CN106220480B - The technique that tank assembling dynamic countercurrent extracts dendrophnol in dendrobium candidum - Google Patents
The technique that tank assembling dynamic countercurrent extracts dendrophnol in dendrobium candidum Download PDFInfo
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- CN106220480B CN106220480B CN201610480595.4A CN201610480595A CN106220480B CN 106220480 B CN106220480 B CN 106220480B CN 201610480595 A CN201610480595 A CN 201610480595A CN 106220480 B CN106220480 B CN 106220480B
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- C07—ORGANIC CHEMISTRY
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- 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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- 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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- 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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- 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
- C07C41/44—Separation; Purification; Stabilisation; Use of additives by treatments giving rise to a chemical modification
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Abstract
The invention discloses the new technology of a kind of extraction for being related to dendrophnol in dendrobium candidum, enrichment and purifying；The dregs of a decoction after dendrobium candidum extracts polysaccharide processed through water; due to wherein there remains mass efficient composition such as dendrophnol; in order to efficiently using the dendrobium candidum dregs of a decoction after polysaccharide processed, this patent exploitation is a kind of simple, efficiently, and in the dendrobium candidum easily accomplished scale production dendrophnol extraction and purification process；This technique main process has tank to assemble the extraction of dynamic countercurrent ethyl acetate, NaCO3Alkalization, CO2Acidification, RP C18 column chromatographies are purified, recrystallized repeatedly；This method takes full advantage of the dendrobium candidum extracted after polysaccharide, and the simple extraction efficiency of technique, and plenty of time and organic solvent are saved compared with traditional handicraft；The dendrophnol high purity 98% obtained by this technique.
Description
Technical field
Field is extracted the present invention relates to effective ingredients in plant, it is particularly a kind of that iron sheet is extracted using tank assembling dynamic countercurrent method
The technique of dendrophnol in the stem of noble dendrobium.
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, tender stem is dried after being twisted into helical form or spring-like, commodity
Yin tonics in referred to as earrings dendrobium, also known as maple bucket, 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, strengthening tendons lipid-loweringing, 6, reduction blood glucose, 7, suppress
Tumour, 8, bright eyes, 9, nourish skin, 10, promote longevity.
Polyoses content is general between 20-30% in dendrobium candidum, and its polysaccharide component is with strengthening human body immune function, resisting and swell
The pharmacological action such as knurl, anti-aging, antifatigue, hypoglycemic has close ties.Not only have in dendrobium candidum abundant polysaccharide into
Divide by antioxidation or the enhancing indirect antitumor action of Immune Function, also with direct anti-cancer active matter
Basis is its luxuriant and rich with fragrance class for containing and Bibenzyl compound, and there are shadow cell cycle and cyclin expression to tumour cell
Ring, be suppressed the propagation of cancer cell.
Especially at present, the polysaccharide that many products are concentrated in exploitation dendrobium candidum, for extracting the dregs of a decoction after polysaccharide, still not
Abundant, reasonable, effectively efficient utilize can be obtained.The present invention is directed to the dendrobium candidum dregs of a decoction after Polyose extraction, to therein
The effective small molecule of effective bibenzyl-dendrophnol carries out efficiently concentrating and purifying.
Wherein ((4- (3- hydroxy-5-methyl epoxides phenethyl) -2- metoxyphenols) has anti-Bibenzyl compound dendrophnol
Mutagenic activity, can block by the expression of lipopolysaccharide-induced nitric oxide synthase type and cyclooxygenase-2.According to another research table
Bright dendrophnol is the active ingredient of anti-cataract in the stem of noble dendrobium, and it can effectively suppress AR (aldose reductase), improves diabetic
Polyalcohol metabolic pathway is abnormal, the occurrence and development of prevention and delay diabetes and its complication cataract.
At present, there is not yet on dendrophnol enriching and purifying technical study report, it is main using bag about content determination
The conventional methods such as infusion process, percolation, water extraction decocting method, reflux extraction are included to be extracted.With technology update with
And the development of new extraction equipment, more and more advanced extraction separation means are developed, of the invention dynamic using tank assembling
Dendrophnol in the dendrobium candidum that state counter-current is extracted.
Pot group type tank assembles dynamic countercurrent extraction process, is, by more than two dynamic extraction pot units connected in series, to extract molten
Inversely sequentially conveying is kept solute concentration gradient of the agent along each tank spice in tank group by each tank, and with spice from low to high
Certain extraction time and time use.This technology mainly make use of the concentration ladder of active ingredient in solid-liquid (medicinal material and solvent) two-phase
Degree is poor, step by step diffuses in the relatively low Extraction solvent of initial concentration active ingredient in medicinal material, reaches and shift 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, is 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
High clarity.
The content of the invention
The purpose of the present invention essentially consists in the technique of dendrophnol in exploitation efficiently concentrating purifying dendrobium candidum, using pot group type
Tank assembles dynamic countercurrent extracting mode, by the concentration difference of extract solution between Rational Arrangement each extraction unit, and to iron sheet
The factors such as 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, the time,
Energy consumption extracts the practicable embodiment of dendrophnol in dendrobium candidum to greatest extent.Using decolorizing with activated carbon, macropore tree
Fat is adsorbed to be refined with the modern separation means of extracting such as positive column chromatography and recrystallization to dendrophnol progress purifying.
To achieve the goal, present invention process step includes：
(1) extract：By the dendrobium candidum dregs of a decoction after degreasing, 10 times of acetic acid second that volume is dendrobium candidum dregs of a decoction quality are added
Ester makees Extraction solvent, is extracted using pot group type tank assembling dynamic countercurrent mode, is concentrated into relative density for 1.10-1.15,
Obtain ethyl acetate and extract medicinal extract, it is standby；
(2) buck is handled：With medicinal extract and unsaturated carbonate solution quality volume ratio 1g:15-25ml, adds saturated sodium carbonate molten
Liquid, stirring reaction is after 2-3 hours, and the centrifugation of 3000r/min rotating speeds obtains supernatant；
(3) removal of impurities：Activated carbon is added into supernatant obtained by step (2), after stirring 1 hour, after standing 3-24 hours, is received
Collect supernatant, it is that 1.10-1.15 obtains medicinal extract that residue is concentrated into relative density；
(4) acid is neutralized：The filling CO 2 gas into supernatant obtained by step (3), with 30mL/min gas flow rates, continuously
Filling CO 2 gas 1-2 hours, obtains white flock precipitate, centrifugation, abandons supernatant, must precipitate, and is cleaned twice with distilled water；
(5) RP-C18 reverse phase silica gels are purified：Precipitation minimum absolute ethyl alcohol is dissolved, concentrated solution is made, for upper anti-phase
Silicon column glue chromatography；Chromatography process includes：1. RP-C18 reverse phase silica gels are pre-processed：Fully soaked using 95% ethanol, then
Using ethanol water gradient elution, 2. loading is adsorbed：After the medicinal extract ethanol aqueous suction filtration containing dendrophnol, above anticipate
Reverse phase silica gel carries out loading absorption；3. after chromatographic elution, loading, first with water, then wash using ethanol-water system as eluent gradient
De-, thin-layered chromatography tracking and monitoring is collected and contains dendrophnol eluent；
(6) refine：Contain dendrophnol eluent by what is be collected into, be recrystallizing repeatedly so as to obtain white crystalline dendrophnol sample
Product.
Extract flow：The extracting mode circulates extraction 3 times per tank successively using 3 tanks as one group, and its step is：First, by iron
Skin stem of noble dendrobium medicinal powder puts the first tank, and tank assembling dynamic countercurrent degreasing is carried out using low polar solvent；After the first tank degreasing
Medicinal material is divided into three parts, is respectively put into second and third tank, and the decoction of second of extraction of the second tank is used as the extraction for the first time of the 3rd tank
Solvent, lays in medical filtration after extraction, the solvent that the decoction that third time is extracted is extracted as the second tank second, i.e., every tank the
N times extract the extract solution that institute solubilizer is a upper tank the N+1 time, and per tank, third time extraction when institute's solubilizer is neat solvent, the
After one tank medicinal material is extracted through three times, the dregs of a decoction are discharged, the 3rd tank are added as the new medicinal material of the second tank, then in the second tank secondary
Extract solution carries out first time extraction, circulates the tail tank extracted as the tank group next round, later each step as stated above one
Secondary circulation.
The specific process parameter of extraction is：First tank medicinal material is extracted for the first time adds 5~10 times of amount Extraction solvents, second
It is secondary, be separately added into for three times 3~6 times amount carry out degreasings；Medicinal material after first tank degreasing is put into the second tank, and toward in the second tank plus
Enter 6~10 times of amount Extraction solvents, the 3rd tank medicinal material supplements 1~3 respectively on the basis of being extracted in the upper tank decoction of addition for the first time
Solvent is measured again；Extracted altogether 3 times per tank medicinal material, each extraction time is 1~2 hour；Extracting temperature is 80 DEG C；Dynamic Extraction
Stirring frequency is 120~200 revs/min, is realized by motor-driven mechanical agitation, makes in extractor temperature everywhere consistent
Increase the contact area of material and solvent simultaneously, improve recovery rate.
Wherein, ethanol-water system can be 20%, 40%, 60%, 80%, 95% in step (5) chromatographic elution.
Wherein, alcohol-water recrystallization system can be 40%, 50%, 60%, 70% in step (6) recrystallization.
The invention has the advantages that：
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；Normal temperature, which is extracted, saves heat energy, shortens
Extracting cycle；Pot group type extracts recycling by solvent, the concentration of active ingredient in final solvent is improved, after reduction
Continuous concentration power consumption.In addition, per tank medicinal material, last time is extracted and adds neat solvent, can effectively control containing for dendrophnol in the dregs of a decoction
Amount, it is ensured that dendrophnol has the advantages that effective component extraction rate is high by defecation in dendrobium candidum.Through experiment, with traditional extraction
Technique is compared, and the present invention can make post processing extraction solvent consumption at least reduce 45%, and corresponding saving heat energy about 60%, recovery rate is improved
20%, and with the increase of tank group number, this advantage is further obvious；
2nd, traditional static extraction is instead of using stirring-type Dynamic Extraction, it is possible to prevente effectively from dendrobium candidum powder is viscous
Pot gelatinization, in addition, Dynamic Extraction improves diffusion of the dendrophnol from medicinal material surface to solvent, realizes Fast-Balance, shortens and extract
Time；
3rd, neutralized and reduced by highly basic salt-forming reaction and acid, be greatly improved the extraction efficiency of dendrophnol in dendrobium candidum；
4th, using alcohol precipitation, decolorizing with activated carbon, RP-C18Silica gel isolates and purifies dendrophnol, and separating effect is preferable, and organic solvent makes
With few, technique is simple, and resin repeats regeneration, cost is low, equipment is simple, small investment, industrial prospect are preferable；
5th, content is obtained using recrystallization technology and is up to 98% dendrophnol sterling.
Brief description of the drawings
Fig. 1 is present invention process flow chart
Embodiment
Embodiment 1
Dry dendrobium candidum medicinal material is taken, is crushed, 60 mesh sieves is crossed, weighs 200g.Dendrobium candidum powder is put in extractor 1.
First tank medicinal material is extracted for the first time adds 10 times of amount petroleum ether degreasings, and after twice of degreasing, the medicinal material after the first tank degreasing is divided equally
For three parts, the ethyl acetate that 8 times of amounts are separately added into first, second and third tank, three tanks is respectively put into, first time extraction is carried out.Second
Secondary, three extractions are separately added into the ethyl acetate of 5 times of amounts, and the decoction of second of extraction of the second tank is used as the extraction for the first time of the 3rd tank
Solvent, medical filtration is laid in after extraction, the decoction that third time is extracted is used as the solvent that the second tank second is extracted, i.e., every tank
N-th extracts the extract solution that institute solubilizer is a upper tank the N+1 time, and per tank, third time extraction when institute's solubilizer is neat solvent.
After first tank medicinal material is extracted through three times, the dregs of a decoction are discharged, the 3rd tank are added as the new medicinal material of the second tank, then in the second tank second
Extract solution carry out first time extraction, the tail tank extracted is circulated as the tank group next round, later each step is as stated above
One cycle.Extracted altogether 3 times per tank medicinal material, each extraction time is 1.5 hours.Obtain coarse extract 19.8g.Add 300ml saturations
Sodium carbonate liquor, stirring reaction 3 hours；Active carbon powder is added in saturated sodium carbonate solution, continues to stir fully absorption 3 small
When, the addition of activated carbon is 8 times of W/V of material.After stirring terminates, place 24 hours, collect supernatant, residue is concentrated
To relative density be 1.13 medicinal extract, carbon dioxide is filled with into supernatant 2 hours, stir 1 hour after, 3000 rpms from
The heart 10 minutes；Dendrophnol enriched substance 3.2g obtained above 5ml ethanol is dissolved, with RP-C pretreated on 3BV/h18Silicon
Glue post carries out adsorbing separation, is first eluted with water, then with water-ethanol system gradient elution, thin-layered chromatography tracing detection collects stone
Dry measure used in former times phenol section eluent, is concentrated under reduced pressure into no alcohol taste, isometric absolute ethyl alcohol is then added inside, make 50% ethanol molten
Liquid, heating makes fully dissolving, is stood after dissolving and separates out crystallization, and recrystallization twice, obtains white crystal, i.e. dendrophnol, surveyed through HPLC
It is 98% to determine product purity, and recovery rate is 0.02%.
Embodiment 2
Dry dendrobium candidum medicinal material is taken, is crushed, 60 mesh sieves is crossed, weighs 100g.Dendrobium candidum powder is put in extractor 1,
First tank medicinal material is extracted for the first time adds 10 times of amount petroleum ether degreasings, and after twice of degreasing, the medicinal material after the first tank degreasing is divided equally
For three parts, the ethyl acetate that 10 times of amounts are separately added into first, second and third tank, three tanks is respectively put into, first time extraction is carried out, the
Secondary, three extractions are separately added into the ethyl acetate of 3 times of amounts, and the decoction of second of extraction of the second tank is carried for the first time as the 3rd tank
The solvent taken, lays in medical filtration after extraction, the solvent that the decoction that third time is extracted is extracted for the second time as the second tank, i.e., every
Tank n-th extracts the extract solution that institute solubilizer is a upper tank the N+1 time, and per tank, third time extraction when institute's solubilizer is pure molten
Agent.After first tank medicinal material is extracted through three times, the dregs of a decoction are discharged, the 3rd tank the is added as the new medicinal material of the second tank, then in the second tank
Secondary extract solution carries out first time extraction, the tail tank extracted is circulated as the tank group next round, later each step is by above-mentioned
Method one cycle.Extracted altogether 3 times per tank medicinal material, each extraction time is 1.5 hours, obtains coarse extract 9.8g, crude extract is used
240ml saturated sodium carbonate solutions are fully suspended, stirring reaction 3 hours；Active carbon powder is added in saturated sodium carbonate solution, after
Continuous stirring is fully adsorbed 3 hours, and the addition of activated carbon is 8 times of W/V of material.After stirring terminates, place 24 hours, on suction strainer
Portion's clear liquid, then washed with 6 times of amount clear water, centrifugation or suction strainer merge clear liquid, carbon dioxide are filled with into filtrate 2 hours, fully stirred
Reaction is mixed, after stirring 1 hour, 3000 rpms centrifuge 10 minutes；By dendrophnol enriched substance 1.56g 5ml obtained above
Ethanol dissolves, with RP-C pretreated on 3BV/h18Silicagel column carries out adsorbing separation, is first eluted with water, then with water-ethanol system
System gradient elution, thin-layered chromatography tracing detection collects dendrophnol section eluent, is concentrated under reduced pressure into no alcohol taste, then inside
Isometric absolute ethyl alcohol is added, 50% ethanol solution is made, heating makes fully dissolving, is stood after dissolving and separates out crystallization, weight
Crystallization twice, obtains white crystal, i.e. dendrophnol, and it is 97% to determine product purity through HPLC, and recovery rate is 0.02%.
Embodiment 3
Dry dendrobium candidum medicinal material is taken, is crushed, 60 mesh sieves is crossed, weighs 100g.Dendrobium candidum powder is put in extractor 1.
Dendrobium candidum powder is put in 2 liters of round-bottomed flasks, flowed back twice using 10 times of amount 90 DEG C of water-baths of petroleum ether, it is every all over 3 hours.By stone
After medicinal material after oily ether degreasing, suction filtration again into 2 liters of round-bottomed flasks, 600mL ethyl acetate, 90 DEG C of water-bath refluxing extractions 3 are added
Time, 3 hours every time.Obtain 6.6 grams of coarse extract.Medicinal extract is suspended in water, successively using petroleum ether, ethyl acetate extraction medicinal extract,
Obtain 4.2 grams of ethyl acetate extract.420 grams of MCI resins are infiltrated 24 hours using methanol, post is filled, uses 3 column volumes (BV)
10% methanol-water balances pillar；4.2 grams of medicinal extract are suspended in 10mL10% methanol-waters, wet method upper prop.Successively using 3BV's
10% methanol-water, 30% methanol-water, 50% methanol-water, 70% methanol-water and 90% methanol water elution, will by thin-layered chromatography
Position concentration containing dendrophnol, obtains enriched substance 1.2g.By ODS reverse-phase chromatographic columns in the enriched substance, successively using the 20% of 2BV
Methanol-water, 40% methanol-water, 60% methanol-water, 80% methanol-water.By thin-layered chromatography tracing detection, collect dendrophnol section and wash
De- liquid, is concentrated under reduced pressure into no alcohol taste, isometric absolute ethyl alcohol is then added inside, make 50% ethanol solution, heats
Make fully dissolving, stood after dissolving and separate out crystallization, recrystallization twice, obtains white crystal, i.e. dendrophnol, it is pure to determine product through HPLC
Spend for 97%, recovery rate is 0.01%.
Embodiment 4
Dry dendrobium candidum medicinal material is taken, is crushed, 60 mesh sieves is crossed, weighs 100g.Dendrobium candidum powder is put in extractor 1,
First tank medicinal material is extracted for the first time adds 5 times of amount petroleum ether degreasings, and after degreasing 1 time, the first tank medicinal material is equally divided into three parts, point
Do not put in three extractors.The ethyl acetate of 11 times of amounts is separately added into three tanks, first time extraction, second, three times points is carried out
Not Jia Ru 7 times of amounts ethyl acetate, second and third tank medicinal material is that 1 times of supplement measures solvent on the basis of upper tank decoction；Per tank medicinal material
Extract 3 times altogether, each extraction time is 1 hour.Coarse extract 7.8g is obtained, crude extract is fully suspended with saturated sodium carbonate solution,
Stirring reaction 3 hours；Active carbon powder is added in saturated sodium carbonate solution, continues to stir fully absorption 3 hours, activated carbon
Addition 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, from
The heart or suction strainer, merge clear liquid, carbon dioxide are filled with into filtrate 2 hours, are sufficiently stirred for reaction, after stirring 1 hour, and 3000 turns every
Minute centrifugation 10 minutes.Dendrophnol enriched substance 1.06g obtained above 5ml ethanol is dissolved, with pretreated on 3BV/h
RP-C18Silicagel column carries out adsorbing separation, is first eluted with water, then with water-ethanol system gradient elution, thin-layered chromatography tracking inspection
Survey, collect dendrophnol section eluent, be concentrated under reduced pressure into no alcohol taste, isometric absolute ethyl alcohol is then added inside, is made
60% ethanol solution, heating makes fully dissolving, is stood after dissolving and separates out crystallization, and recrystallization twice, obtains white crystal, the i.e. stem of noble dendrobium
Phenol, it is 97% to determine product purity through HPLC, and recovery rate is 0.008%.
Above-described embodiment 1 and embodiment 2 are the inventive method, and embodiment 3 is to use traditional reflow method to be non-tank group
Extracting method combination column chromatography is filled, embodiment 4 uses technique for outside for present invention process parameter area.Obtained by dendrophnol
Amount can know that embodiment 1 and the yield of embodiment 2 have exceeded embodiment 3 and embodiment 4.Wherein, embodiment 3 is by contrast, high
Power consumption, and enrichment process is far complicated, consumption organic solvent is more, and yield is low.The stilbene class material of embodiment 4 must be measured far fewer than reality
Apply example 1 and embodiment 2.As can be seen here, there is significant advantage in terms of dendrophnol extraction purification of the present invention.
Claims (1)
1. the technique that tank assembling dynamic countercurrent extracts dendrophnol in dendrobium candidum, it is characterised in that：Comprise the following steps：Take drying
Dendrobium candidum medicinal material, is crushed, and is crossed 60 mesh sieves, is weighed 200g；Dendrobium candidum powder is put in extractor 1；First tank medicinal material first
Secondary extract adds 10 times of amount petroleum ether degreasings, after twice of degreasing, the medicinal material after the first tank degreasing is divided into three parts, is respectively put into
The ethyl acetate of 8 times of amounts is separately added into first, second and third tank, three tanks, first time extraction is carried out；Secondth, three extraction difference
The ethyl acetate of 5 times of amounts is added, the solvent that the decoction that the second tank is extracted for the second time is extracted for the first time as the 3rd tank will after extraction
Medical filtration is laid in, and the decoction that third time is extracted extracts institute's solubilization as the solvent of second of extraction of the second tank per tank n-th
Agent is the extract solution of a upper tank the N+1 times, and it is neat solvent that per tank, third time, which extracts when institute's solubilizer,；First tank medicinal material is through three times
After extraction, the dregs of a decoction are discharged, the secondary extract solution of the 3rd tank is added as the new medicinal material of the second tank, then in the second tank and carries out first
It is secondary to extract, the tail tank extracted is circulated as the tank group next round, later each step is circulated successively as stated above；Per tank medicinal material
Extract 3 times altogether, each extraction time is 1.5 hours；Add 300ml saturated sodium carbonate solutions, stirring reaction 3 hours；By activity
Carbon powder is added in saturated sodium carbonate solution, continues stirring and adsorbing 3 hours, and the addition of activated carbon is 8 times of W/V of material；Stir
Mix after end, place 24 hours, collect supernatant, by residue be concentrated into relative density for 1.13 medicinal extract, into supernatant
It is filled with carbon dioxide 2 hours, after stirring 1 hour, 3000 rpms centrifuge 10 minutes；By dendrophnol enriched substance obtained above
Dissolved with 5ml ethanol, with RP-C pretreated on 3BV/h18Silicagel column carries out adsorbing separation, is first eluted with water, then with water-second
Alcohol system gradient elution, thin-layered chromatography tracing detection collects dendrophnol section eluent, is concentrated under reduced pressure into no alcohol taste, then past
The inside adds isometric absolute ethyl alcohol, makes 50% ethanol solution, dissolves by heating, and is stood after dissolving and separates out crystallization, tied again
Crystalline substance twice, obtains white crystal, i.e. dendrophnol.
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| CN110478437B (en) * | 2019-08-21 | 2021-08-10 | 西华大学 | Dendrobium stem extract and preparation method thereof |
| CN110917297A (en) * | 2019-12-11 | 2020-03-27 | 深圳市兰科植物保护研究中心 | Dendrobium officinale extract with breast cancer resistance and preparation method thereof |
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| CN101407558B (en) * | 2008-11-14 | 2011-02-02 | 浙江大学 | Preparation of Dendrobium nobile polysaccharide extract and use there |
| CN101811939B (en) * | 2010-05-07 | 2013-03-06 | 南昌京林生物科技有限公司 | Process for dynamical countercurrent extraction of resveratrol in giant knotweed |
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