CN105541938B - The method that macroporous adsorbent resin method prepares natural aucubin is increased using UF membrane - Google Patents
The method that macroporous adsorbent resin method prepares natural aucubin is increased using UF membrane Download PDFInfo
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- CN105541938B CN105541938B CN201510993202.5A CN201510993202A CN105541938B CN 105541938 B CN105541938 B CN 105541938B CN 201510993202 A CN201510993202 A CN 201510993202A CN 105541938 B CN105541938 B CN 105541938B
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- 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
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- 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
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Abstract
The present invention relates to aucubins extracted from seed of bark of eucommia and preparation method thereof.The method of the present invention is to extract the methods of glycosides in seed of bark of eucommia with organic solvent, extracting solution is concentrated under reduced pressure to be diluted again, dilution cleans through seperation film, it isolates and purifies to obtain the extract containing aucubin through macroporous absorbent resin again, extract high-temperature pressure-reduction dries to obtain aucubin product, and content is up to 95% or more.The present invention provides efficient, easy preparation methods, and are suitable for large-scale industrial production.
Description
【Technical field】
The present invention relates to a kind of effective ingredient in Chinese extractive technique fields.More particularly it relates to a kind of content
95% or more aucubin further relates to the preparation method of the aucubin.
【Background technology】
Cortex Eucommiae is a kind of rare ancient Chinese medicine, sweet in flavor, warm-natured.Tonify the liver and kidney, strengthen muscles and bones, coordinating Chong and Conception Vessels,
The effect of strengthen meridian and miscarriage prevention.Eucommia ulmoides extracts also have the effects that stronger anti-hypertension, anti-help, anti-oxidant, anti-gastric-ulcer, it
It can also promote collagen synthesis, also there are many other pharmacological effects.The iridoids and its glucosides of Cortex Eucommiae are that it is made to have
There are these active main compounds.The general bitter of iridoid substance, but there are a variety of physiological activity.Aucubin is
A kind of iridoid glucosides separated from folium cortex eucommiae, skin or seed.The conjunction that it has lidan liver, promotes collagen
At multiple pharmacological effects such as, anti-muscle skeleton agings.CN 200910064817 discloses a kind of eucommia ulmoides extracts to be had in preparation
Application in the composition of sedative-hypnotic effect also discloses eucommia ulmoides extracts and is preparing for treating insomnia, anxiety or shying
The application fainted in composition, which is from Bark of Eucommia Ulmoides, folium cortex eucommiae, eucommia Bark male flower and/or Cortex Eucommiae complete stool through oil
Ether, ethyl acetate, n-butanol, second alcohol and water continuously extract.CN 201110202162 discloses eucommia ulmoides extracts and is preparing
For the application in the cosmetics or drug of skin anti-aging, especially anti-light aging.CN201110302835 is related to Cortex Eucommiae
Or eucommia ulmoides extracts are preparing the purposes in being used for as the drug of Vasoprotectant and/or hypotensive agent, or used preparing
Purposes in the drug for the treatment of and/or prevention vascular proliferative disease.CN 201310027831 discloses a kind of Cortex Eucommiae extraction
Object and its application in the pharmaceutical composition for preparing prevention and treatment bone metabolic disturbance disease.
UF membrane is the separation technology occurred in early 20th century.Membrane separation technique is due to having separation, concentration, pure concurrently
Change and refined function, but have efficiently, energy-saving and environmental protection, molecular level filtering and filter process is simple, the features such as easily controllable, because
This, is widely used to the necks such as food, medicine, biology, environmental protection, chemical industry, metallurgy, the energy, oil, water process, electronics, bionical
Domain produces huge economic benefit and social benefit, it has also become one of most important means in current separation science.
Macroporous absorbent resin is a kind of cross-linked polymer for being free of ion-exchange group, stable in physicochemical property, insoluble in acid,
Alkali and organic solvent have concentration, centrifugation to organic matter, and are not done by inorganic salts, strong ion and low molecular compound
It disturbs.Macroporous absorbent resin can selectively adsorb organic substance by physical absorption, so as to achieve the purpose that isolate and purify.
According to resin surface property, macroporous absorbent resin can be divided into nonpolarity, middle polarity and polarity three classes.
The isolation and purification method of high-purity aucubin is solvent extraction, supercritical fluid extraction and column chromatography
Method.The more of high-purity aucubin extract is obtained using organic solvent extractionprocess at present, but is required for using a variety of easy
Explosive organic solvent is fired, height is required to industrial equipment, operating process is complicated, and product yield is not high, waste liquid exhaust emission environment
In place of the deficiencies of serious.The shortcoming of supercritical fluid extraction is that instrument and equipment is of high cost, and energy consumption is serious.Column chromatography
The major defect of method, which is silica gel, to be regenerated, and production cost is high.
Therefore, also need to that a kind of both safety, product yield be high, the side of isolating and purifying environmental-friendly, production cost is low at present
Method, for this purpose, the present inventor completes the present invention finally on the basis for summarizing the prior art by a large number of experiments.
【Invention content】
[technical problems to be solved]
The object of the present invention is to provide a kind of preparation methods of aucubin.
[technical solution]
The present invention is achieved through the following technical solutions.
The present invention relates to a kind of methods for extracting aucubin from seed of bark of eucommia.
The step of this method, is as follows：
A, organic solvent extracts
By seed of bark of eucommia decladding, it is ground into seed of bark of eucommia powder, then according to seed of bark of eucommia powder and alcohol or ketone aqueous solutions of organic solvent
Weight ratio 1:5~10, the seed of bark of eucommia powder under conditions of 45~55 DEG C of temperature is with stirring with concentration by volume 40~
80% alcohol or ketone aqueous solutions of organic solvent extract 2.5~3.5 hours, then repeat extraction 2~3 times in the same fashion, and extracting solution closes
And be then concentrated under reduced pressure, concentrate I is obtained, while recycling organic solvent；
B, UF membrane
According to the volume ratio 2~4 of concentrate I and deionized water, the concentrate I that step A is obtained is diluted with deionized water
To a kind of solution, it is 5000 by being equipped with molecular cut off under conditions of 0.1~0.5MPa of pressure then to allow the solution
The membrane module of~50000 seperation film carries out UF membrane, removes impurity, obtains a kind of filtrate；
C, resin adsorption
Pass through macroporous absorption under conditions of 0.5~2 times of column volume/h of flow velocity and room temperature according to the filtrate that step B is obtained is allowed
Resin column, then eluted with deionized water it is colourless to eluate, according still further to the volume ratio of alcohol eluant, eluent and large pore resin absorption column
It is 2~4, is that 0.5~2 times of column volume/h alcohol eluant, eluent rows elute with flow, collects eluent, be then concentrated under reduced pressure, obtain
Concentrate II, while recycling alcohol；
D, it dries
The concentrate II that step C is obtained is subjected to high-temperature pressure-reduction drying, obtains the aucubin.
According to a preferred embodiment of the invention a, in step, the granularity of the seed of bark of eucommia powder is 20~200
Mesh.
According to another preferred embodiment of the invention, in step, the organic solvent is a kind of selected from second
The organic solvent of alcohol, methanol or acetone.
According to another preferred embodiment of the invention, in stepb, the seperation film is hollow-fibre membrane, pottery
Porcelain film or PS membrane.
According to another preferred embodiment of the invention, in step C, the macroporous absorbent resin be D101,
HP20 or XAD-2 macroporous absorbent resins.
According to another preferred embodiment of the invention, in step C, the large pore resin absorption column be its height with
Diameter ratio is 15~25:1 large pore resin absorption column.
According to another preferred embodiment of the invention, in step C, the eluant, eluent be it is a concentration of by volume
15~90% ethyl alcohol or methanol aqueous solution.
According to another preferred embodiment of the invention, in step A and step C, the reduced pressure is to press
It is concentrated under conditions of 0.01~0.08MPa of power.
According to another preferred embodiment of the invention, in step D, high-temperature pressure-reduction drying is in temperature 55
~65 DEG C with dried under conditions of 0.01~0.05MPa of pressure.
According to another preferred embodiment of the invention, in step D, the water content of the aucubin is with peach
Leaf coral glycosides total weight 3~5%.
The present invention is described in more detail below.
The present invention, which adopts the following technical scheme that, prepares aucubin：Dry Cortex Eucommiae decladding seed is taken, crushes, uses organic solvent
Extraction 2~3 times merges extracting solution and is concentrated under reduced pressure, and obtained concentrate is diluted with deionized water, is then carried out UF membrane, is obtained
To filtrate cross macroporous absorbent resin, first with deionized water flushing eluted again with polar organic solvent, eluent depressurize dense
Contracting, obtains peach jaurel glucoside extract.The extract is dried with high-temperature pressure-reduction again, obtains aucubin product.
In particular it relates to a kind of method for extracting aucubin from seed of bark of eucommia.The preparation of the aucubin
Steps are as follows：
A, organic solvent extracts
By seed of bark of eucommia decladding, it is ground into seed of bark of eucommia powder, then according to seed of bark of eucommia powder and alcohol or ketone aqueous solutions of organic solvent
Weight ratio 1:5~10, the seed of bark of eucommia powder under conditions of 45~55 DEG C of temperature is with stirring with concentration by volume 40~
80% alcohol or ketone aqueous solutions of organic solvent extract 2.5~3.5 hours, then repeat extraction 2~3 times in the same fashion, and extracting solution closes
And be then concentrated under reduced pressure, concentrate I is obtained, while recycling organic solvent；
Cortex Eucommiae decladding seed is crushed using disintegrating apparatus usually used in Chinese medicine manufacture field, Du
The granularity of secondary seed powder is usually 20~200 mesh.Certainly, the granularity of seed of bark of eucommia powder is not very crucial, is more than this particle size range
Seed of bark of eucommia powder can also use, but can influence extraction effect.
In the present invention, alcohol or ketone organic solvent are it should be understood that a kind of can extract aucubin from seed of bark of eucommia
Organic solvent, these organic solvents are a kind of volatile, and residue will not also generate adverse consequences to tobacco product to be had
Solvent.
In the present invention, the organic solvent is a kind of organic solvent selected from ethyl alcohol, methanol or acetone.
Preferably, the organic solvent is ethyl alcohol or acetone.
It is highly preferred that the organic solvent is ethyl alcohol.
In the present invention, the concentration of the organic solvent is by volume 40~80%, if the concentration is less than 40%,
The water-solubility impurities such as a large amount of polysaccharide, protein are will produce, subsequent purification processing brings difficulty；If the concentration is more than 80%,
Excessive organic solvent can be lost, increase production cost；Therefore, a concentration of the 40~80% of the organic solvent are appropriate, excellent
Selection of land is 48~70%, more preferably 56~62%.
The weight ratio of the organic solvent and alcohol or ketone aqueous solutions of organic solvent is 1:5~10, if it exceeds this is heavy
Amount can then dissolve excessive impurity, and can increase solvent loss than range.
The reduced pressure is concentrated under conditions of 0.01~0.08MPa of pressure.It is used when reduced pressure
Equipment is equipment usually used in current processing technique of Chinese herbs field, such as rotary evaporator, vacuum-concentrcted device.
The organic solvent is recycled after the completion of extraction step, the technology people of generally use the art
The way of distillation is recycled known to member.
B, UF membrane
According to the volume ratio 2~4 of concentrate I and deionized water, the concentrate I that step A is obtained is diluted with deionized water
To a kind of solution, it is 5000 by being equipped with molecular cut off under conditions of 0.1~0.5MPa of pressure then to allow the solution
The membrane module of~50000 seperation film carries out UF membrane, removes impurity, obtains a kind of filtrate；
It, can material if the volume ratio of concentrate I and deionized water is less than 2 when concentrate I is diluted with deionized water
Viscosity is excessive, and separation fenestra is easy to block；If the volume ratio of concentrate I and deionized water is more than 4, can volume of material mistake
Greatly, disengaging time is long；Therefore, the volume ratio of concentrate I and deionized water is reasonable for 2~4.
In the present invention, compared with existing isolation and purification method, membrane separation technique can high efficiency, remove to low energy consumption
The small molecular weight impurities such as the big molecular impurities such as protein, polysaccharide for containing in Chinese medical extract ingredient and inorganic salts.Therefore, UF membrane
Technology can significantly improve aucubin purity and quality for the present invention.
In the present invention, the seperation film used is hollow-fibre membrane, ceramic membrane or PS membrane.
Hollow-fibre membrane is a kind of outer likeness in form threadiness, the film with self-supporting effect.Its compacted zone can be located at fiber
Outer surface, such as reverse osmosis membrane may be alternatively located at the inner surface of fiber, such as microfiltration membranes, NF membrane and ultrafiltration membrane.During the present invention uses
Empty fiber membrane is current market sales of product, such as the polyvinyl chloride hollow fiber of the triumphant filter film technology Co., Ltd in Hangzhou
Film.
Ceramic membrane is the solid membrane material belonged in membrane separation technique, mainly with the aluminium oxide of different size, zirconium oxide, oxygen
Change the inorganic ceramic materials such as titanium and silica as supporter, is formed through surface coating, high-temperature firing.The ceramics that the present invention uses
Film is current market sales of product, such as the ceramic membrane of Wuxi Kai Ou membrane separation plants Co., Ltd.
It is the film for repeating to have made of the high-molecular compound of sulfuryl and arlydene screening function that PS membrane, which is main chain,.It is poly-
The sulphur atom of sulfone is highest oxidation state, and the conjugation of sulfuryl makes it have excellent inoxidizability and thermal stability, and ether chain changes
The toughness of polysulfones has been apt to it, phenyl ring improves mechanical strength and modulus.The PS membrane that the present invention uses is current market sales of
Product, for example, Hangzhou Hao Tianmo Science and Technology Ltd.s polysulfone ultrafiltration membrane.
The present invention is 5000~50000 using the molecular cut off of seperation film, if separation retaining molecular weight is too small, meeting
Increase disengaging time, causes the waste of time cost；Separation retaining molecular weight is excessive to introduce a large amount of big molecular impurities, increase
Subsequent purification is born.It is existing market that the present invention, which uses the membrane module for the seperation film for being 5000~50000 equipped with molecular cut off,
The product of upper sale, for example, the triumphant filter film technology Co., Ltd in Hangzhou PVC hollow fiber membrane.
The present invention is progress UF membrane under conditions of 0.1~0.5MPa of operating pressure；If the operating pressure
Less than 0.1MPa, disengaging time is long；Higher than 0.5MPa, pressure of equipment is excessive, is also easy to produce leakage.
C, resin adsorption
The filtrate that step B is obtained is allowed to pass through macroporous absorbent resin under conditions of 0.5~2 times of column volume/h of flow velocity and room temperature
Column, then eluted with deionized water it is colourless to eluate, according still further to the volume ratio of alcohol eluant, eluent and large pore resin absorption column be 2~
4, it is that 0.5~2 times of column volume/h alcohol eluant, eluent rows elute with flow, collects eluent, be then concentrated under reduced pressure, obtain concentrate
II, while recycling alcohol；
In the present invention, macroporous absorbent resin is a kind of polymer adsorption tree for being free of cation exchange groups and having macroporous structure
Fat has good macroreticular structure and larger specific surface area, can be optionally through in physical absorption aqueous solution
Organic matter.It is widely used in separation and the purification process of Chinese herbal medicine effective ingredients.It is single that it, which is with styrene and acrylate,
Body, using divinylbenzene as crosslinking agent, using toluene, dimethylbenzene as pore-foaming agent, their polymerizations that are cross-linked with each other form stephanoporate framework knot
Structure.This resin has adsorptivity by Van der Waals force and hydrogen bond action between itself and the molecule adsorbed, because of it
Reticular structure and high-specific surface area and can be realized point with the ability for selectively adsorbing organic substance, therefore using this resin
From the purpose with purifying.
In the present invention, the macroporous absorbent resin used is D101, HP20 or XAD-2 type macroporous absorbent resin or its pole
Property with the comparable other macroporous absorbent resins of the macroporous absorbent resin, they are all the products sold extensively currently on the market,
Such as by the D101 types macroporous absorbent resin of the great poly resin Science and Technology Ltd. in Tianjin production, by Mitsubishi chemical production
HP20 types macroporous absorbent resin, the XAD-2 types macroporous absorbent resin produced by Rhom and Hass of the U.S. know science and technology by Xi'an indigo plant
The other macroporous absorbent resins of LX-11, D101C type of Co., Ltd's production.
The large pore resin absorption column that the present invention uses is its height and diameter ratio is 15~25:1 macroporous absorbent resin
Column.
The macroporous absorbent resin that the present invention uses needs to be pre-processed as follows before using：
95% ethyl alcohol impregnates for 24 hours, and efflux and water 1 are washed till with 95% ethyl alcohol：5 is muddy, is washed with water to no alcohol taste；It uses again
5%HCl impregnates 2~4h, is washed to neutrality by resin column；2~4h is impregnated, is washed to by resin column with 2%NaOH again
Neutrality, it is spare.
Then, the filtrate that step B is obtained is allowed to be inhaled by macropore under conditions of 0.5~2 times of column volume/h of flow velocity is with room temperature
Attached resin column reaches complete absorption.
The large pore resin absorption column first eluted with deionized water after absorption it is colourless to eluate, in this way can be more
Fully, thoroughly the water-soluble big polar impurity cleaning such as carbohydrate, the mucus juice of large pore resin absorption column absorption is removed, then,
Alcohol eluent is used again.
In the present invention, the alcohol eluant, eluent is ethyl alcohol or methanol aqueous solution.The ethyl alcohol or methanol aqueous solution it is dense
Degree is by weight by volume 15~90%.If the concentration of the alcohol eluant, eluent be less than 15%, eluant, eluent polarity compared with
Greatly, object is difficult to elute, if the concentration of the alcohol eluant, eluent is more than 90%, solvent loss is larger, and increase is produced into
This, therefore, a concentration of the 15~90% of the alcohol eluant, eluent is reasonable, and preferably 20~65%, more preferably 35~
50%.
Preferably, the alcohol eluant, eluent be it is a concentration of by weight 20~65% ethanol water.
When elution, eluant, eluent is slowly added in adsorption column, flow velocity is adjusted and reaches 0.5~2 times of column volume/h.
Situation is concentrated under reduced pressure and is described with step B identical, details are not described herein.
D, it dries
The concentrate II that step C is obtained is subjected to high-temperature pressure-reduction drying, obtains the aucubin.
The described high-temperature pressure-reduction drying is dried under conditions of 55~65 DEG C of temperature is with 0.01~0.05MPa of pressure
It is dry.
The main function of this baking step is to remove moisture in product, convenient for storage.
In the present invention, equipment used in high-temperature pressure-reduction drying is current market sales of product, such as by Shanghai
The vacuum drying chamber of precision instrumentation Co., Ltd.
Acquired aucubin product is analyzed under the following conditions using conventional H PLC methods：
Use instrument：Japanese Shimadzu high performance liquid chromatograph Essentia LC-15C
Assay method：Area external standard method
Determination condition：With Nucleosi17-C18 (Φ 4.6 × 250mm, 10 μm) for analytical column, mobile phase is methanol-water
(5∶95)；Column temperature:25℃；Detection wavelength:203nm；Flow velocity:1.0ml/min,
Measurement result show to use the aucubin content of the method for the present invention products therefrom be by weight 95% with
On.
Recovery rate is calculated according to following the equation by seed of bark of eucommia amount and aucubin product amount：
Recovery rate=(A × B)/(C × D) × 100%
A:Product quality
B:Aucubin content in product
C:Material quality
D:Aucubin content in raw material
The recovery rate that seed of bark of eucommia is extracted using the method for the present invention is 95% or more.
[advantageous effect]
Active constituent content is high in glucoside extract containing peach jaurel prepared by the present invention, and content is 95% or more.
Due to select membrane separation technique, for existing isolation and purification method, can high efficiency, remove to low energy consumption
The small molecular weight impurities such as the big molecular impurities such as protein, polysaccharide ingredient and inorganic salts, can reach and significantly improve aucubin purity
With the purpose of quality.
Good to the adsorptive selectivity of aucubin due to selecting macroporous absorbent resin, absorption is fast, and desorption is also fast,
Adsorption capacity is larger；Physical and chemical stability is high, and mechanical strength is good, and regeneration is easy；Operation is very easy, and step is few, at low cost
Honest and clean, 95% or more extraction rate reached, solvent all recoverables are also applied for large-scale industrial production.
【Description of the drawings】
Fig. 1 is aucubin extractive HPLC figure prepared by the method for the present invention.
【Specific implementation mode】
The present invention will be clarified in more detail below by embodiment.
Embodiment 1：Aucubin is extracted from seed of bark of eucommia
The implementation steps of the embodiment are as follows：
A, organic solvent extracts
By seed of bark of eucommia decladding, 80 mesh seed of bark of eucommia powder are ground into, then according to the weight of seed of bark of eucommia powder and alcohol or ketone aqueous solution
Than 1:9, with concentration, 65% ethanol water extracts the seed of bark of eucommia powder by volume under conditions of 52 DEG C of temperature and stirring
2.5 hours, then extraction 2 times is repeated in the same fashion, extracting solution merges, and then uses and is produced by Shanghai Yarong Biochemical Instrument Plant
Rotary evaporator is concentrated under reduced pressure under conditions of pressure 0.08MPa, obtains concentrate I, while recycling organic solvent；
B, UF membrane
According to the volume ratio 2 of concentrate I and deionized water, the concentrate I that step A is obtained is diluted to obtain one with deionized water
Kind of solution, then allow the solution under conditions of pressure 0.1MPa by equipped with molecular cut off be 5000 it is triumphant by Hangzhou
The membrane module of the PVC hollow fiber membrane of filter film technology Co., Ltd production carries out UF membrane, removes impurity, obtains one kind
Filtrate；
C, resin adsorption
Allow the filtrate that step B is obtained under conditions of 1.5 times of column volume/h of flow velocity and room temperature by by the great poly resin in Tianjin
The D101 type large pore resin absorption columns of Science and Technology Ltd.'s production, its height are 22 with diameter ratio:1, then use deionization
Water wash is colourless to eluate, is 3 according still further to the volume ratio of alcohol eluant, eluent and large pore resin absorption column, with flow for 1.4 times of columns
A concentration of 95% ethanol waters by volume of volume/h elute the elution of agent row, collect eluent, then use by Shanghai Asia
The rotary evaporator of flourish biochemical instrument factory production is concentrated under reduced pressure under conditions of pressure 0.08MPa, obtains concentrate II, returns simultaneously
Receive alcohol；
D, it dries
Using the vacuum drying chamber produced by Shanghai precision instrumentation Co., Ltd, the concentrate II that step C is obtained
High-temperature pressure-reduction drying is carried out under conditions of 55 DEG C of temperature and pressure 0.02MPa, it is with aucubin gross weight to obtain water content
The peach jaurel glucoside extract of gauge 3.0%.
Aucubin extractive HPLC analysis result prepared by the embodiment is referring to attached drawing 1.
Use method described in this specification measure the aucubin content of its peach jaurel glucoside extract for
95.25%, it is 95.01% that recovery rate, which is calculated,.
Embodiment 2：Aucubin is extracted from seed of bark of eucommia
The implementation steps of the embodiment are as follows：
A, organic solvent extracts
By seed of bark of eucommia decladding, 140 mesh seed of bark of eucommia powder are ground into, then according to the weight of seed of bark of eucommia powder and alcohol or ketone aqueous solution
Than 1:10, with concentration, 40% methanol aqueous solution extracts the seed of bark of eucommia powder by volume under conditions of temperature 45 C is with stirring
2.8 hours, then extraction 3 times is repeated in the same fashion, extracting solution merges, and then uses and is produced by Shanghai Yarong Biochemical Instrument Plant
Rotary evaporator is concentrated under reduced pressure under conditions of pressure 0.01MPa, obtains concentrate I, while recycling organic solvent；
B, UF membrane
According to the volume ratio 3 of concentrate I and deionized water, the concentrate I that step A is obtained is diluted to obtain one with deionized water
Then kind of solution allows the solution under conditions of pressure 0.4MPa by being 10000 by Wuxi equipped with molecular cut off
The membrane module of the ceramic membrane of Kai Ou membrane separation plants Co., Ltd carries out UF membrane, removes impurity, obtains a kind of filtrate；
C, resin adsorption
Allow the filtrate that step B is obtained under conditions of 1.8 times of column volume/h of flow velocity and room temperature by by Mitsubishi chemistry
The HP20 type large pore resin absorption columns of production, its height are 25 with diameter ratio:1, then eluted to wash-off with deionized water
Liquid is colourless, is 2 according still further to the volume ratio of alcohol eluant, eluent and large pore resin absorption column, with flow for 0.5 times of column volume/h concentration
It is eluted for 1% ethyl alcohol by volume or methanol aqueous solution eluant, eluent row, collects eluent, then used by the sub- flourish biochemical instruments in Shanghai
The rotary evaporator of device factory production is concentrated under reduced pressure under conditions of pressure 0.01MPa, obtains concentrate II, while recycling alcohol；
D, it dries
Using the vacuum drying chamber produced by Shanghai precision instrumentation Co., Ltd, the concentrate II that step C is obtained
High-temperature pressure-reduction drying is carried out under conditions of 58 DEG C of temperature and pressure 0.01MPa, it is with aucubin gross weight to obtain water content
The peach jaurel glucoside extract of gauge 3.6%.
Aucubin extractive HPLC analysis chart prepared by the embodiment is identical as the result of embodiment 1.
Use method described in this specification measure the aucubin content of its peach jaurel glucoside extract for
95.43%, it is 95.06% that recovery rate, which is calculated,.
Embodiment 3：Aucubin is extracted from seed of bark of eucommia
The implementation steps of the embodiment are as follows：
A, organic solvent extracts
By seed of bark of eucommia decladding, 20 mesh seed of bark of eucommia powder are ground into, then according to the weight of seed of bark of eucommia powder and alcohol or ketone aqueous solution
Than 1:5, with concentration, 45% aqueous acetone solution extracts the seed of bark of eucommia powder by volume under conditions of 48 DEG C of temperature and stirring
3.2 hours, then extraction 2 times is repeated in the same fashion, extracting solution merges, and then uses and is produced by Shanghai Yarong Biochemical Instrument Plant
Rotary evaporator is concentrated under reduced pressure under conditions of pressure 0.02MPa, obtains concentrate I, while recycling organic solvent；
B, UF membrane
According to the volume ratio 4 of concentrate I and deionized water, the concentrate I that step A is obtained is diluted to obtain one with deionized water
Then kind of solution allows the solution under conditions of pressure 0.5MPa by being 30000 by Hangzhou equipped with molecular cut off
The membrane module of the polysulfone ultrafiltration membrane of Hao Tian films Science and Technology Ltd. production carries out UF membrane, removes impurity, obtains a kind of filtrate；
C, resin adsorption
Allow the filtrate that step B is obtained under conditions of 2.0 times of column volume/h of flow velocity and room temperature by by U.S.'s ROHM AND HAAS
The XAD-2 type large pore resin absorption columns of company's production, its height are 15 with diameter ratio:1, then with deionized water elute to
Eluate is colourless, is 3 according still further to the volume ratio of alcohol eluant, eluent and large pore resin absorption column, is that 0.8 times of column volume/h is used with flow
A concentration of elution of 35% ethanol water by volume agent row elution, collects eluent, then uses by the sub- flourish biochemical instruments in Shanghai
The rotary evaporator of device factory production is concentrated under reduced pressure under conditions of pressure 0.02MPa, obtains concentrate II, while recycling alcohol；
D, it dries
Using the vacuum drying chamber produced by Shanghai precision instrumentation Co., Ltd, the concentrate II that step C is obtained
High-temperature pressure-reduction drying is carried out under conditions of 62 DEG C of temperature and pressure 0.04MPa, it is with aucubin gross weight to obtain water content
The peach jaurel glucoside extract of gauge 4.3%.
Aucubin extractive HPLC analysis chart prepared by the embodiment is identical as the result of embodiment 1.
Use method described in this specification measure the aucubin content of its peach jaurel glucoside extract for
95.72%, it is 95.10% that recovery rate, which is calculated,.
Embodiment 4：Aucubin is extracted from seed of bark of eucommia
The implementation steps of the embodiment are as follows：
A, organic solvent extracts
By seed of bark of eucommia decladding, 200 mesh seed of bark of eucommia powder are ground into, then according to the weight of seed of bark of eucommia powder and alcohol or ketone aqueous solution
Than 1:7, with concentration, 80% ethanol water extracts the seed of bark of eucommia powder by volume under conditions of 55 DEG C of temperature and stirring
3.5 hours, then extraction 3 times is repeated in the same fashion, extracting solution merges, and then uses and is produced by Shanghai Yarong Biochemical Instrument Plant
Rotary evaporator is concentrated under reduced pressure under conditions of pressure 0.06MPa, obtains concentrate I, while recycling organic solvent；
B, UF membrane
According to the volume ratio 3 of concentrate I and deionized water, the concentrate I that step A is obtained is diluted to obtain one with deionized water
Then kind of solution allows the solution under conditions of pressure 0.2MPa by being 50000 by Hangzhou equipped with molecular cut off
The membrane module of the PVC hollow fiber membrane of triumphant filter film technology Co., Ltd production carries out UF membrane, removes impurity, obtains one
Kind filtrate；
C, resin adsorption
Allow the filtrate that step B is obtained under conditions of 1.4 times of column volume/h of flow velocity and room temperature by by Mitsubishi chemistry
The HP20 type large pore resin absorption columns of production, its height are 18 with diameter ratio:1, then eluted to wash-off with deionized water
Liquid is colourless, is 4 according still further to the volume ratio of alcohol eluant, eluent and large pore resin absorption column, with flow for 2.0 times of column volumes/h concentration
The elution of agent row is eluted for 50% ethanol water by volume, eluent is collected, then uses by Shanghai Yarong Biochemical Instrument Plant
The rotary evaporator of production is concentrated under reduced pressure under conditions of pressure 0.06MPa, obtains concentrate II, while recycling alcohol；
D, it dries
Using the vacuum drying chamber produced by Shanghai precision instrumentation Co., Ltd, the concentrate II that step C is obtained
High-temperature pressure-reduction drying is carried out under conditions of 65 DEG C of temperature and pressure 0.05MPa, it is with aucubin gross weight to obtain water content
The peach jaurel glucoside extract of gauge 5.0%.
Aucubin extractive HPLC analysis chart prepared by the embodiment is identical as the result of embodiment 1.
Use method described in this specification measure the aucubin content of its peach jaurel glucoside extract for
95.89%, it is 95.14% that recovery rate, which is calculated,.
Embodiment 5：Aucubin is extracted from seed of bark of eucommia
The implementation steps of the embodiment are as follows：
A, organic solvent extracts
By seed of bark of eucommia decladding, 80 mesh seed of bark of eucommia powder are ground into, then according to the weight of seed of bark of eucommia powder and alcohol or ketone aqueous solution
Than 1:8, with concentration, 80% aqueous acetone solution extracts the seed of bark of eucommia powder by volume under conditions of 48 DEG C of temperature and stirring
2.5 hours, then extraction 3 times is repeated in the same fashion, extracting solution merges, and then uses and is produced by Shanghai Yarong Biochemical Instrument Plant
Rotary evaporator is concentrated under reduced pressure under conditions of pressure 0.02MPa, obtains concentrate I, while recycling organic solvent；
B, UF membrane
According to the volume ratio 3 of concentrate I and deionized water, the concentrate I that step A is obtained is diluted to obtain one with deionized water
Then kind of solution allows the solution under conditions of pressure 0.1MPa by being 10000 by Hangzhou equipped with molecular cut off
The membrane module of the polysulfone ultrafiltration membrane of Hao Tian films Science and Technology Ltd. carries out UF membrane, removes impurity, obtains a kind of filtrate；
C, resin adsorption
Allow the filtrate that step B is obtained under conditions of 1.0 times of column volume/h of flow velocity and room temperature by by the great poly resin in Tianjin
The D101 type large pore resin absorption columns of Science and Technology Ltd.'s sale, its height are 23 with diameter ratio:1, then use deionization
Water wash is colourless to eluate, is 3 according still further to the volume ratio of alcohol eluant, eluent and large pore resin absorption column, with flow for 1.4 times of columns
A concentration of 10% ethanol waters by volume of volume/h elute the elution of agent row, collect eluent, then use by Shanghai Asia
The rotary evaporator of flourish biochemical instrument factory production is concentrated under reduced pressure under conditions of pressure 0.04MPa, obtains concentrate II, returns simultaneously
Receive alcohol；
D, it dries
Using the vacuum drying chamber produced by Shanghai precision instrumentation Co., Ltd, the concentrate II that step C is obtained
High-temperature pressure-reduction drying is carried out under conditions of temperature 60 C and pressure 0.03MPa, it is with aucubin gross weight to obtain water content
The peach jaurel glucoside extract of gauge 4.6%.
Aucubin extractive HPLC analysis chart prepared by the embodiment is identical as the result of embodiment 1.
Use method described in this specification measure the aucubin content of its peach jaurel glucoside extract for
96.02%, it is 95.7% that recovery rate, which is calculated,.
Embodiment 6：Aucubin is extracted from seed of bark of eucommia
The implementation steps of the embodiment are as follows：
A, organic solvent extracts
By seed of bark of eucommia decladding, 140 mesh seed of bark of eucommia powder are ground into, then according to the weight of seed of bark of eucommia powder and alcohol or ketone aqueous solution
Than 1:6, with concentration, 62% ethanol water extracts the seed of bark of eucommia powder by volume under conditions of 54 DEG C of temperature and stirring
3.0 hours, then extraction 2 times is repeated in the same fashion, extracting solution merges, and then uses and is produced by Shanghai Yarong Biochemical Instrument Plant
Rotary evaporator is concentrated under reduced pressure under conditions of pressure 0.04MPa, obtains concentrate I, while recycling organic solvent；
B, UF membrane
According to the volume ratio 2 of concentrate I and deionized water, the concentrate I that step A is obtained is diluted to obtain one with deionized water
Then kind of solution allows the solution under conditions of pressure 0.4MPa by being 30000 by Hangzhou equipped with molecular cut off
The membrane module of the PVC hollow fiber membrane of triumphant filter film technology Co., Ltd production carries out UF membrane, removes impurity, obtains one
Kind filtrate；
C, resin adsorption
Allow the filtrate that step B is obtained under conditions of 1.2 times of column volume/h of flow velocity and room temperature by by Mitsubishi chemistry
The HP20 type large pore resin absorption columns of production, its height are 20 with diameter ratio:1, then eluted to wash-off with deionized water
Liquid is colourless, is 4 according still further to the volume ratio of alcohol eluant, eluent and large pore resin absorption column, with flow for 1.5 times of column volumes/h concentration
The elution of agent row is eluted for 40% ethanol water by volume, eluent is collected, then uses by Shanghai Yarong Biochemical Instrument Plant
The rotary evaporator of production is concentrated under reduced pressure under conditions of pressure 0.05MPa, obtains concentrate II, while recycling alcohol；
D, it dries
Using the vacuum drying chamber produced by Shanghai precision instrumentation Co., Ltd, the concentrate II that step C is obtained
High-temperature pressure-reduction drying is carried out under conditions of temperature 60 C and pressure 0.03MPa, it is with aucubin gross weight to obtain water content
The peach jaurel glucoside extract of gauge 3.2%.
Aucubin extractive HPLC analysis chart prepared by the embodiment is identical as the result of embodiment 1.
Use method described in this specification measure the aucubin content of its peach jaurel glucoside extract for
95.66%, it is 95.46% that recovery rate, which is calculated,.
Claims (8)
1. a kind of method for extracting aucubin from seed of bark of eucommia, it is characterised in that the step of this method is as follows：
A, organic solvent extracts
By seed of bark of eucommia decladding, it is ground into seed of bark of eucommia powder, then according to the weight of seed of bark of eucommia powder and alcohol or ketone aqueous solutions of organic solvent
Than 1:5~10, the seed of bark of eucommia powder is under conditions of 45~55 DEG C of temperature is with stirring with concentration 40~80% alcohol by volume
Or ketone aqueous solutions of organic solvent extracts 2.5~3.5 hours, then extraction 2~3 times is repeated in the same fashion, extracting solution merges, then
It is concentrated under reduced pressure, obtains concentrate I, while recycling organic solvent；The organic solvent is a kind of selected from ethyl alcohol, methanol or acetone
Organic solvent；
B, UF membrane
According to the volume ratio 2~4 of concentrate I and deionized water, the concentrate I that step A is obtained is diluted to obtain one with deionized water
Kind of solution, then allow the solution be 5000 by being equipped with molecular cut off under conditions of 0.1~0.5MPa of pressure~
The membrane module of 50000 seperation film carries out UF membrane, removes impurity, obtains a kind of filtrate；The seperation film is doughnut
Film, ceramic membrane or PS membrane；
C, resin adsorption
Allow the filtrate that step B is obtained 0.5~2 times of column volume/h of flow velocity and under conditions of room temperature by large pore resin absorption column,
Then eluted with deionized water it is colourless to eluate, according still further to the volume ratio of alcohol eluant, eluent and large pore resin absorption column be 2~4,
It is that 0.5~2 times of column volume/h is eluted with alcohol eluant, eluent with flow, collects eluent, be then concentrated under reduced pressure, obtain concentrate
II, while recycling alcohol；
D, it dries
The concentrate II that step C is obtained is subjected to high-temperature pressure-reduction drying, obtains the aucubin.
2. according to the method described in claim 1, it is characterized in that in step, the granularity of the seed of bark of eucommia powder is 20~
200 mesh.
3. according to the method described in claim 1, it is characterized in that in step C, the macroporous absorbent resin be D101,
HPD20 or XAD-2 macroporous absorbent resins.
4. according to the method described in claim 1, it is characterized in that in step C, the large pore resin absorption column is its height
It is 15~25 with diameter ratio:1 large pore resin absorption column.
5. extracting method according to claim 1, it is characterised in that in step C, the eluant, eluent be it is a concentration of with
The ethyl alcohol or methanol aqueous solution of stereometer 15~90%.
6. extracting method according to claim 1, it is characterised in that in step A and step C, the reduced pressure is
It is concentrated under conditions of 0.01~0.08MPa of pressure.
7. extracting method according to claim 1, it is characterised in that in step D, the high-temperature pressure-reduction drying be
55~65 DEG C of temperature with dried under conditions of 0.01~0.05MPa of pressure.
8. extracting method according to claim 1, it is characterised in that in step D, the water content of the aucubin
It is with aucubin total weight 3~5%.
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| CN102219814A (en) * | 2011-05-25 | 2011-10-19 | 河南大学 | Method for extracting aucubin from eucommia ulmoides oliver seed draff |
| CN103864867B (en) * | 2012-12-14 | 2015-04-08 | 湖北老龙洞杜仲开发有限公司 | Method for extracting aucubin from folium cortex eucommiae |
| CN104546992A (en) * | 2015-01-30 | 2015-04-29 | 四川九章生物科技有限公司 | Folium cortex eucommiae extract as well as preparation method and application thereof |
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Address after: 850000 Lhasa economic and Technological Development Zone, Tibet autonomous region, road, investment building, Applicant after: HUABAO FLAVOURS & FRAGRANCES CO.,LTD. Address before: 850000 Lhasa economic and Technological Development Zone, Tibet autonomous region, road, investment building, Applicant before: Huabao flavor Ltd. Address after: 850000 Lhasa economic and Technological Development Zone, Tibet autonomous region, road, investment building, Applicant after: Huabao flavor Ltd. Address before: 201821 Yecheng Road, Shanghai, No. 1299, No. Applicant before: Huabao Flavours & Fragrances Co.,Ltd |
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