CN107903292A - The extracting method of Stibene-glucoside in a kind of fleece-flower root - Google Patents
The extracting method of Stibene-glucoside in a kind of fleece-flower root Download PDFInfo
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Abstract
The invention discloses a kind of extracting method of Stibene-glucoside in fleece-flower root, comprise the following steps:1) fleece-flower root powder is provided;2) entrainment reagent is added into fleece-flower root powder, the entrainment reagent is ultra-pure water;3) fleece-flower root powder is through supercritical CO2Extraction obtains extraction product, and the extraction temperature is 48 52 DEG C, and the extracting pressure is 36Mpa 40Mpa;The extraction product through separation reactor I and separation reactor I I, obtains Stibene-glucoside crude product successively, and the separation reactor I temperature is 43 47 DEG C, and pressure is 11 13Mpa, and the separation reactor I I temperature is 28 32 DEG C, and pressure is 7 9Mpa;4) the Stibene-glucoside crude product dissolves through absolute ethyl alcohol, filters acquisition filtrate, and Stibene-glucoside finished product is obtained after the filtrate drying.Extracting method provided by the invention, simple operation, post processing is simple, and environment friendly and pollution-free, for extraction yield up to 5.25%, purity has reached 98%.
Description
Technical field
The present invention relates to field of traditional Chinese medicine extraction, the extracting method of Stibene-glucoside specially in a kind of fleece-flower root.
Background technology
The fleece-flower root is the root tuber of polygonaceae platymiscium, and the Li Shizhen (1518-1593 A.D.) meaning tuber of multiflower knotweed has red white point.China's pharmacopeia with polygonaceae plant it
Root tuber is certified products, i.e., the red tuber of multiflower knotweed.《Compendium of Materia Medica》Record:" fleece-flower root is only pained, replenishing qi and blood, black beard and hair, happy color, long term usage length
Muscles and bones, benefiting quintessence, macrobiosis be not old ".The Stibene-glucoside contained in the fleece-flower root is its reducing blood lipid, intelligence development, the master of anti-aging effects
Active ingredient is wanted, is widely used in terms of functional food.
Since the nineties in last century, the development and application to the fleece-flower root such as the U.S., Japan have made intensive studies, with the fleece-flower root
International market is had been enter into for raw material development functionality food.In recent years, extracted from the fleece-flower root using Stibene-glucoside as mainization
Study point, developing new drug and functional food also cause the very big concern of domestic and international scientific worker.
CO2Supercritical extraction technique is that development is swift and violent in recent years, and obtained in Chinese herbal medicine effective ingredients abstraction technique field
To widely applied technology.The technology has the following advantages:The extraction temperature of technique is relatively low, can make in spices or Chinese herbal medicine effectively
Component exempts from destruction, keeps its bioactivity;And mass transfer velocity is fast in extraction process, rate of extraction is fast, and extraction yield is high;CO2Nothing
Poison, not residual organic solvent, product is pure natural, while saves substantial amounts of organic solvent, reduces environmental pollution, easily separated.
At present, in the prior art, the preparation process of the Stilbene Glucoside in the fleece-flower root has document report second
Alcohol carries out CO as entrainment reagent2Supercritical extract, but this method still cannot be by whole Stibene-glucoside extractions in the fleece-flower root
Completely.In the prior art, still Stibene-glucoside in the fleece-flower root is not extracted using water as entrainment reagent, and higher can be obtained
The report of recovery rate.
The content of the invention
The present invention provides a kind of extracting method of Stibene-glucoside in fleece-flower root, extracting method post processing letter
Single, purity is high, and extraction yield is good, is conducive to the industrialized production of Stibene-glucoside and as medicinal mechanism study.
To solve the above problems, the present invention provides a kind of extracting method of Stibene-glucoside in fleece-flower root, including following steps
Suddenly:
1) fleece-flower root powder is provided;
2) entrainment reagent is added into fleece-flower root powder, the entrainment reagent is ultra-pure water;
3) fleece-flower root powder is through supercritical CO2Extraction obtains extraction product, and the extraction temperature is 48-52 DEG C, the extraction
Pressure power is 36Mpa-40Mpa;The extraction product obtains Stibene-glucoside crude product, institute successively through separation reactor I and separation reactor I I
Separation reactor I temperature is stated as 43-47 DEG C, pressure 11-13Mpa, the separation reactor I I temperature is 28-32 DEG C, pressure 7-9Mpa;
4) the Stibene-glucoside crude product dissolves through ethanol, filters acquisition filtrate, and hexichol second is obtained after the filtrate drying
Alkene glycosides finished product.
Preferably, the preparation method of the step 1) fleece-flower root powder is ground into the powder of 6-9 mesh for the fleece-flower root is dried in the shade
End.
Preferably, the step 1) fleece-flower root is any in Sichuan Wanyuan, enshi, Ankang, Tongren district Guizhou Province
The place of production.
Preferably, the step 2) entrainment reagent and the weight ratio of the fleece-flower root are (1.5-2.2):5.
Preferably, the step 2) entrainment reagent and the weight ratio of the fleece-flower root are 2:5.
Preferably, the step 3) extraction temperature is 50 DEG C, pressure 38Mpa.
Preferably, step 3) is cycling extraction, extraction time 1.8-2.2h.
Preferably, step 3) extraction time is 2h.
Preferably, step 3) the separation reactor I temperature is 45 DEG C, pressure 12Mpa.
Preferably, step 3) the separation reactor I I temperature is 30 DEG C, pressure 8Mpa.
Preferably, CO in step 3)2Flow is 10-11 l/h.
Preferably, CO in step 3)2Flow is 10.5 l/h.
Preferably, described be filtered into of step 4) is filtered using macroreticular resin.
It is more highly preferred to, the macroreticular resin is one kind in D101, DM130, S-8, D600, HPD500, II, ZTC-1
It is or a variety of.
Supercritical CO2Extract (SC-CO2) in, CO2It is apolar substance, there is selective dissolution, SC-CO2It is right
Low molecule, low polarity, lipophilicity, low-boiling component such as volatile oil, hydrocarbon, ester, lactone, ether, epoxide etc. show excellent
Different dissolubility.The effective elements of the medicine is the compound that polarity group is more and molecular weight is larger in major part, SC-CO2To big
Material more than molecule and polarity group then extracts relative difficulty, it is necessary to add entrainment reagent to change its dissolubility.It is common to carry under one's arms
Agent has methanol, ethanol, acetone, ethyl acetate etc..
Extract is in SC-CO2In course of dissolution, by molecular weight, molecular structure, molecular polarity, containing parent/hydrophobicity
The number and CO of functional group2Many factors such as the compatibility of molecule influence.After adding entrainment reagent, SC-CO is formd2—
Entrainment reagent new system, is that the dissolubility of system changes first;Secondly SC-CO can also be changed2Critical point;In addition hold under the arm
Interaction force-Van der Waals force can be formed between band agent and solute molecule;The entrainment reagent and solute particular functional of hydrogen bond can be formed
Hydrogen bond complexing and other active forces can also be formed between group.The molecular polarity of entrainment reagent is bigger, and solute is in supercritical CO2In
Solubility is bigger;The increase of the relative molecular mass or molecular volume of entrainment reagent, it is in supercritical CO2In solubility reduce,
Extraction yield reduces;Easily form hydrogen bond carries under one's arms agent molecule, can significantly improve extraction yield;Multi-component entrainment reagent, to extracting efficiency
Raising it is more notable.
For the present invention using water as entrainment reagent, hydrone molecular weight is less than ethanol molecule, molecular weight and molecular volume
Reduction adds in the fleece-flower root Stibene-glucoside in supercritical CO2Solubility in fluid, and the polarity and hexichol of hydrone
The polarity of ethene glycosides more closely, all polyhydroxy in the hydroxyl and Stibene-glucoside contained in hydrone can be formed it is intermolecular
Hydrogen bond, further increases supercritical CO2The extraction efficiency of fluid, and hydrone non-poisonous material itself pollutes, through macroreticular resin mistake
After filter, obtain being free of organic solvent, impurity is few, the high Stibene-glucoside sterling of purity.
The present invention first dries in the shade Radix Polygoni Multiflori, adds disintegrating machine and smashes in powdered, the Radix Polygoni Multiflori place of production is Sichuan Wanyuan,
Enshi, Ankang, any place of Tongren district Guizhou Province, are preferably Sichuan Wanyuan and/or enshi.Accurately weigh a certain amount of powder
End is fitted into extraction bucket, and entrainment reagent is directly added in bucket is extracted, and supercritical extraction unit is opened, to extraction kettle and separation reactor I
Extraction kettle is separately heated to separation reactor I I and when separating still reaches certain temperature, open CO2Gas cylinder, opens certain C O2Flow,
When being forced into certain pressure to extraction kettle and two separating stills, extraction is started the cycle over, keeps each kettle pressure balance.The timing of extraction one
Between after, obtain separation product.Dissolved with absolute ethyl alcohol, filter, filter vacuum is dried into 3h, up to product.With standard control,
Content is measured by high performance liquid chromatography, calculates extraction yield.
The present invention overcomes the problem of the difficulty that pure water does entrainment reagent post processing.The post processing of material by extraction needs to use
Filtered after absolute ethyl alcohol dissolving with macroreticular resin, in the prior art, generally select identical with entrainment reagent solvent dissolving, and used and surpass
Pure water makees solvent, not strong by macroreticular resin mobility, and which results in ultra-pure water to do one of the reason for entrainment reagent extraction yield is low.This
Invention post processing is dissolved using absolute ethyl alcohol first, is solved the shortcomings that post processing is difficult, is improved extraction yield.
The present invention specify that supercritical CO2Extract the optimum condition of Stibene-glucoside in the fleece-flower root, i.e. entrainment reagent ultra-pure water
Weight ratio with the fleece-flower root is 2:5th, extracting pressure 38MPa, temperature are 50 DEG C;The pressure of separating still I is 12Mpa, and temperature is
45℃;The pressure of separating still II is 8Mpa, and temperature is 30 DEG C;CO2Flow 10.5l/h, final extraction yield is up to 5.25%, purity
Reach 98%.
Since Stibene-glucoside total content is not high in the fleece-flower root, be 5.62%, this data source in Zhao Ronghua, Zhao Shenglan in
It is published within 2008 the 31st phase of Yunnan University of Traditional Chinese Medicine's journal article of page 12《Fleece-flower root different parts Stibene-glucoside is containing measurement
It is fixed》.Therefore extracting process provided by the invention can more completely extract the Stibene-glucoside component in the fleece-flower root, and operate letter
Victory, post processing is rapid, Nonpoisonous, non-environmental-pollution, and the present invention also specify that the optimal place of production of raw material is Sichuan Wanyuan and Hubei grace
Apply, be conducive to the industrialized production of Stibene-glucoside and as medicinal mechanism study.
Embodiment
In order to make those skilled in the art more fully understand the technical solution of invention, with reference to embodiment pair
The present invention is described in further detail.
The fleece-flower root, the also known as tuber of multiflower knotweed, the red tuber of multiflower knotweed, are few section's Plant-Polygonum (Polygonum multif lorum Thunb)
Dried root.Modern medicine shows that the fleece-flower root has enhancing immune function, and antioxidation, delays brain aging, improves
DNA repair functions, extend the service life, reduce cholesterol, improve the multiple functions such as fat metabolism.The main component of the fleece-flower root has hydroxyl
Anthraquinone analog compound (the predominantly glucoside such as rheum emodin, rheum officinale atmosphere, Rhein, be stilbenes compound), quinones
Compound, stibene glucoside type compound, amides compound, chromogen ketone compounds, lecithin, microelements of calcium, iron,
Zinc, manganese, copper etc..
Stibene-glucoside is distinctive bioactive ingredients in the fleece-flower root, and chemical name is 2,3,5,4'- tetrahydroxy hexichol
Ethene -2-O- β-D-Glucose glycosides, molecular formula C20H22O9, molecular weight 406.39, chemical structural formula sees below formula.
Its appearance is white amorphous powder, soluble easily in water, methanol, ethanol, acetone etc., dissolves in ethyl acetate, indissoluble
Trans stilbene glycosides is converted into cis-stilbene glycosides under lipophylic organic solvents, illumination condition, in hot conditions (> 60
DEG C), it is very unstable in acid solution, under strong acid, basic conditions, glucose, aglycon or quinones can be hydrolyzed to respectively.
Research shows that Stibene-glucoside, which has, to slow down aging, protects liver, adjust the effect such as blood fat, neuroprotection, antitumor.
Stibene-glucoside category polyol, has stronger molecular polarity, is soluble in low molecule alcohol solvent, acetone
Deng being insoluble in lipophylic organic solvents.At present, the Extraction solvent of Stibene-glucoside selects ethanol solution more, its extraction process master
Room temperature cold-maceration, alkali pickling is taken to sink method, heating reflux method, microwave irradiation and ultrasonic extraction method etc..Wherein, room temperature is cold
Leaching method and heating reflux method are common scale extracting methods.
In the prior art, also ethanol conduct is used using the report of supercritical extraction extraction Stibene-glucoside mostly
Entrainment reagent, improves extraction yield.But still Stibene-glucoside component in the fleece-flower root can not be extracted complete.And prior art table
Bright, if entrainment reagent is changed to water from ethanol, its extraction yield is less than ethanol, does not reach the requirement of industrialization.
The extracting method of Stibene-glucoside, comprises the following steps in the fleece-flower root provided by the invention:
1) fleece-flower root powder is provided;The preparation method of fleece-flower root powder is ground into the powder of 6-9 mesh for the fleece-flower root is dried in the shade
End.
2) entrainment reagent is added into fleece-flower root powder, the entrainment reagent is ultra-pure water;The weight of the entrainment reagent and the fleece-flower root
It is (1.5-2.2) to measure ratio:5;Preferably, entrainment reagent and the weight ratio of the fleece-flower root are 2:5.
3) fleece-flower root powder is through supercritical CO2Extraction obtains extraction product, and the extraction temperature is 48-52 DEG C, preferably warm
Spend for 50 DEG C;The extracting pressure is 36Mpa-40Mpa;It is preferred that pressure is 38Mpa;The extraction product is successively through separation reactor I
With separation reactor I I, Stibene-glucoside crude product is obtained, the separation reactor I temperature is 43-47 DEG C, and preferable temperature is 45 DEG C, and pressure is
11-13Mpa, preferably pressure are 12Mpa;The separation reactor I I temperature is 28-32 DEG C, and preferable temperature is 30 DEG C, pressure 7-
9Mpa, preferably pressure are 8Mpa.
It is 2h to extract as cycling extraction, preferably extraction time 1.8-2.2h, time;CO2Flow is 10-11 l/h, excellent
It is 10.5 l/h to select flow.
4) the Stibene-glucoside crude product dissolves through absolute ethyl alcohol, filters acquisition filtrate, and two are obtained after the filtrate drying
Styrene glycosides finished product.Filtering using macroreticular resin filter, macroreticular resin preferably 101, DM130, S-8, D600, HPD500, II,
One or more in ZTC-1.
Following reference examples closest to the present invention for being the embodiment of the present invention and being filtered out from existing literature, control
It using ethanol is entrainment reagent that example, which is, using supercritical CO2Abstraction technique extracts Stibene-glucoside in the fleece-flower root.Wherein
Reference examples 1 provide only extraction step, not provide separating step, its extraction yield is very low, less than < 1%.What reference examples 2 used
Ethanol is as entrainment reagent, and extraction conditions is different from the present invention, and the extraction yield of acquisition is 4.6%.And in the prior art, almost do not have
There is the report for using ultra-pure water as entrainment reagent, even if there is small part researcher to be attempted, its extraction yield is also very low, much
Less than using extraction yield of the ethanol as entrainment reagent.
And extracting method provided by the invention, it is much smaller than existing skill by the use of ultra-pure water as entrainment reagent, its entrainment reagent dosage
Art dosage, and its extraction yield is higher than reachable as the extraction yield of entrainment reagent, optimal extraction yield by the use of ethanol in the prior art
More than 5.25%, purity is up to 98%.And according to the report of the prior art, the total content of Stibene-glucoside is in the fleece-flower root
5.62%, largely in the prior art, complete extraction, highest extraction can not be all realized to the Stibene-glucoside in the fleece-flower root
Rate that is to say 4.6% reached in reference examples 2, and the present invention overcomes the prejudice of the prior art, reducing entrainment reagent dosage
On the basis of, extraction yield has been brought up to 5.25%, has improved nearly one percentage point, close to Stibene-glucoside in the fleece-flower root
Complete extraction, obtain unexpected advantageous effects.
The present invention also determines the place of production of the fleece-flower root by screening, in several genunie medicinal materials, final definite Sichuan Wanyuan,
Enshi, Ankang, the raw material sources that Tongren district Guizhou Province is the fleece-flower root of the present invention, wherein Sichuan Wanyuan are excellent with enshi
The place of production is selected, Sichuan Wanyuan is the most preferably place of production.
Above-mentioned elaborating for the present invention, is the embodiment of the present invention below.
Embodiment 1
Radix Polygoni Multiflori powder (place of production Sichuan Wanyuan) 500g is taken, entrainment reagent ultra-pure water is added directly in bucket is extracted
100ml, opens supercritical extraction unit, 48 DEG C of extraction kettle and separating still I 43 is separately heated to extraction kettle and two separating stills
DEG C, II 28 DEG C of separating still when, open CO2Gas cylinder, opens 10 l/h of certain C O2 flows, to extraction kettle and two separating still pressurizations
During to 36Mpa, 11Mpa, 7Mpa, extraction is started the cycle over, extracts 1.8h, obtains separation product.Dissolved with absolute ethyl alcohol, use macropore
Resin filters, macroreticular resin D101, filtrate drying, product purity 97%, extraction yield 4.86%.
Embodiment 2
Radix Polygoni Multiflori powder 500g (place of production enshi) is taken, entrainment reagent ultra-pure water is added directly in bucket is extracted
150ml, opens supercritical extraction unit, 52 DEG C of extraction kettle and separating still I 47 is separately heated to extraction kettle and two separating stills
DEG C, II 32 DEG C of separating still when, open CO2Gas cylinder, opens certain C O211 l/h of flow, to extraction kettle and two separating still pressurizations
During to 40Mpa, 13Mpa, 9Mpa, extraction is started the cycle over, extracts 2.2h, obtains separation product.Dissolved with absolute ethyl alcohol, use macropore
Resin filters, macroreticular resin DM130, filtrate drying, product purity 98%, extraction yield 5.14%.
Embodiment 3
Radix Polygoni Multiflori (place of production Sichuan Wanyuan) powder 500g is taken, entrainment reagent ultra-pure water is added directly in bucket is extracted
220ml, opens supercritical extraction unit, 50 DEG C of extraction kettle and separating still I 45 is separately heated to extraction kettle and two separating stills
DEG C, II 30 DEG C of separating still when, open CO2Gas cylinder, opens certain C O210.5 l/h of flow, adds extraction kettle and two separating stills
When being depressed into 38Mpa, 12Mpa, 8Mpa, extraction is started the cycle over, extracts 2h, obtains separation product.Dissolved with absolute ethyl alcohol, use macropore
Resin filters, macroreticular resin S-8, filtrate drying, product purity 98%, extraction yield 5.18%.
Embodiment 4
Radix Polygoni Multiflori powder (place of production Sichuan Wanyuan) 500g is taken, entrainment reagent ultra-pure water is added directly in bucket is extracted
200ml, opens supercritical extraction unit, 50 DEG C of extraction kettle and separating still I 45 is separately heated to extraction kettle and two separating stills
DEG C, II 30 DEG C of separating still when, open CO2Gas cylinder, opens certain C O210.5 l/h of flow, adds extraction kettle and two separating stills
When being depressed into 38Mpa, 12Mpa, 8Mpa, extraction is started the cycle over, extracts 2h, obtains separation product.Dissolved with absolute ethyl alcohol, use macropore
Resin filters, macroreticular resin HPD500, filtrate drying, product purity 98%, extraction yield 5.25%.
Embodiment 5
Radix Polygoni Multiflori (place of production enshi) powder 500g is taken, entrainment reagent ultra-pure water is added directly in bucket is extracted
200ml, opens supercritical extraction unit, 50 DEG C of extraction kettle and separating still I 45 is separately heated to extraction kettle and two separating stills
DEG C, II 30 DEG C of separating still when, open CO2Gas cylinder, opens certain C O210.5 l/h of flow, adds extraction kettle and two separating stills
When being depressed into 38Mpa, 12Mpa, 8Mpa, extraction is started the cycle over, extracts 2h, obtains separation product.Dissolved with absolute ethyl alcohol, use macropore
Resin filters, macroreticular resin ZTC-1, filtrate drying, product purity 98%, extraction yield 5.13%.
Embodiment 6
Radix Polygoni Multiflori (place of production Ankang) powder 500g is taken, entrainment reagent ultra-pure water is added directly in bucket is extracted
200ml, opens supercritical extraction unit, 50 DEG C of extraction kettle and separating still I 45 is separately heated to extraction kettle and two separating stills
DEG C, II 30 DEG C of separating still when, open CO2Gas cylinder, opens certain C O210.5 l/h of flow, adds extraction kettle and two separating stills
When being depressed into 38Mpa, 12Mpa, 8Mpa, extraction is started the cycle over, extracts 2h, obtains separation product.Dissolved with absolute ethyl alcohol, use macropore
Resin filters, macroreticular resin II, filtrate drying, product purity 98%, extraction yield 4.86%.
Embodiment 7
Radix Polygoni Multiflori (place of production Tongren district Guizhou Province) powder 500g is taken, entrainment reagent ultra-pure water is added directly in bucket is extracted
200ml, opens supercritical extraction unit, 50 DEG C of extraction kettle and separating still I 45 is separately heated to extraction kettle and two separating stills
DEG C, II 30 DEG C of separating still when, open CO2Gas cylinder, opens certain C O210.5 l/h of flow, adds extraction kettle and two separating stills
When being depressed into 38Mpa, 12Mpa, 8Mpa, extraction is started the cycle over, extracts certain time 2h, obtains separation product.It is molten with absolute ethyl alcohol
Solution, is filtered, macroreticular resin D101 with macroreticular resin, filtrate drying, product purity 98%, extraction yield 4.97%.
Reference examples 1
In existing literature, using supercritical CO2Abstraction technique, using ethanol as entrainment reagent, extracts hexichol second in the fleece-flower root
The step of alkene glycosides, is as follows:
The fleece-flower root coarse powder 400g of drying and crushing is taken, extracting pressure 40Mpa, 60 DEG C of extraction temperature, extraction time 2h, holds under the arm
With 20% that 95% amount of alcohol of agent is crude drug, after extract drying, using high effective liquid chromatography for measuring, Stibene-glucoside purity
For 6.192mg.g-1。
Above-mentioned document does not carry out separating step, extraction yield < 1%.
Reference examples 2
In existing literature, using supercritical CO2Abstraction technique, using ethanol as entrainment reagent, extracts hexichol second in the fleece-flower root
The step of alkene glycosides, is as follows:
It is in powdered that fleece-flower root addition pulverizer, which crushes, accurately weighs 200g and loads extraction bucket, adds directly in bucket is extracted
Enter entrainment reagent ethanol 150mL.Supercritical extraction unit is opened, extraction kettle and two separating stills are heated respectively, when extraction kettle temperature
When degree reaches 45 DEG C, the temperature of separating still I reaches 45 DEG C, when the temperature of separating still II is 30 DEG C, opens CO2Gas cylinder, extraction kettle
35MPa is forced into, the pressure of separating still I is 15MPa, when the pressure of extraction-container II is 5MPa, starts the cycle over extraction, CO2Flow
For 12.5L/h when, each kettle pressure balance can be kept.After extracting 2.5h, pressure release, stops extraction, opens extraction kettle and separating still bottom
Valve, obtains separation product.Dissolved with ethanol, filtered with macroreticular resin, filtrate is put into vacuum drying chamber dries 3h at room temperature, i.e.,
Obtain product, extraction yield 4.64%.
It the above is only the preferred embodiment of the present invention, it is noted that above-mentioned preferred embodiment is not construed as pair
The limitation of the present invention, protection scope of the present invention should be subject to claim limited range.For the art
For those of ordinary skill, without departing from the spirit and scope of the present invention, some improvements and modifications can also be made, these change
Protection scope of the present invention is also should be regarded as into retouching.
Claims (10)
1. the extracting method of Stibene-glucoside, comprises the following steps in a kind of fleece-flower root:
1) fleece-flower root powder is provided;
2) entrainment reagent is added into fleece-flower root powder, the entrainment reagent is ultra-pure water;
3) fleece-flower root powder is through supercritical CO2Extraction obtains extraction product, and the extraction temperature is 48-52 DEG C, the extracting pressure
For 36Mpa-40Mpa;The extraction product obtains Stibene-glucoside crude product, the separation successively through separation reactor I and separation reactor I I
Kettle I temperature is 43-47 DEG C, pressure 11-13Mpa, and the separation reactor I I temperature is 28-32 DEG C, pressure 7-9Mpa;
4) the Stibene-glucoside crude product dissolves through absolute ethyl alcohol, filters acquisition filtrate, and hexichol second is obtained after the filtrate drying
Alkene glycosides finished product.
2. extracting method according to claim 1, it is characterised in that the preparation method of the step 1) fleece-flower root powder is
The fleece-flower root is dried in the shade, is ground into 6-9 mesh powders.
3. extracting method according to claim 1, it is characterised in that the step 1) fleece-flower root is selected from Sichuan Wanyuan, lake
North is bestowed favour, Ankang, any place of production in Tongren district Guizhou Province.
4. extracting method according to claim 1, it is characterised in that the step 2) entrainment reagent and the weight ratio of the fleece-flower root
For (1.5-2.2):5.
5. extracting method according to claim 1, it is characterised in that the step 3) extraction temperature is 50 DEG C, and pressure is
38Mpa。
6. extracting method according to claim 1, it is characterised in that step 3) is cycling extraction, extraction time 1.8-
2.2h。
7. extracting method according to claim 1, it is characterised in that step 3) the separation reactor I temperature is 45 DEG C, pressure
For 12Mpa.
8. extracting method according to claim 1, it is characterised in that step 3) the separation reactor I I temperature is 30 DEG C, pressure
Power is 8Mpa.
9. extracting method according to claim 1, it is characterised in that CO in step 3)2Flow is 10-11 l/h.
10. extracting method according to claim 1, it is characterised in that step 4) is described to be filtered into using macroreticular resin mistake
Filter.
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CN201711427879.8A CN107903292B (en) | 2017-12-26 | 2017-12-26 | Method for extracting stilbene glucoside from polygonum multiflorum |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110787222A (en) * | 2019-11-19 | 2020-02-14 | 暨南大学 | Extract with anti-aging effect and preparation method and application thereof |
CN114736109A (en) * | 2022-03-02 | 2022-07-12 | 华南理工大学 | A kind of method for selectively extracting stilbene glycosides in Polygonum multiflorum |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS61171427A (en) * | 1985-01-24 | 1986-08-02 | Osaka Chem Lab | Substance for preventing thrombosis or the like |
CN102321129A (en) * | 2011-07-14 | 2012-01-18 | 中国人民解放军第四军医大学 | Stilbene glycoside injection and preparation process thereof |
-
2017
- 2017-12-26 CN CN201711427879.8A patent/CN107903292B/en active Active
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS61171427A (en) * | 1985-01-24 | 1986-08-02 | Osaka Chem Lab | Substance for preventing thrombosis or the like |
CN102321129A (en) * | 2011-07-14 | 2012-01-18 | 中国人民解放军第四军医大学 | Stilbene glycoside injection and preparation process thereof |
Non-Patent Citations (3)
Title |
---|
向文军 等: "二氧化碳超临界萃取何首乌中的二苯乙烯苷的研究", 《应用化工》 * |
吴帧 等: "超临界CO2萃取何首乌中二苯乙烯苷的工艺考察", 《中草药》 * |
张俊娜 等: "何首乌中二苯乙烯苷提取纯化研究进展", 《中国中医药信息杂质》 * |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110787222A (en) * | 2019-11-19 | 2020-02-14 | 暨南大学 | Extract with anti-aging effect and preparation method and application thereof |
CN110787222B (en) * | 2019-11-19 | 2022-03-29 | 暨南大学 | Extract with anti-aging effect and preparation method and application thereof |
CN114736109A (en) * | 2022-03-02 | 2022-07-12 | 华南理工大学 | A kind of method for selectively extracting stilbene glycosides in Polygonum multiflorum |
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