CN106215455B - The new technology of stilbene class material collection purifying in a kind of dendrobium candidum - Google Patents
The new technology of stilbene class material collection purifying in a kind of dendrobium candidum Download PDFInfo
- Publication number
- CN106215455B CN106215455B CN201610464044.9A CN201610464044A CN106215455B CN 106215455 B CN106215455 B CN 106215455B CN 201610464044 A CN201610464044 A CN 201610464044A CN 106215455 B CN106215455 B CN 106215455B
- Authority
- CN
- China
- Prior art keywords
- tank
- extraction
- dendrobium candidum
- extracted
- stilbene class
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active - Reinstated
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/88—Liliopsida (monocotyledons)
- A61K36/898—Orchidaceae (Orchid family)
- A61K36/8984—Dendrobium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/028—Flow sheets
- B01D11/0284—Multistage extraction
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D2011/002—Counter-current extraction
Landscapes
- Health & Medical Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Microbiology (AREA)
- Pharmacology & Pharmacy (AREA)
- Botany (AREA)
- Medical Informatics (AREA)
- Medicinal Chemistry (AREA)
- Alternative & Traditional Medicine (AREA)
- Mycology (AREA)
- Biotechnology (AREA)
- Epidemiology (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Engineering & Computer Science (AREA)
- Extraction Or Liquid Replacement (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
It is related to the new technology of the extraction of stilbene class material, enrichment and purifying in dendrobium candidum the invention discloses a kind of.Stilbene class material is important symbol composition in dendrobium candidum, including luxuriant and rich with fragrance class and bibenzyl.Stilbene class has significant bioactivity, but extraction and purification process not yet effective, easy at present.Based on this, this patent exploitation is a kind of simple, efficiently, and in the dendrobium candidum easily accomplished scale production stilbene class material extraction and purification process.This technique main process is followed successively by petroleum ether degreasing, the extraction of tank assembling dynamic countercurrent ethyl acetate, NaOH alkalization, hydrochloric acid acidification etc..The relatively conventional macroporous resin purification of this method, saves substantial amounts of organic solvent, time, and specificity is strong.Stilbene class material purity is up to 80%.
Description
Technical field
Field is extracted the present invention relates to effective ingredients in plant, it is particularly a kind of using the extraction of tank assembling dynamic countercurrent method, alkali
Stilbene class material extraction and purification process in molten and sour heavy dendrobium candidum.
Background technology
Dendrobium candidum is orchid family Dendrobium herbaceos perennial.The stem of noble dendrobium can be divided into tens of kinds of yellow grass, Jin Chai, horsewhip etc.,
Dendrobium candidum exists《Chinese Pharmacopoeia》Version is recorded within 2015.Dendrobium candidum is medicine-food two-purpose rare species resource.Dendrobium candidum because
Epidermis is gained the name in iron green, is the superfine product of the stem of noble dendrobium, is used as medicine with its stem, and tender stem is dried after being twisted into helical form or spring-like, commodity
Referred to as earrings dendrobium, also known as maple bucket, the yin tonics in category tonic.Therefrom medical angle summarizes ten main big work(of dendrobium candidum
Effect has：1st, yin jin is nourished, 2, build up health, 3, strengthen the spleen and stomach, 4, protect liver cholagogic, 5, strong muscle lipid-loweringing, 6, reduce blood sugar, 7, suppress
Tumour, 8, bright eyes, 9, nourish skin, 10, promote longevity.
Stilbene class material (stilbenoids) is that the natural products with 1,2 1 talan parent nucleus or its polymer is total
Claim.In recent years, substantial amounts of such compound is isolated from stone solution platymiscium, the derivative of predominantly luxuriant and rich with fragrance class and its bibenzyl
Thing.Such substance bioactivity significantly, is acknowledged as the active ingredient in dendrobium candidum.Such as Bibenzyl compound for Dendrobium is planted
The characteristic chemical constituent of thing, with antitumor, anti-platelet aggregation, anti-oxidant isoreactivity.
There is abundant stilbene class material, content is more, species is abundant, bioactivity is strong in dendrobium candidum.But to current, not yet
See that the purifying process on stilbene class material in dendrobium candidum studies report., about content determination, main use includes dipping for it
The conventional methods such as method, percolation, water extraction decocting method, reflux extraction are extracted.These method extraction efficiencies are not high, Er Qiegao
Power consumption, unsuitable large-scale production.Conventional purification methods, it is common to have macroporous resin column chromatography, column chromatography mostly using column chromatography
Enrichment reappearance is not high, and needs to use substantial amounts of organic solvent.With updating and new extraction equipment for technology
Development, more and more advanced extraction separation means are developed, and the present invention is extracted using tank assembling dynamic countercurrent method
Stilbene class material in dendrobium candidum, and according to the chemical structure characteristic of stilbene class material in dendrobium candidum, using the method that alkali soluble acid is heavy
Enriching and purifying is carried out to it.
Pot group type tank assembles dynamic countercurrent extraction process, is, by more than two dynamic extraction pot units connected in series, to extract molten
Agent is inversely sequentially conveyed by each tank from low to high along the solute concentration gradient of each tank spice in tank group, and is kept with spice
Certain extraction time and time use.This technology mainly make use of solid-liquid（Medicinal material and solvent）The concentration ladder of active ingredient in two-phase
Degree is poor, during active ingredient in medicinal material diffused into the relatively low Extraction solvent of initial concentration step by step, reaches and shifts medicinal material to greatest extent
The purpose of middle active ingredient.Using pot group type adverse current extraction process, the concentration gradient of solid-liquid two-phase can be effectively utilized, increased dense
Degree is poor, and extraction rate is fast, and the concentration of extract solution increases, and extracting cycle is short, and filtering layer is made using medicinal material body while extraction, can carry
Clarity high.
The content of the invention
The purpose of the present invention essentially consists in the technique of stilbene class material in exploitation efficiently concentrating purifying dendrobium candidum, using tank group
Formula tank assembles dynamic countercurrent extracting mode, by the concentration difference of extract solution between Rational Arrangement each extraction unit, and to iron
The factors such as skin stem of noble dendrobium medicinal material extract time, Extraction solvent, solid-liquid ratio it is preferred, finally realize it is a kind of with few solvent of trying one's best, when
Between, energy consumption extract the practicable embodiment of stilbene class material in dendrobium candidum to greatest extent；Using decolorizing with activated carbon and
The carrying out purifying of " alkali soluble acid is heavy " is refined.
To achieve the goal, present invention process step includes：（1）Petroleum ether degreasing：Dendrobium candidum medicinal powder is weighed, is used
Petroleum ether backflow carries out degreasing；（2）Ethyl acetate is extracted：By by the dendrobium candidum dregs of a decoction after petroleum ether degreasing, using tank group
Formula tank assembling dynamic countercurrent round-robin method is extracted；（3）Buck treatment：Stilbene class material in extract solution is converted into water solubility
Alkali salt；（4）Removal of impurities：The method removal of impurities that hydrolyzate is passed through into decolorizing with activated carbon；（5）Sour water is neutralized：Buck after decolouring is molten
Liquid is neutralized with sour water, and filtering to precipitate；（6）Vacuum drying, dissolving, its content is surveyed using ultraviolet specrophotometer.
Wherein, technique content is as follows：
（1）Degreasing：Dendrobium candidum powder is weighed, 10 times of amount petroleum ethers are added, flowed back 5 hours；
（2）Extract：By the dendrobium candidum dregs of a decoction after degreasing, 10 times of amount ethyl acetate are added to make Extraction solvent, using tank group
Formula tank assembling dynamic countercurrent mode is extracted, and is concentrated, and is obtained ethyl acetate and is extracted medicinal extract, is weighed, standby；
（3）Buck treatment：：With medicinal extract and sodium hydroxide solution mass volume ratio 1g:15-25ml, adds 0.1mol/L hydrogen
Sodium hydroxide solution, be fully suspended ethyl acetate extract, stirring reaction 3 hours；
（4）Centrifugation, 3000r/min rotating speeds obtain supernatant；
（5）Removal of impurities：Toward step（4）In supernatant in add activated carbon, stirring is allowed to be fully contacted, and stirs 1-2 hours,
3-24 hours is stood, the centrifugation of 3000r/min rotating speeds takes supernatant, and residue is concentrated to give medicinal extract；
（6）Sour water is neutralized：Toward the alkali lye after decolorization and impurity removal by active carbon, neutralized using the hydrochloric acid solution of 0.1mol/L, plus
It is 1.5-2 times of alkali lye volume to enter hydrochloric acid solution volume, is sufficiently stirred for, and is stood, and obtains white flock precipitate；
（7）Centrifugation, abandons supernatant, must precipitate, and cleaned twice with distilled water；
（8）Vacuum drying, measures stilbene class content of material.
Extract flow：First with low polar solvent in the first tank degreasing, after degreasing three times, successively according to following extraction side
Formula, is one group with 3 tanks, circulates extraction 3 times successively per tank, and its step is：First, dendrobium candidum medicinal powder is put into the first tank,
By the use of low polar solvent as degreasing solvent, tank assembling dynamic countercurrent degreasing, the liquid mistake that the first tank is extracted for the first time are carried out
Fluid reservoir is put into after filter, second liquid of extraction stores up medical filtration after extraction as the solvent of the second tank extraction for the first time
Standby, the solvent that the liquid that third time is extracted is extracted for second as the second tank extracts gained liquid as the 3rd tank first time
Extraction solvent, i.e., extract the extract solution that institute's solubilizer is a tank the N+1 time per tank n-th, the extraction when institute for the third time per tank
Solubilizer is neat solvent, after the first tank medicinal material is extracted through three times, discharges the dregs of a decoction, puts into new medicinal material, adds the 3rd tank secondary
Extract solution carries out first time extraction, as the tail tank that tank group next round circulation is extracted, each step as stated above later
Secondary circulation.
The technological parameter of extraction is：It is molten as extracting that ethyl acetate is measured in 6-10 times of first tank medicinal material extraction addition for the first time
Agent, second, be separately added into 3-6 times three times and measure ethyl acetate；Medicinal material after first tank degreasing is put into the second tank, and past second
6-10 times is added to measure ethyl acetate in tank, the 3rd tank medicinal material is supplemented respectively on the basis of being extracted in the upper tank liquid of addition for the first time
1-3 times is measured ethyl acetate；Extracted altogether 3 times per tank medicinal material, each extraction time is 0.5-2 hours；Extracting temperature is 80 DEG C；It is dynamic
The stirring frequency that state is extracted is 20-200 revs/min, is realized by motor-driven mechanical agitation, makes the interior temperature everywhere of extractor
Increase the contact area of material and solvent while consistent, improve recovery rate.
Wherein, low polar solvent is in petroleum ether, hexamethylene, ether described in described tank assembling dynamic countercurrent extraction
It is a kind of.
Wherein, the buck is 0.1 mol/L NaOH or 0.1 mol/L potassium hydroxide solutions.
Wherein, the sour water is 0.1 mol/L hydrochloric acid or 0.1 mol/L phosphoric acid.
Advantages of the present invention has the following aspects：
1st, extracted using pot group type tank assembling dynamic countercurrent and instead of traditional single-pot and repeatedly extract, it is ensured that between tank group compared with
Big active ingredient concentration difference, considerably increases extraction motive force, accelerates extraction rate；Pot group type is extracted by the anti-of solvent
It is multiple to utilize, the concentration of active ingredient in final solvent is improve, reduce subsequent concentration power consumption.Additionally, per tank medicinal material for the last time
Extraction add neat solvent, can effectively control the content of stilbene class material in the dregs of a decoction, it is ensured that in dendrobium candidum stilbene class material by defecation,
Have the advantages that effective component extraction rate is high.Through experiment, compared with traditional extraction process, the present invention can make post processing extraction solvent consumption
45% is at least reduced, corresponding saving heat energy about 60%, recovery rate improves 60%, and with the increase of tank group number, this advantage heals
Plus substantially；
2nd, traditional static extraction instead of using stirring-type Dynamic Extraction, it is possible to prevente effectively from dendrobium candidum powder is viscous
Pot gelatinization.Additionally, Dynamic Extraction improves diffusion of the active ingredient from medicinal material surface to solvent, Fast-Balance is realized, shortening is carried
Take the time；
3rd, neutralized by highly basic salt-forming reaction and acid, be greatly improved the extraction efficiency of stilbene class material in dendrobium candidum.Should
Purge process mild condition, economical and efficient, and it is particularly suitable for large-scale production；
4th, this law carries out assay using ultraviolet spectrophotometry, and required equipment is simple；
5th, the stilbene class content of material for obtaining is up to 80%.
Brief description of the drawings
Fig. 1 is present invention process flow chart
Specific embodiment
Embodiment 1：
Take and dry dendrobium candidum medicinal material, crush, cross 60 mesh sieves, weigh 200g, dendrobium candidum powder is put in extractor, the
One tank medicinal material extracts add 10 times of amount petroleum ether degreasings for the first time, flows back 5 hours, after twice of degreasing, after the first tank degreasing
Medicinal material is divided into three parts, is respectively put into first, second and third tank, and 8 times of ethyl acetate is separately added into three tanks, carry for the first time
Take, second, extract for three times and be separately added into 5 times of amount ethyl acetate, the liquid that the second tank is extracted for second is used as the 3rd tank first
The solvent of secondary extraction, lays in medical filtration after extraction, the solvent that the liquid that third time is extracted is extracted for second as the second tank,
The extract solution that institute's solubilizer is a tank the N+1 time is extracted per tank n-th, third time extraction when institute's solubilizer is pure per tank
Solvent.After first tank medicinal material is extracted through three times, the dregs of a decoction are discharged, the 3rd tank is added as the new medicinal material of the second tank, then in the second tank
Secondary extract solution carries out first time extraction, and used as the tail tank that tank group next round circulation is extracted, each step is by upper later
State method one cycle.Extracted altogether 3 times per tank medicinal material, each extraction time is 1.5 hours, obtains CE 19.8g；By crude extract
Fully it is suspended with the 0.1mol/L sodium hydroxide solutions of 300ml, active carbon powder is added 0.1mol/L by stirring reaction 3 hours
In sodium hydroxide solution, continue to stir fully absorption 3 hours, the addition of activated carbon is 8 times of W/V of material, after stirring terminates,
Place 24 hours, suction strainer upper clear supernate, then washed with 6 times of amount clear water, be centrifuged or suction strainer, merge clear liquid；1.5 are added toward filtrate
0.1mol/L hydrochloric acid solutions again, are sufficiently stirred for reaction, and after stirring 1 hour, 3000 rpms are centrifuged 10 minutes；The stilbene for obtaining
Class enriched substance 3.18g.
Embodiment 2
Take and dry dendrobium candidum medicinal material, crush, cross 60 mesh sieves, weigh 100g, dendrobium candidum powder is put in extractor, the
One tank medicinal material extracts add 10 times of amount petroleum ether degreasings for the first time, after twice of degreasing, the first tank medicinal material is equally divided into three parts, point
In not putting three extractors.6 times of ethyl acetate of amount are separately added into three tanks, first time extraction is carried out, second, three difference
4 times of ethyl acetate of amount are added, second and third tank medicinal material is 1.5 times of amount solvents of supplement on the basis of upper tank liquid；Per tank medicinal material
Extract 3 times altogether, each extraction time is 1.5 hours, obtains CE 9.8g；Crude extract sodium hydroxide solution is fully suspended,
Stirring reaction 3 hours；By in the 0.1mol/L potassium hydroxide solutions of active carbon powder addition 150ml, continue to stir fully absorption 3
Hour, the addition of activated carbon is 8 times of W/V of material, after stirring terminates, is placed 24 hours, suction strainer upper clear supernate, then with 6 times
Amount clear water washing, centrifugation or suction strainer, merge clear liquid, and 2 times of 0.1mol/L phosphoric acid solutions are added toward filtrate, are sufficiently stirred for anti-
Should, after stirring 1 hour, 3000 rpms are centrifuged 10 minutes.The stilbene class enriched substance 1.51g for obtaining.
Embodiment 3
Take and dry dendrobium candidum medicinal material, crush, cross 60 mesh sieves, weigh 100g, dendrobium candidum powder is put into 2 liters of round-bottomed flasks
In, flowed back twice using 10 times of amount petroleum ethers, 90 DEG C of water-baths, it is every all over 3 hours, by medicinal material after petroleum ether degreasing, after suction filtration again extremely
In 2 liters of round-bottomed flasks, 600mL ethyl acetate is added, 90 DEG C of water-bath refluxing extractions 3 times 3 hours every time, obtain 6.8 grams of CE；
Crude extract is fully suspended with 0.05mol/L sodium hydroxide solutions, stirring reaction 3 hours；Active carbon powder is added into hydroxide
In sodium solution, continue to stir fully absorption 3 hours, the addition of activated carbon is 8 times of W/V of material, after stirring terminates, places 24
Hour, suction strainer upper clear supernate, then washed with 6 times of amount clear water, it is centrifuged or suction strainer, merge clear liquid.Added toward filtrate excessive
0.1mol/L hydrochloric acid solutions, are sufficiently stirred for reaction, and after stirring 1 hour, 3000 rpms are centrifuged 10 minutes.The stilbene class for obtaining is rich
Collection thing 1.01g.
Embodiment 4
Take and dry dendrobium candidum medicinal material, crush, cross 60 mesh sieves, weigh 100g, dendrobium candidum powder is put in extractor, the
One tank medicinal material extracts add 7 times of amount petroleum ether degreasings, after degreasing 1 time, the first tank medicinal material is equally divided into three parts, respectively for the first time
Put in three extractors, 11 times of ethyl acetate of amount are separately added into three tanks, carry out first time extraction, second, three difference
11 times of ethyl acetate of amount are added, second and third tank medicinal material is 3.5 times of amount solvents of supplement on the basis of upper tank liquid；Per tank medicine
Material is extracted 2 times altogether, and each extraction time is 0.5 hour, obtains CE 5.8g；Crude extract is fully mixed with sodium hydroxide solution
It is outstanding, stirring reaction 3 hours；Active carbon powder is added in the sodium hydroxide solution of 0.1mol/L of 100ml, continue to stir abundant
Absorption 3 hours, the addition of activated carbon is 4 times of W/V of material, after stirring terminates, is placed 24 hours, suction strainer upper clear supernate, then
Washed with 6 times of amount clear water, be centrifuged or suction strainer, merge clear liquid, 1.5 times of 0.1mol/L hydrochloric acid solutions of amount are added toward filtrate, filled
Divide stirring reaction, after stirring 1 hour, 3000 rpms are centrifuged 10 minutes, the stilbene class enriched substance 0.51g for obtaining.
Above-described embodiment 1 and embodiment 2 are the inventive method, and embodiment 3 is using the i.e. non-tank group of traditional reflow method
Dress extracting method, the technique that uses of embodiment 4 is for outside for present invention process parameter area.Must be measured and can be known by stilbene class material,
Embodiment 1 and embodiment 2 must be measured and exceed embodiment 3 and embodiment 4.Wherein, embodiment 3 by contrast, highly energy-consuming, and second
Acetoacetic ester consumption is big.The stilbene class material of embodiment 4 must be measured far fewer than embodiment 1 and embodiment 2.
Claims (7)
1. the technique that stilbene class material collection is purified in a kind of dendrobium candidum, it is characterised in that：Comprise the steps of：（1）Petroleum ether
Degreasing：Dendrobium candidum medicinal powder is weighed, degreasing is carried out using petroleum ether backflow；（2）Ethyl acetate is extracted：Will be by petroleum ether
The dendrobium candidum dregs of a decoction after degreasing, are extracted using tank assembling dynamic countercurrent round-robin method；（3）Buck treatment：By extract solution
In stilbene class material be converted into water miscible alkali salt；（4）Removal of impurities：The method removal of impurities that hydrolyzate is passed through into decolorizing with activated carbon；（5）Acid
Water is neutralized：Aqueous alkali after decolouring is neutralized with sour water, filtering to precipitate；（6）Vacuum drying, dissolving, using ultraviolet spectrometry
Luminosity measures its content.
2. the technique that stilbene class material collection is purified in a kind of dendrobium candidum according to claim 1, it is characterised in that：Technique
Content is as follows:
（1）Degreasing：Dendrobium candidum powder is weighed, 10 times of amount petroleum ethers are added, flowed back 5 hours；
（2）Extract：By the dendrobium candidum dregs of a decoction after degreasing, 10 times of amount ethyl acetate are added to make Extraction solvent, it is dynamic using tank assembling
State reflux type is extracted, concentration, is obtained ethyl acetate and is extracted medicinal extract, is weighed, standby；
（3）Buck treatment：With medicinal extract and sodium hydroxide solution mass volume ratio 1g:15-25ml, adds 0.1mol/L NaOH
Solution, be fully suspended ethyl acetate extract, stirring reaction 3 hours；
（4）Centrifugation, rotating speed is 3000r/min, obtains supernatant；
（5）Removal of impurities：Toward step（4）In supernatant in add activated carbon, stirring is allowed to be fully contacted, and stirs 1-2 hour, standing
3-24 hours, the centrifugation of 3000r/min rotating speeds took supernatant, and residue is concentrated to give medicinal extract；
（6）Sour water is neutralized：Toward the alkali lye after decolorization and impurity removal by active carbon, neutralized using the hydrochloric acid solution of 0.1mol/L, add salt
Acid solution volume is 1.5-2 times of alkali lye volume, is sufficiently stirred for, and is stood, and obtains white flock precipitate；
（7）Centrifugation, abandons supernatant, must precipitate, and cleaned twice with distilled water；
（8）Vacuum drying, measures stilbene class content of material.
3. the technique that stilbene class material collection is purified in a kind of dendrobium candidum according to claim 2, it is characterised in that：It is described
Tank assembling dynamic countercurrent extracting mode be：The extraction is one group with 3 tanks, circulates extraction 3 times successively per tank, and its step is：It is first
First, dendrobium candidum medicinal powder is put into the first tank, by the use of low polar solvent as degreasing solvent, carries out tank assembling dynamic countercurrent and take off
Fat；Medicinal material after first tank degreasing is divided into three parts, first, second and third tank, the liquid that the second tank is extracted for second is respectively put into
As the solvent that the 3rd tank is extracted for the first time, medical filtration is laid in after extraction, the liquid that third time is extracted is used as the 3rd tank the
The solvent of second extraction, i.e., extract the extract solution that institute's solubilizer is a tank the N+1 time per tank n-th, and often tank third time is carried
Institute's solubilizer is neat solvent when taking, and after the first tank medicinal material is extracted through three times, discharges the dregs of a decoction, puts into new medicinal material, adds the 3rd tank the
Secondary extract solution carries out first time extraction, and used as the tail tank that tank group next round circulation is extracted, each step is by above-mentioned later
Method one cycle.
4. the technique that stilbene class material collection is purified in a kind of dendrobium candidum according to claim 2, it is characterised in that：It is described
Tank assembling dynamic countercurrent Extraction technique be：First tank medicinal material extracts add 6-10 times to measure ethyl acetate as carrying for the first time
Solvent is taken, second, be separately added into 3-6 times three times and measure ethyl acetate；Medicinal material after first tank degreasing is put into the second tank, and it is past
6-10 times is added to measure ethyl acetate in second tank, the 3rd tank medicinal material is distinguished on the basis of being extracted in the upper tank liquid of addition for the first time
1-3 times of supplement measures ethyl acetate solvent；Extracted altogether 3 times per tank medicinal material, each extraction time is 0.5-2 hours；Extracting temperature
It is 80 °C；The stirring frequency of Dynamic Extraction is 20-200 revs/min.
5. the technique that stilbene class material collection is purified in a kind of dendrobium candidum according to claim 3, it is characterised in that：It is described
Tank assembling dynamic countercurrent extract described in low polar solvent be petroleum ether, hexamethylene, ether in one kind.
6. the technique that stilbene class material collection is purified in a kind of dendrobium candidum according to claim 1, it is characterised in that：It is described
Buck is 0.1 mol/L NaOH or 0.1 mol/L potassium hydroxide solutions.
7. the technique that stilbene class material collection is purified in a kind of dendrobium candidum according to claim 1, it is characterised in that：It is described
Sour water is 0.1 mol/L hydrochloric acid or 0.1 mol/L phosphoric acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610464044.9A CN106215455B (en) | 2016-06-23 | 2016-06-23 | The new technology of stilbene class material collection purifying in a kind of dendrobium candidum |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610464044.9A CN106215455B (en) | 2016-06-23 | 2016-06-23 | The new technology of stilbene class material collection purifying in a kind of dendrobium candidum |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106215455A CN106215455A (en) | 2016-12-14 |
| CN106215455B true CN106215455B (en) | 2017-05-31 |
Family
ID=57519076
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610464044.9A Active - Reinstated CN106215455B (en) | 2016-06-23 | 2016-06-23 | The new technology of stilbene class material collection purifying in a kind of dendrobium candidum |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106215455B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110037335A (en) * | 2019-03-20 | 2019-07-23 | 福建绿色黄金生物科技有限公司 | A kind of processing method and its application of dendrobium candidum |
| CN110724121B (en) * | 2019-12-17 | 2020-06-09 | 江西中医药大学 | Bibenzyl derivative in dendrobium officinale leaf and preparation method and application thereof |
| CN111228407A (en) * | 2020-02-21 | 2020-06-05 | 沈阳药科大学 | Dendrobium officinale extract containing total phenanthrene compounds as well as preparation method and application thereof |
| CN113713046A (en) * | 2021-05-25 | 2021-11-30 | 中国热带农业科学院热带生物技术研究所 | Extract of Dendrobium candidum and application of two chemical components thereof as anti-inflammatory preparation |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2183765Y (en) * | 1993-06-23 | 1994-11-30 | 赵履祥 | Screwed reverse flow extraction tank |
| CN1533801A (en) * | 2003-03-31 | 2004-10-06 | 深圳康泰生物制品股份有限公司 | Golden hairpin dendrobium extract and its medicinal composition |
| CN101015649A (en) * | 2006-11-23 | 2007-08-15 | 天津市轩宏医药技术有限公司 | Dendrobium candidum polysaccharide extractive, medicine composition thereof and its preparation and use |
| CN102274138A (en) * | 2010-06-11 | 2011-12-14 | 上海家化联合股份有限公司 | Dendrobe extract and preparation method and application thereof |
| CN104258106A (en) * | 2014-10-14 | 2015-01-07 | 宁波枫康生物科技有限公司 | Preparation method of effective part of dendrobium officinale |
| KR101593061B1 (en) * | 2008-07-22 | 2016-02-11 | 롱-춘 우 | Polysaccharides extract from dendrobium for treating allergic diseases |
-
2016
- 2016-06-23 CN CN201610464044.9A patent/CN106215455B/en active Active - Reinstated
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2183765Y (en) * | 1993-06-23 | 1994-11-30 | 赵履祥 | Screwed reverse flow extraction tank |
| CN1533801A (en) * | 2003-03-31 | 2004-10-06 | 深圳康泰生物制品股份有限公司 | Golden hairpin dendrobium extract and its medicinal composition |
| CN101015649A (en) * | 2006-11-23 | 2007-08-15 | 天津市轩宏医药技术有限公司 | Dendrobium candidum polysaccharide extractive, medicine composition thereof and its preparation and use |
| KR101593061B1 (en) * | 2008-07-22 | 2016-02-11 | 롱-춘 우 | Polysaccharides extract from dendrobium for treating allergic diseases |
| CN102274138A (en) * | 2010-06-11 | 2011-12-14 | 上海家化联合股份有限公司 | Dendrobe extract and preparation method and application thereof |
| CN104258106A (en) * | 2014-10-14 | 2015-01-07 | 宁波枫康生物科技有限公司 | Preparation method of effective part of dendrobium officinale |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106215455A (en) | 2016-12-14 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106215455B (en) | The new technology of stilbene class material collection purifying in a kind of dendrobium candidum | |
| CN103059075B (en) | A kind of production method of separation and purification rhodioside from Root of Kirilow Rhodiola | |
| CN104140471B (en) | A kind of method preparing Rhizoma Dioscoreae high-purity polysaccharide from yam food processing fent | |
| CN102675139A (en) | Method for extracting ceramide from konjak flying powder | |
| CN103044566A (en) | Method for preparing antioxidant polysaccharide from dictyophora indusiata aqueous extract residues | |
| CN1313479C (en) | Method for preparing holothurin from waste solution of sea cucumber processing | |
| CN100465176C (en) | Method for extracting cantharidin | |
| CN103709211A (en) | Method for preparing glucoraphanin from broccoli | |
| CN106220480B (en) | The technique that tank assembling dynamic countercurrent extracts dendrophnol in dendrobium candidum | |
| CN106279462B (en) | The preparation method of the extracting method of astragalus polyose and astragalus polysaccharides oral liquid for animals | |
| CN102352119A (en) | Method for preparing natural edible coloring agent | |
| CN108485530B (en) | Production process and equipment of food-grade rosin | |
| CN101357192A (en) | Separation preparation method of gastrodia elata crude polysaccharide and gastrodia elata alcohol extract using fresh gastrodia elata as raw material | |
| CN102311509A (en) | Extracting method of sweet potato stem leaf polysaccharide | |
| CN104945532B (en) | The preparation method of Gynura divaricata polysaccharide | |
| CN104398619B (en) | Fevervine extract and application thereof | |
| CN103695157B (en) | A kind of Health-care sesame oil with ease constipation effect of enriching blood | |
| CN1332010C (en) | Preparation and purification method for plant linoleic acid | |
| CN105906738B (en) | The method of separating polyose is extracted in a kind of cockscomb | |
| CN106811303A (en) | A kind of method that gingko episperm extracts essential oil and pectin simultaneously | |
| CN109984314A (en) | A kind of full ingredient instant powder of jujube and its extracting method | |
| CN108264576A (en) | The method for extracting water shield active material | |
| CN107982310A (en) | The preparation method of compound kudzu root flavones preparation | |
| CN104004108B (en) | A kind of enzymolysis is prepared the method for cynomorium songaricum polysaccharide | |
| CN106518653A (en) | Membrane extraction process for hydroxycitric acid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB03 | Change of inventor or designer information |
Inventor after: Huang Lili Inventor after: Wang Guoxin Inventor after: Chen Jinlong Inventor after: Zhu Peilin Inventor after: He Bin Inventor after: Song Xihong Inventor before: Huang Lili Inventor before: Chen Jinlong Inventor before: Zhu Peilin Inventor before: Wang Guoxin Inventor before: He Bin Inventor before: Song Xihong |
|
| COR | Change of bibliographic data | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20170531 Termination date: 20190623 |
|
| RR01 | Reinstatement of patent right | ||
| RR01 | Reinstatement of patent right |
Former decision: termination of patent right due to unpaid annual fee Former decision publication date: 20200623 |