CN107879904A - The method that sequoyitol and oleanolic acid are extracted from orpiment skin - Google Patents
The method that sequoyitol and oleanolic acid are extracted from orpiment skin Download PDFInfo
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- CN107879904A CN107879904A CN201711092346.9A CN201711092346A CN107879904A CN 107879904 A CN107879904 A CN 107879904A CN 201711092346 A CN201711092346 A CN 201711092346A CN 107879904 A CN107879904 A CN 107879904A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
- C07C41/36—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
- C07C41/38—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
- C07C41/40—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation
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- 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
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Abstract
The present invention relates to a kind of method that high-purity sequoyitol and oleanolic acid are extracted in skin from orpiment, and orpiment skin is extracted using alcohol reflux, filtering, filtrate concentration, obtains medicinal extract；Medicinal extract adds ethyl acetate to extract, and the upper large pore resin absorption column purifying of extract concentration, eluent is heavy using alkali soluble acid, crystallizes to obtain oleanolic acid sterling；Lower floor's medicinal extract is dissolved in water, filtering, large pore resin absorption column on filtrate, eluent concentration, crystallization, recrystallizes to obtain sequoyitol sterling.This method can make full use of the active ingredient of orpiment skin, can obtain sequoyitol and oleanolic acid sterling simultaneously, improve the added value of orpiment skin, while reduce production cost.
Description
Art
The present invention relates to a kind of method that high-purity sequoyitol and oleanolic acid are extracted in skin from orpiment, belong to natural production
The technical field of thing chemistry.
Background technology
Orpiment skin, also known as tuber fern, Ma red horses ovum, circle fern, perennial herb, high 30~60cm.Ground life or the Yu Xibian that grows nonparasitically upon another plant
Under, in crack of stone or on trunk.Main product is in Southwestern China and Fujian, Taiwan, Guangdong, Guangxi, Zhejiang, Hunan.Tuber fern is nontoxic, and its is complete
Grass and stem tuber can be used as medicine, tool clearing heat and promoting diuresis, subdhing swelling and detoxicating, peaceful lung cough-relieving, hemostasis and other effects, and China is among the people to be used for hair of catching a cold
Heat, high temperature do not move back, cough with lung heat, chordapsus, dysentery, urinary system infection contamination, infantile malnutrition due to digestive disturbances or intestinalparasites, scrofula hernia, five leaching gonorrhoeas, collapse band,
The diseases such as acute mastitis, postpartum edema and scald, centipde-bite, knife wound bleeding etc. are treated.Document report orpiment skin chemical composition master
There are terpene, flavonoids, phenolic compound, alkaloids, steroidal etc., studying more active component at present mainly has western Qu Yi
Alcohol, oleanolic acid, cupreol etc..
Sequoyitol is also known as sequoyitol, is the methylated derivative of inositol, in the presence of sequoyitol dehydrogenase, can make
NAD (+) is changed into NADP, participates in basic physiological biochemical process, has the function that to prevent and treat diabetes, and its toxicity pole
It is low, it is an of great value antidiabetic medicine.Sequoyitol is white or off-white powder.Water is dissolved in, is slightly soluble in methanol,
It is practically insoluble in acetoneand ethyl acetate.Molecular formula C7H14O6, molecular weight 194.18.
Oleanolic acid has protect liver drop enzyme, promotes the effect such as liver cell regeneration, anti-inflammatory, cardiac stimulant, diuresis, antitumor, also has
There are hypoglycemic, reducing blood lipid, calmness, be the active ingredient of exploitation treatment hepatopathy and diabetes.Oleanolic acid is white pin
Crystalline substance, 308 DEG C~310 DEG C of fusing point, molecular formula C30H48O3, molecular weight 456.71, methanol, ethanol, benzene and chloroform are dissolved in, hardly
It is dissolved in water.Because oleanolic acid is complicated, it is difficult to obtained with chemical synthesis process, mainly extracted at present from natural plants
Arrive.Extraction process mainly has：Solvent extraction method, supercritical fluid extraction, ultrasonic extraction and macroreticular resin absorbing method.
Publication No. CN102408318A Introduction To Cn Patent is a kind of to be extracted and the method for purifying sequoyitol, including red
The crushing of beans China fir raw material, Chinese yew concentrated extracting solution processed, isolate taxol decoction, to add flocculant sequoyitol crude product, system red
The steps such as China fir alcohol crystals, preparing high-purity sequoyitol.The present invention from Chinese yew raw material extract isolation of taxol decoction after, pass through to
Raffinate adds flocculant, and sequoyitol crude product is directly made after processing, makes the comprehensive utilization of Chinese yew raw material, simplifies obtained
The processing step of sequoyitol crude product, the production cost of sequoyitol extraction process is reduced, use and have more suitable for industrial production
Beneficial to environmental protection.
Publication No. CN101244991 Introduction To Cn Patent is a kind of using solvent deposition extraction and purifying sequoyitol
Method：Chinese yew raw material crushes；Raw material is extracted with Extraction solvent, obtains Chinese yew concentrated extract；Chinese yew concentrated extract
Concentration, stirring, ethanol, at least one of acetone are added, stood, precipitation collects solid content or precipitation, and dry Chinese yew does dense
Contracting thing；Dry concentrate adds methanol eddy extraction, collects reflux extracting liquid, stirring, precipitation solvent is added in reflux extracting liquid,
Cooling, stand, collection precipitates to obtain sequoyitol crude product；Sequoyitol crude product adds methanol eddy dissolving, filtering, collects phegma, dense
Contracting, cool down, stand, low temperature crystallization, filtering, collect crystal；Chinese larch alcohol crystals add water heating stirring to be added rudimentary to dissolution of crystals
One of alcohol, acetone, acetonitrile, stir, and are incubated, and stand, and cooling, low temperature crystallization, filtering, collect crystal, at least repeat crystallization 3
It is secondary, dry, sampling carries out HPLC detections by detection method, obtains the sequoyitol high sterling of content >=99%.
Publication No. CN1994995 Introduction To Cn Patent a kind of method of extraction and purification sequoyitol, the method are main
Including three parts, 1. with alcohols, acetone or water be that extractant extracts active ingredient containing sequoyitol from Chinese yew raw material, is obtained
Sequoyitol coarse raw materials containing 0.3~5% (wt)；2. using above-mentioned sequoyitol coarse raw materials as raw material, through chromatography, obtain 10% with
The Chinese larch raw polyol of upper content；3. with the sequoyitol of more than 10% content through 2-4 times crystallization, obtain more than 99% sterling it is red
China fir alcohol.
The extraction from the tuber fern platymiscium of Publication No. CN101185662 Introduction To Cn Patent one kind mainly contains western song
According to the preparation method of the extract of alcohol, and application of the extract for preventing and treating diabetes.From tuber fern platymiscium root,
Stem, leaf etc. are raw material, by methanol, ethanol or acetone extraction, with chloroform, ethyl acetate, dichloromethane or n-butanol with
Water two-phase extraction, recycling design, water section macroreticular resin etc. separate and purify to obtain extract, are white powder, its is main
Composition is sequoyitol, and wherein the content of sequoyitol is in 10.00%-99.99%, the extraction owner obtained using this method
It is used to prevent and treat diabetes and its complication.
The method that Publication No. CN105348364A Introduction To Cn Patent extracts oleanolic acid from the fruit of glossy privet, can have
Effect solves the problems, such as that low existing extracting method extraction efficiency, pollution environment, extract purity are low, and method is to use the fruit of glossy privet super
Particle comminution adds ethanol, ultrasonic extraction, is centrifuged off precipitating, obtain supernatant, supernatant is used into the fine powder of 10-5 μm of granularity
NaOH is adjusted to pH=11-13, is stirred 10-14 hours, filtering, and filtrate adjusts pH=2.5-3.5 with HCl, and stirring 10-14 is small
When, 50 DEG C of relative density 1.1-1.2 are concentrated into, concentrate are purified by flash by D101 macroporous resin columns, eluent is volume
The ethanol of concentration 90%, eluent dosage are 6-8 times of column volume, collect eluent, are condensed into medicinal extract, medicinal extract is used
Sephadex LH-20 gels are further purified, and produce oleanolic acid.
Oleanolic acid and ursolic acid in a kind of kiwifruit oil of Publication No. CN105301122A Introduction To Cn Patent
Content assaying method, it is mainly by using reversed-phased high performace liquid chromatographic, its chromatographic condition：A. chromatographic column：C18 posts,
250 × 4.6mm, 5 μm；B. phase composition is flowed：The triethylamine of -0.1% glacial acetic acid of -35% water of 265% methanol -0.05%, wherein, stream
It is dynamic mutually to be configured by methanol 265mL, water 35mL, glacial acetic acid 0.05mL and triethylamine 0.05mL；C. the detection of UV-detector used
Wavelength：210nm；D. flow velocity：0.6mL/min, sampling volume：20 μ L, column temperature：20℃.
A kind of method that oleanolic acid is extracted from olive leaf of Publication No. CN105085601A Introduction To Cn Patent,
Comprise the steps:Immersion treatment, Feedstock treating, digest, deoil, alcohol extracting, column chromatography, recrystallization.The present invention is first carried using enzyme
Vegetable fat is taken, is divided oily and non-oil component to oily different with the affinity difference and profit proportion of water using non-oil component
From, add product yield and improve recovery rate, the hypericin that the present invention obtains, content more than 0.5% (UV detections),
Below ash content 7%.
Publication No. CN105061544A Introduction To Cn Patent is a kind of to extract oleanolic acid from the fresh pawpaw fruit
Method, can quickly, safety extraction oleanolic acid, good economy performance, be suitable for the needs of industrialized production, set without large-scale
Standby, extraction time is short, and production efficiency is high, it is ensured that oleanolic acid quick separate out to greatest extent, obtains the neat of high-purity
Pier tartaric acid crystal；And the extracting method processing step is simple, mild condition, there is wide industrial application value, be suitable for
Large-scale production.
A kind of method that oleanolic acid is extracted from selfheal of Publication No. CN104592343A Introduction To Cn Patent.
Comprise the following steps：Dry selfheal is crushed, adds alcohol reflux extraction, be concentrated under reduced pressure to obtain extractum A；Add petroleum ether leaching
Wash, ethanol dissolution filter, separated through SMBC, obtain the component B rich in oleanolic acid；Dry purity
More than 95% oleanolic acid.Oleanolic acid extracting method of the present invention, using microwave radiation exaraction and Simulation moving bed
The technique that chromatography separating-purifying combines, it is determined that related process parameters, step is simple, and product purity is higher, when extraction separates
Between it is shorter, production efficiency is improved.
Publication No. CN104478985A Introduction To Cn Patent is a kind of from this Aralia wood blades to extract oleanolic acid
Method, step is as follows：This Aralia wood blades particle is added in extract solution and is heated to 90-95 DEG C, until mixeding liquid volume subtracts
It is few to 1/5th, the liquid after separation and Extraction, then rejoin extract solution in this Aralia woods of blade powder and be heated to
90-95 DEG C, until mixeding liquid volume is reduced to 1/5th, repeat said extracted process 3-4 times；Merge the liquid after extraction,
Room temperature is cooled to, filtrate is obtained through membrane filtration；Filtrate is mixed with deionized water, 90 DEG C of water-baths make ethanol volatilization until occurring
Light brown slurries；Slurries are extracted with ether, then 70 DEG C of water-baths are until ether volatilization completely, obtains oleanolic acid extract.
The present invention the advantages of be：Method technique that this extracts oleanolic acid from this Aralia wood blades is simple, time-consuming short, extraction effect
Rate is high, and testing result shows：Through 3 extractions, 2 hours used times, recovery rate can reach 99.81%.
With the rapid development of economy, the continuous improvement of living standards of the people, the rising of diabetes morbidity and patient's
Become younger outstanding aobvious protrusion, and the antidiabetic drug market demand also constantly expands.Sequoyitol and oleanolic acid are respectively provided with hypoglycemic pharmacology
Effect, and be natural products, small toxicity, it is of great value antidiabetic medicine, in having a extensive future for medicine.
Therefore, extraction sequoyitol and oleanolic acid from orpiment skin is explored to mean a great.
The content of the invention
Presently disclosed documents and materials only extract sequoyitol from orpiment skin, and other active components are not carried out with extraction point
From causing the waste of resource.For the non-comprehensive development and utilization problem of active component of orpiment skin, the present invention provides a kind of operation
Simply, rational technology, the quick production technology for extracting sequoyitol and oleanolic acid simultaneously.
The technical solution adopted by the present invention includes：Orpiment skin is extracted using alcohol reflux, filtering, filtrate concentration, obtains medicinal extract；
Medicinal extract adds ethyl acetate to extract, and the upper large pore resin absorption column purifying of extract concentration, eluent is heavy using alkali soluble acid, crystallizes together
Pier tartaric acid sterling；Lower floor's medicinal extract is dissolved in water, filtering, large pore resin absorption column on filtrate, eluent concentration, crystallizes, recrystallization
Obtain sequoyitol sterling.
Therefore, the present invention provides a kind of method for extracting high-purity sequoyitol and oleanolic acid simultaneously in skin from orpiment,
Specific steps include as follows：
(1) orpiment skin is crushed to the mesh of 80 mesh~120, adds 60~80% ethanol solution refluxing extraction 3 times, 2 hours every time,
Filtering, merging filtrate, filtrate are concentrated under reduced pressure at 55 DEG C~65 DEG C, obtain medicinal extract I；
(2) medicinal extract I plus the ethyl acetate of two volumes are extracted 2 times, 1 hour every time, combined ethyl acetate extract, obtained
Acetic acid ethyl fluid and lower floor's medicinal extract II；
(3) acetic acid ethyl fluid is concentrated to dryness, adds a certain amount of 70-90% ethanol to dissolve, filtered, D101 macropores on filtrate
Polymeric adsorbent, after adsorbing 30min, first with the water elution of 3-5BV upper prop liquid, discard water elution, then with 5-8BV upper prop liquid
80-95% ethanol elutions, collect eluent I；
(4) eluent I is concentrated into certain volume, 5-10% sodium hydroxide solutions is added dropwise and adjust PH to 10-11, add a certain amount of
Charcoal absorption 10min, filtering, filtrate add hydrochloric acid to adjust PH to 1-3, place and separate out crystallization, ceramic membrane filter, with distillation water washing
Crystal, obtain oleanolic acid sterling；
(5) lower floor's medicinal extract II in step (2) is dissolved in water, filtered, D101 macroporous absorbent resins on filtrate, absorption
20min, first eluted with the water of 2-5BV column volumes, then eluted with the 5-20% ethanol solutions of 2-5BV column volumes, closed
And two kinds of eluents II；
(6) eluent II is concentrated under reduced pressure into the 1/20~1/30 of original volume at 50 DEG C~60 DEG C, adds ethanol to crystallization
Separate out, ceramic membrane filter, then recrystallize 2 times, obtain sequoyitol sterling.
Ceramic membrane filter is used in the step, fenestra pore size is 0.22 μm；BV refers to a times column volume.
60-80% ethanol solutions are added described in the step (1), are 10- by volume (L)/orpiment tare weight amount (kg) ratio
15:1。
70-90% ethanol solutions are added described in the step (3), are 3-5 by volume (L)/residue weight (kg) ratio:1.
1/10~1/20 that certain volume is original volume is concentrated into described in the step (4)；The amount of activated carbon is by weight
(kg)/liquor capacity ratio (L) is 0.01-0.05:1.
The amount of water is added described in the step (5), is 1-2 by volume (L)/medicinal extract (L) ratio:1.
Technique effect：
1st, extracted simultaneously by using orpiment skin and obtain the sequoyitol and oleanolic acid of high-purity, substantially increase orpiment
The utilization rate of skin, improves added value；The production cost of sequoyitol and oleanolic acid is reduced simultaneously, saves Chinese medicine aptitude
Source.
2nd, sequoyitol is extracted from orpiment skin, substitute has been found for Chinese yew, extend sequoyitol extraction raw material
Medicine resource, protect first-grade state protection plant again.
3rd, raw material of the present invention is extracted using alcohol reflux, is obtained sequoyitol and oleanolic acid alcohol extract, is improved recovery rate,
Extraction time is shortened simultaneously, greatlys save energy consumption again.
4th, equipment used in the inventive method, method for extraction and purification are common conventional equipment and method, are avoided
For the dependence of expensive instrument and equipment in commercial process, its production cost is greatly reduced.
5th, the reagent used in the present invention is nontoxic, cheap, volume production chemical reagent, using maturation in whole process
The routine techniques of reagent recovery, significantly reduces the risk to environmental emission discarded object.
Embodiment
With reference to specific embodiment, the invention will be further described, following examples be intended to illustrate invention rather than
Limitation of the invention further.
Embodiment 1
Orpiment skin crushes, and crosses 80 mesh sieves, weighs 5kg, adds 50L 60% ethanol solution refluxing extraction 3 times, 2 hours every time,
Filtering, merging filtrate, filtrate are concentrated under reduced pressure at 55 DEG C~65 DEG C, obtain 5L medicinal extract I；By medicinal extract I plus 10L ethyl acetate extraction 2
It is secondary, 1 hour every time, combined ethyl acetate extract, obtain acetic acid ethyl fluid and lower floor's medicinal extract II；Acetic acid ethyl fluid is concentrated into
It is dry, add 1L 70% ethanol dissolve, filter, D101 macroporous absorbent resins on filtrate, after absorption 30min, first with 3L water elution,
Water elution, then 80% ethanol elution with 5L are discarded, collects eluent I；Eluent I is concentrated into 0.5L, 5% hydrogen-oxygen is added dropwise
Change sodium solution and adjust PH to 10, add 5g charcoal absorption 10min, filtering, filtrate adds hydrochloric acid to adjust PH to 1, places and separates out crystallization, pottery
Porcelain membrane filtration, with distilled water wash crystallization thing, obtain 16.4mg oleanolic acid sterlings；Lower floor's medicinal extract II plus 8L water are dissolved, mistake
Filter, D101 macroporous absorbent resins on filtrate, adsorb 20min, first eluted with 10L water, then entered with 10L 10% ethanol solution
Row elution, merges two kinds of eluents II；Eluent II is concentrated under reduced pressure into 1L at 50 DEG C~60 DEG C, add ethanol to crystallize separate out,
Ceramic membrane filter, then recrystallize 2 times, obtain 11.2g sequoyitol sterlings.Detected through HPLC, the purity of oleanolic acid sample is
99.04%, the purity of sequoyitol sample is 98.73%.
Embodiment 2
Orpiment skin crushes, and crosses 120 mesh sieves, weighs 10kg, adds 120L 70% ethanol solution refluxing extraction 3 times, 2 is small every time
When, filtering, merging filtrate, filtrate is concentrated under reduced pressure at 55 DEG C~65 DEG C, obtains 12L medicinal extract I；Medicinal extract I plus 24L ethyl acetate are extracted
Take 2 times, 1 hour every time, combined ethyl acetate extract, obtain acetic acid ethyl fluid and lower floor's medicinal extract II；Acetic acid ethyl fluid is concentrated
To doing, add 2.5L 80% ethanol to dissolve, filter, D101 macroporous absorbent resins on filtrate, after adsorbing 30min, first with 10L water
Elution, water elution, then 95% ethanol elution with 15L are discarded, collect eluent I；Eluent I is concentrated into 1L, is added dropwise 5%
Sodium hydroxide solution adjusts PH to 11, adds 20g charcoal absorption 10min, filtering, and filtrate adds hydrochloric acid to adjust PH to 2, places and separates out knot
Crystalline substance, ceramic membrane filter, with distilled water wash crystallization thing, obtain 35.7mg oleanolic acid sterlings；By the water-soluble of lower floor's medicinal extract II plus 15L
Solution, filter, D101 macroporous absorbent resins on filtrate, adsorb 20min, first eluted with 20L water, then 10% ethanol with 20L
Solution is eluted, and merges two kinds of eluents II；Eluent II is concentrated under reduced pressure into 2L at 50 DEG C~60 DEG C, adds ethanol to crystallization
Separate out, ceramic membrane filter, then recrystallize 2 times, obtain 25.1g sequoyitol sterlings.Detected through HPLC, the purity of oleanolic acid sample
For 98.72%, the purity of sequoyitol sample is 98.91%.
Embodiment 3
Orpiment skin crushes, and crosses 120 mesh sieves, weighs 20kg, adds 150L 70% ethanol solution refluxing extraction 3 times, 2 is small every time
When, filtering, merging filtrate, filtrate is concentrated under reduced pressure at 55 DEG C~65 DEG C, obtains 25L medicinal extract I；Medicinal extract I plus 50L ethyl acetate are extracted
Take 2 times, 1 hour every time, combined ethyl acetate extract, obtain acetic acid ethyl fluid and lower floor's medicinal extract II；Acetic acid ethyl fluid is concentrated
To doing, add 8L 90% ethanol to dissolve, filter, D101 macroporous absorbent resins on filtrate, after adsorbing 30min, first with 25L washing
It is de-, water elution, then 95% ethanol elution with 50L are discarded, collects eluent I；Eluent I is concentrated into 2.5L, is added dropwise 5%
Sodium hydroxide solution adjusts PH to 11, adds 40g charcoal absorption 10min, filtering, and filtrate adds hydrochloric acid to adjust PH to 2, places and separates out knot
Crystalline substance, ceramic membrane filter, with distilled water wash crystallization thing, obtain 68.3mg oleanolic acid sterlings；By the water-soluble of lower floor's medicinal extract II plus 25L
Solution, filter, D101 macroporous absorbent resins on filtrate, adsorb 20min, first eluted with 40L water, then 10% ethanol with 40L
Solution is eluted, and merges two kinds of eluents II；Eluent II is concentrated under reduced pressure into 4L at 50 DEG C~60 DEG C, adds ethanol to crystallization
Separate out, ceramic membrane filter, then recrystallize 2 times, obtain 48.6g sequoyitol sterlings.Detected through HPLC, the purity of oleanolic acid sample
For 97.83%, the purity of sequoyitol sample is 98.46%.
Claims (6)
1. extracting the method for high-purity sequoyitol and oleanolic acid in a kind of skin from orpiment, its specific steps includes as follows：
(1) orpiment skin is crushed to the mesh of 80 mesh~120, adds 60~80% ethanol solution refluxing extraction 3 times, 2 hours every time, mistake
Filter, merging filtrate, filtrate are concentrated under reduced pressure at 55 DEG C~65 DEG C, obtain medicinal extract I；
(2) medicinal extract I plus the ethyl acetate of two volumes are extracted 2 times, 1 hour every time, combined ethyl acetate extract, obtains acetic acid
Ethyl ester liquid and lower floor's medicinal extract II；
(3) acetic acid ethyl fluid is concentrated to dryness, adds a certain amount of 70-90% ethanol to dissolve, filtered, D101 macroporous absorptions on filtrate
Resin, after adsorbing 30min, first with the water elution of 3-5BV upper prop liquid, discard water elution, then the 80- with 5-8BV upper prop liquid
95% ethanol elution, collect eluent I；
(4) eluent I is concentrated into certain volume, 5-10% sodium hydroxide solutions is added dropwise and adjust PH to 10-11, add a certain amount of activity
Charcoal adsorbs 10min, filtering, and filtrate adds hydrochloric acid to adjust PH to 1-3, places and separates out crystallization, ceramic membrane filter, with distilled water wash crystallization
Thing, obtain oleanolic acid sterling；
(5) lower floor's medicinal extract II in step (2) is dissolved in water, filtered, D101 macroporous absorbent resins on filtrate, adsorb 20min,
First eluted with the water of 2-5BV column volumes, then eluted with the 5-20% ethanol solutions of 2-5BV column volumes, merge two kinds
Eluent II；
(6) eluent II is concentrated under reduced pressure into the 1/20~1/30 of original volume at 50 DEG C~60 DEG C, add ethanol to crystallize separate out,
Ceramic membrane filter, then recrystallize 2 times, obtain sequoyitol sterling.
2. claim 1 method, ceramic membrane filter is used in the step, fenestra pore size is 0.22 μm；BV refers to a times post
Volume.
3. 60-80% ethanol solutions are added described in claim 1 method, wherein step (1), by volume l/ orpiment tare weight amounts kg
Than for 10-15:1.
4. 70-90% ethanol solutions are added described in claim 1 method, wherein step (3), by volume l/ residue weights kg ratios
For 3-5:1.
5. 1/10~1/20 that certain volume is original volume is concentrated into described in claim 1 method, wherein step (4)；Activity
The amount of charcoal kg/ liquor capacities by weight are 0.01-0.05 than l:1.
It is 1-2 by volume l/ medicinal extract l ratios 6. adding the amount of water described in claim 1 method, wherein step (5):1.
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| CN1994995A (en) * | 2006-01-06 | 2007-07-11 | 上海百灵医药科技有限公司 | Method for extracting and purifying sequoyitol |
| CN101185662A (en) * | 2006-11-15 | 2008-05-28 | 广州联创思远利生物科技有限公司 | Method and use for preparing novel medicine for treating diabetes prepared from tuber fern |
| CN101244991A (en) * | 2008-03-21 | 2008-08-20 | 昆明自主择业集源生物科技有限公司 | Method for extracting and purifying sequoyitol by using solvent deposition |
| CN102659899A (en) * | 2012-04-24 | 2012-09-12 | 劲牌有限公司 | Method for extracting purified oleanolic acid from glossy privet fruits |
| CN105348364A (en) * | 2015-11-06 | 2016-02-24 | 郑州师范学院 | Method for extraction of oleanolic acid from fructus ligustri lucidi |
| CN105753927A (en) * | 2016-03-31 | 2016-07-13 | 长沙湘资生物科技有限公司 | Method for extracting oleanolic acid from talinum crassifolium |
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2017
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