BV water -4-6BV10-30% ethanol solution -6-9BV50-80% ethanol to step
Solution.
Step 3. middle filter membrane species and filter condition：Milipore filter is molecular cut off 3000-7000 hollow composite membrane,
NF membrane is the hollow composite membrane of molecular cut off 150.Filter pressure 0.2-0.7MPa.
Embodiment 1：Fructus Corni raw material is crushed using disintegrating apparatus, takes the Fructus Corni after 5kg crushing to put into microwave, surpass
In sound wave synergic extractor, 15L40% ethanol is added, the frequency of ultrasonic transmitter 80kHz is adjusted to, power is adjusted to 10kW,
The frequency of microwave emitter is 2500kHz, and power is 10kW, then carries out microwave, ultrasonic synergistic and extracts, 30 points are extracted every time
Clock, is extracted 2 times, all extract solutions is merged, and reclaims the ethanol in extract solution, and extract solution is added into 2LHPD850 macropores
Resin column is adsorbed, and flow control is in 3L/h, and absorption uses 20L water -15L10% ethanol solution -18L60% second successively after terminating
Alcoholic solution is eluted, and collects 60% ethanol eluate, and the filter membrane for adding molecular cut off 3000-7000 carries out ultrafiltration, will
Inlet pressure is controlled in 0.2-0.7MPa, and the NF membrane that filtered fluid adds molecular cut off 150 is concentrated, and concentrate is transferred to
Extractor, the water-saturated n-butanol for adding 3BV is extracted 4 times, and extract is concentrated, n-butanol is then reclaimed, you can is concentrated
Medicinal extract.Concentrated extract adds 10BV ethyl acetate dissolving, removes water layer, filters insoluble matter, and filtrate adds anhydrous sodium sulfate and returned
Ethyl acetate is received, dichloromethane will be added in filtrate, then stirs evenly up to there is Precipitation, is subsequently placed with crystallization, crystal is again
Dichloromethane is added with ethyl acetate dissolving and repeats crystallization 3 times, and filtering is dried under reduced pressure to obtain Monot glycoside product 75g, content 97%.
Embodiment 2：Fructus Corni raw material is crushed using disintegrating apparatus, takes the Fructus Corni after 5kg crushing to put into microwave, surpass
In sound wave synergic extractor, 15L40% ethanol is added, the frequency of ultrasonic transmitter 60kHz is adjusted to, power is adjusted to 8kW, micro-
The frequency of wave launcher is 2500kHz, and power is 10kW, then carries out microwave, ultrasonic synergistic and extracts, 30 points are extracted every time
Clock, is extracted 3 times, all extract solutions is merged, and reclaims the ethanol in extract solution, and extract solution is added into 2LHPD850 macropores
Resin column is adsorbed, and flow control is in 3L/h, and absorption uses 20L water -15L10% ethanol solution -18L60% second successively after terminating
Alcoholic solution is eluted, and collects 60% ethanol eluate, and the filter membrane for adding molecular cut off 3000-7000 carries out ultrafiltration, will
Inlet pressure is controlled in 0.2-0.7MPa, and the NF membrane that filtered fluid adds molecular cut off 150 is concentrated, and concentrate is transferred to
Extractor, the water-saturated n-butanol for adding 3BV is extracted 4 times, and extract is concentrated, n-butanol is then reclaimed, you can is concentrated
Medicinal extract.Concentrated extract adds 10BV ethyl acetate dissolving, removes water layer, filters insoluble matter, and filtrate adds anhydrous sodium sulfate and returned
Ethyl acetate is received, dichloromethane will be added in filtrate, then stirs evenly up to there is Precipitation, is subsequently placed with crystallization, crystal is again
Dichloromethane is added with ethyl acetate dissolving and repeats crystallization 3 times, and filtering is dried under reduced pressure to obtain Monot glycoside product 71g, content 96%.
Embodiment 3：Fructus Corni raw material is crushed using disintegrating apparatus, takes the Fructus Corni after 5kg crushing to put into microwave, surpass
In sound wave synergic extractor, 30L50% ethanol is added, the frequency of ultrasonic transmitter 20kHz is adjusted to, power is adjusted to 1kW, micro-
The frequency of wave launcher is 2500kHz, and power is 10kW, then carries out microwave, ultrasonic synergistic and extracts, 60 points are extracted every time
Clock, is extracted 2 times, all extract solutions is merged, and reclaims the ethanol in extract solution, and extract solution is added into 3LS-8 macropore trees
Fat post is adsorbed, and flow control is in 2L/h, and absorption uses 22L water -9L15% ethanol solution -12L65% ethanol successively after terminating
Solution is eluted, and collects 65% ethanol eluate, and the filter membrane for adding molecular cut off 3000-7000 carries out ultrafiltration, will enter
Mouth Stress control is in 0.2-0.7MPa, and the NF membrane that filtered fluid adds molecular cut off 150 is concentrated, and concentrate is transferred to extraction
Tank is taken, the water-saturated n-butanol for adding 5BV is extracted 3 times, and extract is concentrated, n-butanol is then reclaimed, you can obtain concentration leaching
Cream.Concentrated extract adds 17BV ethyl acetate dissolving, removes water layer, filters insoluble matter, and filtrate adds anhydrous sodium sulfate and reclaimed
Ethyl acetate, will add dichloromethane in filtrate, then stir evenly up to there is Precipitation, be subsequently placed with crystallization, crystal is used again
Ethyl acetate dissolving adds dichloromethane and repeats crystallization 3 times, and filtering is dried under reduced pressure to obtain Monot glycoside product 68g, content 96%
Embodiment 4：Fructus Corni raw material is crushed using disintegrating apparatus, take 10kg crush after Fructus Corni put into microwave,
In ultrasonic synergistic extractor, 65L60% ethanol is added, the frequency of ultrasonic transmitter 80kHz is adjusted to, power is adjusted to 1kW,
The frequency of microwave emitter is 2500kHz, and power is 10kW, then carries out microwave, ultrasonic synergistic and extracts, 30 points are extracted every time
Clock, extracts 2 times, all extract solutions is merged, and reclaims the ethanol in extract solution, and it is big that extract solution is added into 2LLNAK-II
Hole resin column is adsorbed, and flow control is in 3L/h, and absorption uses 80L water -28L20% ethanol solutions -33L60% successively after terminating
Ethanol solution is eluted, and collects 60% ethanol eluate, and the filter membrane for adding molecular cut off 3000-7000 carries out ultrafiltration,
By inlet pressure control in 0.2-0.7MPa, the NF membrane that filtered fluid adds molecular cut off 150 is concentrated, and concentrate turns
Enter extractor, the water-saturated n-butanol for adding 7BV is extracted 4 times, and extract is concentrated, n-butanol is then reclaimed, you can obtains dense
Contracting medicinal extract.Concentrated extract adds 18BV ethyl acetate dissolving, removes water layer, filters insoluble matter, and filtrate adds anhydrous sodium sulfate
Ethyl acetate is reclaimed, dichloromethane will be added in filtrate, then stirs evenly up to there is Precipitation, is subsequently placed with crystallization, crystal
Dichloromethane being added with ethyl acetate dissolving again and repeating crystallization 3 times, filtering is dried under reduced pressure to obtain Monot glycoside product 142g, content 99%
Embodiment 5：Fructus Corni raw material is crushed using disintegrating apparatus, take 15kg crush after Fructus Corni put into microwave,
In ultrasonic synergistic extractor, 70L50% ethanol is added, the frequency of ultrasonic transmitter 70kHz is adjusted to, power is adjusted to 2kW,
The frequency of microwave emitter is 2500kHz, and power is 10kW, then carries out microwave, ultrasonic synergistic and extracts, 40 points are extracted every time
Clock, is extracted 3 times, all extract solutions is merged, and reclaims the ethanol in extract solution, and extract solution is added into 9LLAS-7 macropores
Resin column is adsorbed, and flow control is in 9L/h, and absorption uses 95L water -39L10% ethanol solution -55L70% second successively after terminating
Alcoholic solution is eluted, and collects 70% ethanol eluate, and the filter membrane for adding molecular cut off 3000-7000 carries out ultrafiltration, will
Inlet pressure is controlled in 0.2-0.7MPa, and the NF membrane that filtered fluid adds molecular cut off 150 is concentrated, and concentrate is transferred to
Extractor, the water-saturated n-butanol for adding 5BV is extracted 3 times, and extract is concentrated, n-butanol is then reclaimed, you can is concentrated
Medicinal extract.Concentrated extract adds 8BV ethyl acetate dissolving, removes water layer, filters insoluble matter, and filtrate adds anhydrous sodium sulfate and reclaimed
Ethyl acetate, will add dichloromethane in filtrate, then stir evenly up to there is Precipitation, be subsequently placed with crystallization, crystal is used again
Ethyl acetate dissolving adds dichloromethane and repeats crystallization 3 times, and filtering is dried under reduced pressure to obtain Monot glycoside product 196g, content 98%
Embodiment 6：Fructus Corni raw material is crushed using disintegrating apparatus, take 20kg crush after Fructus Corni put into microwave,
In ultrasonic synergistic extractor, 82L50% ethanol is added, the frequency of ultrasonic transmitter 80kHz is adjusted to, power is adjusted to 5kW,
The frequency of microwave emitter is 2500kHz, and power is 10kW, then carries out microwave, ultrasonic synergistic and extracts, 50 points are extracted every time
Clock, extracts 2 times, all extract solutions is merged, and reclaims the ethanol in extract solution, and it is big that extract solution is added into 12LLADS-17
Hole resin column is adsorbed, flow control in 20L/h, absorption terminate after successively with 125L water -46L10% ethanol solutions -
78L65% ethanol solutions are eluted, and collect 65% ethanol eluate, and the filter membrane for adding molecular cut off 3000-7000 enters
Row ultrafiltration, by inlet pressure control in 0.2-0.7MPa, the NF membrane that filtered fluid adds molecular cut off 150 is concentrated,
Concentrate is transferred to extractor, and the water-saturated n-butanol for adding 6BV is extracted 4 times, and extract is concentrated, n-butanol is then reclaimed, i.e.,
It can obtain concentrated extract.Concentrated extract adds 12BV ethyl acetate dissolving, removes water layer, filters insoluble matter, and filtrate adds nothing
Aqueous sodium persulfate reclaims ethyl acetate, dichloromethane will be added in filtrate, then stirs evenly up to there is Precipitation, is subsequently placed with knot
Crystalline substance, crystal adds dichloromethane with ethyl acetate dissolving again and repeats crystallization 3 times, and filtering is dried under reduced pressure to obtain Monot's glycoside product
273g, content 98%.
Embodiment 7：Fructus Corni raw material is crushed using disintegrating apparatus, take 25kg crush after Fructus Corni put into microwave,
In ultrasonic synergistic extractor, 95L40% ethanol is added, the frequency of ultrasonic transmitter 60kHz is adjusted to, power is adjusted to 4kW,
The frequency of microwave emitter is 2500kHz, and power is 10kW, then carries out microwave, ultrasonic synergistic and extracts, 35 points are extracted every time
Clock, extracts 3 times, all extract solutions is merged, and reclaims the ethanol in extract solution, and it is big that extract solution is added into 15LLNAK-II
Hole resin column is adsorbed, flow control in 22L/h, absorption terminate after successively with 150L water -52L10% ethanol solutions -
112L50% ethanol solutions are eluted, and collect 50% ethanol eluate, and the filter membrane for adding molecular cut off 3000-7000 enters
Row ultrafiltration, by inlet pressure control in 0.2-0.7MPa, the NF membrane that filtered fluid adds molecular cut off 150 is concentrated,
Concentrate is transferred to extractor, and the water-saturated n-butanol for adding 7BV is extracted 4 times, and extract is concentrated, n-butanol is then reclaimed, i.e.,
It can obtain concentrated extract.Concentrated extract adds 15BV ethyl acetate dissolving, removes water layer, filters insoluble matter, and filtrate adds nothing
Aqueous sodium persulfate reclaims ethyl acetate, dichloromethane will be added in filtrate, then stirs evenly up to there is Precipitation, is subsequently placed with knot
Crystalline substance, crystal adds dichloromethane with ethyl acetate dissolving again and repeats crystallization 3 times, and filtering is dried under reduced pressure to obtain Monot's glycoside product
351g, content 99%.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie
In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit is required rather than described above is limited, it is intended that all in the implication and scope of the equivalency of claim by falling
Change is included in the present invention.
Moreover, it will be appreciated that although the present specification is described in terms of embodiments, not each embodiment is only wrapped
Containing an independent technical scheme, this narrating mode of specification is only that for clarity, those skilled in the art should
Using specification as an entirety, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
It may be appreciated other embodiment.
Claims (7)
1. a kind of preparation method of morroniside, it is characterised in that including following steps：
(1) raw material add ethanol to be extracted using microwave, ultrasonic synergistic extraction method：Fructus Corni raw material is crushed plus 5-10 times
Ethanol is measured, is extracted 40-60 minutes, extracted 2-3 times by microwave, Ultrasound-assisted；
(2) macroporous resin adsorption extract solution is used：The ethanol in extract solution is reclaimed, macroporous resin column is added after filtering and is inhaled
It is attached, then using water-alcohol gradient elution, finally collect morroniside flow point；
(3) morroniside flow point carries out filter operation by filter membrane：Morroniside flow point is added into milipore filter and carries out ultrafiltration, ultrafiltration is complete
NF membrane is added after to be filtered, and then collects concentrate；
(4) extraction behaviour and crystallization operation are carried out to the concentrate being collected into：Above-mentioned concentrate is added water saturation extracting n-butyl alcohol 2-4
It is secondary, then extract is merged, then be concentrated under reduced pressure, concentrated extract is can obtain after concentration, medicinal extract is dissolved in ethyl acetate
Insoluble matter and water layer are removed, anhydrous sodium sulfate is added and reclaims ethyl acetate, solution adds dichloromethane after filtering, then
It can be seen that there is white precipitate precipitation, crystallization is finally placed, crystallization 3-4 times is repeated, takes and morroniside is can obtain after being dried under reduced pressure
Product.
2. extracting method according to claim 1, it is characterised in that 1. middle concentration of alcohol is 20-60% to step.
3. extracting method according to claim 1, it is characterised in that 1. middle supersonic frequency is 20-80kHz to step, and power is 1-
50kW。
4. extracting method according to claim 1, it is characterised in that 1. middle microwave frequency is 2500kHz, power 10kW to step.
5. extracting method according to claim 1, it is characterised in that 2. middle macroreticular resin can be from HPD850, S-8, NAK- for step
Chosen in II, LAS-7, ADS-17.
6. extracting method according to claim 1, it is characterised in that 2. middle water-alcohol gradient elution is 6-10BV water -4- to step
6BV10-30% ethanol solution -6-9BV50-80% ethanol solutions.
7. extracting method according to claim 1, it is characterised in that step 3. filter membrane species and filter condition：Milipore filter is
Molecular cut off 3000-7000 filter membrane, NF membrane is the filter membrane of molecular cut off 150.Filter pressure 0.2-0.7MPa.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101974048A (en) * | 2010-06-28 | 2011-02-16 | 南京泽朗农业发展有限公司 | Method for extracting morroniside from dogwood |
| CN102127140A (en) * | 2010-11-25 | 2011-07-20 | 南京泽朗医药科技有限公司 | Method for combinedly extracting Morroniside, dogwood polysaccharide and ursolic acid from dogwood |
| CN102329353A (en) * | 2007-09-13 | 2012-01-25 | 山东绿叶天然药物研究开发有限公司 | Method for preparing morroniside |
| CN104147079A (en) * | 2014-07-09 | 2014-11-19 | 陕西师范大学 | Ultrasonic-microwave synergetic extracted cornel iridoid glycoside, as well as extraction and determination method thereof |
-
2017
- 2017-02-14 CN CN201710094742.9A patent/CN107286211A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102329353A (en) * | 2007-09-13 | 2012-01-25 | 山东绿叶天然药物研究开发有限公司 | Method for preparing morroniside |
| CN101974048A (en) * | 2010-06-28 | 2011-02-16 | 南京泽朗农业发展有限公司 | Method for extracting morroniside from dogwood |
| CN102127140A (en) * | 2010-11-25 | 2011-07-20 | 南京泽朗医药科技有限公司 | Method for combinedly extracting Morroniside, dogwood polysaccharide and ursolic acid from dogwood |
| CN104147079A (en) * | 2014-07-09 | 2014-11-19 | 陕西师范大学 | Ultrasonic-microwave synergetic extracted cornel iridoid glycoside, as well as extraction and determination method thereof |
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