CN106038737B - A kind of method that ultrasonic wave couples extraction Sorbus alnifolia flavones with double-aqueous phase system - Google Patents
A kind of method that ultrasonic wave couples extraction Sorbus alnifolia flavones with double-aqueous phase system Download PDFInfo
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Abstract
The present invention relates to a kind of ultrasonic waves to couple the method for extracting Sorbus alnifolia flavones with double-aqueous phase system, it is characterized in that: specific step is as follows for this method: step 1) Sorbus alnifolia leaf extracting flavonoids and separation, using propyl alcohol-ammonium sulfate aqueous two-phase, phase liquid and lower phase liquid are obtained；Lower phase liquid in step 1) is cooled down, crystallization, filtering, recycles ammonia sulfate crystal by step 2；The finished product that upper phase liquid dehydrated alcohol in step 1) is purified, is concentrated, dried by step 3).This method advantage is that split-phase is rapid, extracts the process integration of separation, improves Flavonoid substances in the concentration and purity of upper phase；Material consumption reduces, and small toxicity, ethyl alcohol and ammonium sulfate are easy to be recycled；And Sorbus alnifolia leaf flavonoid substance recovery is high, production method is simple, is easy to grasp, not affected by environment；It is at low cost, it is suitble to industrialization production.
Description
Technical field
Field is isolated and purified the invention belongs to active ingredient of natural product, is related to a kind of ultrasonic wave and is coupled with double-aqueous phase system
The method for extracting Sorbus alnifolia flavones.
Background technique
Sorbus alnifolia (Sorbus alnifolia) be rosaceae (Rosaceae) Sorbus alnifolia category (Sorbus) plant,
It is distributed in Heilungkiang, Jilin, Liaoning, Henan, Shaanxi etc., is distributed on Qinling Mountains in Shaanxi north and south slope.Tianshan Mountains Sorbus alnifolia plant
In there is strong anti-oxidation, anti-containing the ingredients such as more rich flavones, anthocyanidin, duplex phenol, Heterodendrin and in pharmacological action
Radiation, anticancer and it is relieving cough and asthma the effects of.But the research of the active constituent in relation to Sorbus alnifolia has not been reported at present.
Bi-aqueous extraction technology (Aqueous Two Phase Extraction, ATPE) it is a kind of novel separation
Technology, due to Bi-aqueous extraction technology have it is efficient, mild, easy to operate, be easy amplification, can effectively keep heat-sensitive ingredients
Activity the advantages that be widely used in Separation of Natural Products, biological extraction, pharmacy, food chemistry, separation of metal ion etc.
Field.But because using the biggish polymer of viscosity in traditional polymer-salt double-aqueous phase system, there are at high cost, recycling is difficult,
The disadvantages of being not easy subsequent processing.As that studies Two-phase system deepens continuously, commonly having for high polymer is replaced with inorganic salts
The advantages that machine object double-aqueous phase system is inexpensive with its, less toxic, system is simple, the recycling of solvent and subsequent processing are easy, and by
It is larger in system component polarity, it is particularly suitable for the extraction and purifying of polar substances, makes it possible the industrialization of aqueous two-phase.
Currently, traditional extracting flavonoids method has water boiling method, organic solvent reflux, soxhlet extraction seeps deer method etc., these
All there is low extraction efficiency, time-consuming, energy consumption, heat-sensitive ingredients the disadvantages of easily decomposing in method.In recent years, and new method such as enzyme occurs
Method extraction, microwave method etc..Enzyme process mild condition, recovery rate are higher, but the time is longer, and extraction efficiency is not high.Microwave method is due to right
The broken wall of plant cell is very capable, and it is efficient, energy saving, time saving the advantages that be widely used in the extraction of effective component,
But heat-sensitive ingredients are destroyed larger.
Ultrasonic wave is a kind of elastic wave, it can generate and transmit powerful energy.Excusing from death wave technology is greatly improved extraction
Rate and extraction rate are ultrasonic effect, cavitation effect since ultrasonic wave has a series of mechanics, calorifics, electromagnetism and chemistry
It answers, fuel factor and chemical effect etc..Wherein the cavitation effect of ultrasonic wave promotes solvent greatly to penetrate into cell, is vibrating
In when being in rarefaction state, ultrasonic wave penetrates in plant tissue cell than electromagnetic wave deeper, and the residence time is also longer, improves object
The transmission speed of matter；And its second order effect such as mechanical effect, mechanical oscillation, emulsification, spread, smash can with chemical effect etc.
Make cell wall rupture and accelerates the diffusion and release of effective components in plants.Immersed effective component is living in the moment biology that is broken
Property remain unchanged, while improving broken speed and recovery rate.Ultrasonic wave can generate solubilization and be widely used in effectively at
The reinforcing divided is extracted, and has many advantages, such as that at low cost, equipment is simple, operation is easy, recovery rate is high.
Summary of the invention
In view of the deficiencies of the prior art, it is an object of the present invention to provide a kind of ultrasonic waves to couple extraction water with double-aqueous phase system
The method of elm Sorbus alnifloria flavones, this method not only promote the intersecting of extraction and isolation technics, infiltration and merge, effectively improve
Extract with isolated efficiency, and also avoid the use of toxic solvent and heat-sensitive ingredients are decomposed, and can be by the Huang in crude extract
The separation of the impurity such as ketone and hydrophilic polysaccharide, protein, achievees the purpose that purification of flavone and separates impurity.This method is at low cost
It is honest and clean, it is easy to operate；Meanwhile also compensating for the insufficient problem of Sorbus alnifolia study of active components.
Technical solution of the present invention: a kind of method that ultrasonic wave couples extraction Sorbus alnifolia flavones with double-aqueous phase system,
Be characterized in: specific step is as follows for this method:
Step 1) Sorbus alnifolia leaf extracting flavonoids and separation obtain phase liquid and lower phase using propyl alcohol-ammonium sulfate aqueous two-phase
Liquid；
Lower phase liquid in step 1) is cooled down, crystallization, filtering, recycles ammonia sulfate crystal by step 2；
The finished product that upper phase liquid dehydrated alcohol in step 1) is purified, is concentrated, dried by step 3).
The step 1) Sorbus alnifolia leaf extracting flavonoids and separation: fresh Sorbus alnifolia leaf is dried, and is crushed；First use sulfuric acid
Ammonium 4.50-6.00g, propyl alcohol 6mL-7mL, water 10mL form stable double-aqueous phase system, and water elm is added in double-aqueous phase system
Chinese catalpa leaf 0.5-0.7g carries out ultrasonic wave extraction 20-40min at power 300W, temperature 50 C, filters, and removes Sorbus alnifolia slag,
Filtrate stands 1-3h, is layered as phase liquid and lower phase liquid, while hot separates upper phase liquid and lower phase liquid, obtains phase liquid and lower phase
Liquid.
The step 3) is by the upper phase liquid dehydrated alcohol purifying in step 1), concentration, dry finished product: upper phase liquid is added
After the dehydrated alcohol precipitating of 3-5 times of volume removes ammonium sulfate residual impurities, ethyl alcohol is recycled, at 60 DEG C -70 DEG C after upper phase liquid concentration
Lower vacuum drying both obtains Sorbus alnifolia leaf flavones finished product.
The upper phase liquid of the step 1) and lower phase liquid are by being cooled to room temperature, using rutin as standard specimen, using Al (NO3)3-
NaNO2Colorimetric method is respectively measured upper phase liquid and lower phase liquid, and flavones is big in the distribution coefficient of upper phase liquid and lower phase liquid
In 12, the rate of recovery is between 81.4-91.4%.
The alcohol water ratio 0.5-0.7 of third alcohol and water.
The step 1) Sorbus alnifolia leaf extracting flavonoids and separation: fresh Sorbus alnifolia leaf is dried, and is crushed；First use sulfuric acid
Ammonium 5.25g, propyl alcohol 6mL, water 10mL form stable double-aqueous phase system, and Sorbus alnifolia leaf 0.5g is added in double-aqueous phase system,
Ultrasonic wave extraction 40min is carried out at power 300W, temperature 50 C, is filtered, Sorbus alnifolia slag is removed, and filtrate stands 2h, layering
For upper phase liquid and lower phase liquid, upper phase liquid and lower phase liquid are separated while hot, obtain phase liquid and lower phase liquid.
Present invention application ultrasonic wave is coupled with double-aqueous phase system extracts Sorbus alnifolia flavones, has clear advantage:
(1) split-phase is rapid
It is experimentally observed, is coupled using ultrasonic wave with propyl alcohol-ammonium sulfate double-aqueous phase system and extract Sorbus alnifolia flavones,
Sorbus alnifolia leaf, propyl alcohol, ammonium sulfate are proportionally added into, after ultrasonic wave extraction, about 10min or so can split-phase (do not need to be centrifuged
Separation), and there is no emulsion layer, shorten the test period.
(2) process integration
Ultrasonic wave is separated with propyl alcohol-ammonium sulfate aqueous two-phase extraction, that is, has been achieved the purpose that extract, purified, and concentrated material
Liquid.It shows as impurity (such as hydrophily sugar, protein) and enters lower phase, Flavonoid substances are enriched in phase, above compare original place
It manages liquid to reduce, general flavone concentration and purity all improve.
Distribution coefficient K of the Sorbus alnifolia flavones in system is 16.218, and extraction yield Y is up to 91.4%.
(3) material consumption is reduced
The method of the present invention uses propyl alcohol to be easy to recycle as the organic solvent of aqueous two-phase, small toxicity, propyl alcohol and ammonium sulfate,
Greatly reduce the loss of raw material.
High with the rate of recovery of method Sorbus alnifolia flavones of the invention, production method is simple, is easy to grasp, not by environment shadow
It rings；It is low in cost, it is suitble to industrialization production.
The present invention is described in further details below by specific embodiment, but not as a limitation of the invention.
Specific embodiment
Embodiment 1
A kind of method that ultrasonic wave couples extraction Sorbus alnifolia flavones with double-aqueous phase system, the specific steps are as follows:
Step 1) Sorbus alnifolia leaf extracting flavonoids and separation obtain phase liquid and lower phase using propyl alcohol-ammonium sulfate aqueous two-phase
Liquid；
Lower phase liquid in step 1) is cooled down, crystallization, filtering, recycles ammonia sulfate crystal by step 2；
The finished product that upper phase liquid dehydrated alcohol in step 1) is purified, is concentrated, dried by step 3).
Embodiment 2
A kind of method that ultrasonic wave couples extraction Sorbus alnifolia flavones with double-aqueous phase system, the specific steps are as follows:
Step 1) Sorbus alnifolia leaf extracting flavonoids and separation obtain phase liquid and lower phase using propyl alcohol-ammonium sulfate aqueous two-phase
Liquid: fresh Sorbus alnifolia leaf is dried, and is crushed；Ammonium sulfate 4.50-6.00g, propyl alcohol 6mL-7mL are first used, water 10mL is formed and stablized
Double-aqueous phase system, in double-aqueous phase system be added Sorbus alnifolia leaf 0.5-0.7g, surpassed at power 300W, temperature 50 C
Sound wave extracts 20-40min, filters, and removes Sorbus alnifolia slag, and filtrate stands 1-3h, is layered as phase liquid and lower phase liquid, while hot will
Upper phase liquid and lower phase liquid separate, and obtain phase liquid and lower phase liquid.
Lower phase liquid in step 1) is cooled down, crystallization, filtering, recycles ammonia sulfate crystal by step 2；
Step 3) is by the upper phase liquid dehydrated alcohol purifying in step 1), concentration, dry finished product: upper phase liquid is added 3-5
After the dehydrated alcohol precipitating of times volume removes ammonium sulfate residual impurities, ethyl alcohol is recycled, it is true at 60 DEG C -70 DEG C after upper phase liquid concentration
Sky is dried to obtain Sorbus alnifolia leaf flavones finished product.
In aqueous two-phase enrichment flavone compound technology, widely used enrichment phase macromolecular polymer is not only more difficult
It is separated with flavone compound, and the price of macromolecular polymer is generally relatively high, not utilizing reduces cost.
Using propyl alcohol-ammonium sulfate aqueous two-phase, use propyl alcohol that can recycle as the organic solvent of aqueous two-phase, propyl alcohol and ammonium sulfate
It utilizes, it is low in cost, it is easy to operate.With method of the invention, Sorbus alnifolia leaf flavonoid material collection is separated in upper phase propyl alcohol
Phase, after upper phase liquid adds dehydrated alcohol precipitating to remove the residual impurities such as ammonium sulfate, recycling ethyl alcohol, concentration are dried in vacuo up to water elm
Sorbus alnifloria leaf flavones finished product；The ammonia sulfate crystal of lower phase liquid crystallisation by cooling filtering is recycled altogether.
Embodiment 3
A kind of method that ultrasonic wave couples extraction Sorbus alnifolia flavones with double-aqueous phase system, the specific steps are as follows:
Step 1) Sorbus alnifolia leaf extracting flavonoids and separation obtain phase liquid and lower phase using propyl alcohol-ammonium sulfate aqueous two-phase
Liquid: fresh Sorbus alnifolia leaf is dried, and is crushed；Ammonium sulfate 5.25g, propyl alcohol 6mL are first used, water 10mL forms stable aqueous two-phase
Sorbus alnifolia leaf 0.5g is added in double-aqueous phase system, ultrasonic wave extraction is carried out at power 300W, temperature 50 C for system
40min is filtered, and removes Sorbus alnifolia slag, and filtrate stands 2h, phase liquid and lower phase liquid is layered as, while hot by upper phase liquid and lower phase
Liquid separates, and obtains phase liquid and lower phase liquid.By upper phase liquid and lower phase liquid by being cooled to room temperature, phase liquid and lower phase liquid are taken
Product, respectively 6mL and 9.26mL, compared to (upper phase liquid and lower phase liquid volume ratio) 0.6522, using rutin as standard specimen, using Al
(NO3)3-NaNO2Colorimetric method is respectively measured upper phase liquid and lower phase liquid, and the flavonoid concentration of upper phase liquid is 7.039mg/
ML, the flavonoid concentration of lower phase liquid are 0.434mg/mL, and flavones is 16.218 in the distribution coefficient of upper phase liquid and lower phase liquid, general flavone
Yield up to 91.4%.
Lower phase liquid in step 1) is cooled down, crystallization, filtering, recycles ammonia sulfate crystal by step 2；
The finished product that upper phase liquid dehydrated alcohol in step 1) is purified, is concentrated, dried by step 3): by 5 times of bodies of upper phase liquid
After long-pending dehydrated alcohol precipitating removes ammonium sulfate residual impurities, ethyl alcohol is recycled, is dried in vacuo both at 60 DEG C after upper phase liquid concentration
Obtain Sorbus alnifolia leaf flavones finished product (0.04782g).The embodiment is most preferred embodiment.
Embodiment 4
A kind of method that ultrasonic wave couples extraction Sorbus alnifolia flavones with double-aqueous phase system, the specific steps are as follows:
Step 1) Sorbus alnifolia leaf extracting flavonoids and separation obtain phase liquid and lower phase using propyl alcohol-ammonium sulfate aqueous two-phase
Liquid: fresh Sorbus alnifolia leaf is dried, and is crushed；Ammonium sulfate 6g, propyl alcohol 6mL are first used, water 10mL forms stable aqueous two-phase body
Sorbus alnifolia leaf 0.6g is added in system in double-aqueous phase system, and ultrasonic wave extraction 20min is carried out at power 300W, temperature 50 C,
It filtering, removes Sorbus alnifolia slag, filtrate stands 1h, is layered as phase liquid and lower phase liquid, while hot separates upper phase liquid and lower phase liquid,
Obtain phase liquid and lower phase liquid.By upper phase liquid and lower phase liquid by being cooled to room temperature, phase liquid and lower phase liquid product are taken, respectively
4.2mL and 12mL, compared to (upper phase liquid and lower phase liquid volume ratio) 0.3500, using rutin as standard specimen, using Al (NO3)3-NaNO2Than
Color method is respectively measured upper phase liquid and lower phase liquid, and the flavonoid concentration of upper phase liquid is 11.829mg/mL, the flavones of lower phase liquid
Concentration is 0.945mg/mL, and flavones is 12.517 in the distribution coefficient of upper phase liquid and lower phase liquid, and the yield of general flavone is up to 81.4%.
Lower phase liquid in step 1) is cooled down, crystallization, filtering, recycles ammonia sulfate crystal by step 2；
The finished product that upper phase liquid dehydrated alcohol in step 1) is purified, is concentrated, dried by step 3): by 4 times of bodies of upper phase liquid
After long-pending dehydrated alcohol precipitating removes ammonium sulfate residual impurities, ethyl alcohol is recycled, is dried in vacuo both at 65 DEG C after upper phase liquid concentration
Obtain Sorbus alnifolia leaf flavones finished product (0.05419g).
Embodiment 5
A kind of method that ultrasonic wave couples extraction Sorbus alnifolia flavones with double-aqueous phase system, the specific steps are as follows:
Step 1) Sorbus alnifolia leaf extracting flavonoids and separation obtain phase liquid and lower phase using propyl alcohol-ammonium sulfate aqueous two-phase
Liquid: fresh Sorbus alnifolia leaf is dried, and is crushed；Ammonium sulfate 5.25g, propyl alcohol 7mL are first used, water 10mL forms stable aqueous two-phase
Sorbus alnifolia leaf 0.7g is added in double-aqueous phase system, ultrasonic wave extraction is carried out at power 300W, temperature 50 C for system
20min is filtered, and removes Sorbus alnifolia slag, and filtrate stands 3h, phase liquid and lower phase liquid is layered as, while hot by upper phase liquid and lower phase
Liquid separates, and obtains phase liquid and lower phase liquid.By upper phase liquid and lower phase liquid by being cooled to room temperature, phase liquid and lower phase liquid are taken
Product, respectively 5.4mL and 11.5mL, compared to (upper phase liquid and lower phase liquid volume ratio) 0.4696, using rutin as standard specimen, using Al
(NO3)3-NaNO2Colorimetric method is respectively measured upper phase liquid and lower phase liquid, and the flavonoid concentration of upper phase liquid is 10.251mg/
ML, the flavonoid concentration of lower phase liquid are 0.670mg/mL, and flavones is 15.300 in the distribution coefficient of upper phase liquid and lower phase liquid, general flavone
Yield up to 81.4%.
Lower phase liquid in step 1) is cooled down, crystallization, filtering, recycles ammonia sulfate crystal by step 2；
The finished product that upper phase liquid dehydrated alcohol in step 1) is purified, is concentrated, dried by step 3): by 3 times of bodies of upper phase liquid
After long-pending dehydrated alcohol precipitating removes ammonium sulfate residual impurities, ethyl alcohol is recycled, is dried in vacuo both at 70 DEG C after upper phase liquid concentration
Obtain Sorbus alnifolia leaf flavones finished product (0.06205g).
The present invention is based on following discoveries: Flavonoid substances content is higher in Sorbus alnifolia leaf.Table 1 gives Sorbus alnifolia
Distribution coefficient of the leaf flavonoid substance in propyl alcohol-ammonium sulfate aqueous two-phase.The principle of double-aqueous phase system extraction and separation technology is: water
Elm Sorbus alnifloria leaf flavonoid substance carries out selective distribution in aqueous two-phase phase system, shows certain distribution coefficient.Water elm
Chinese catalpa leaf flavonoid substance is affinity to propyl alcohol, and Sorbus alnifolia leaf flavones is made to be easier to distribute in the upper phase rich in propyl alcohol, and one
A little impurity such as sugar, protein equal part fit over lower phase, and the distribution coefficient of Sorbus alnifolia leaf flavones is greater than 12 in scope of experiment, recycling
Rate is between 81.4-91.4%.
Distribution behavior of the 1 Sorbus alnifolia leaf flavones of table in propyl alcohol-ammonium sulfate aqueous two-phase
In table: R=Vt/Vb;K=Ct/Cb；Y=RK/(RK+1)
In formula: R--- is compared；VtUpper phase volume；VbLower phase volume；K-distribution of the Sorbus alnifolia leaf flavones in aqueous two-phase
Coefficient；Ct--- the mass concentration of upper phase liquid Sorbus alnifolia leaf flavones, mg/mL；Cb--- the matter of lower phase liquid Sorbus alnifolia leaf flavones
Measure concentration, mg/mL；Y-extraction yield (yield).
Therefore, it is heavy fixed etc. that extracting and developing, dehydrated alcohol are coupled with propyl alcohol-ammonium sulfate double-aqueous phase system through above-mentioned ultrasonic wave
The processing of process makes Sorbus alnifolia leaf flavonoid substance be extracted, be concentrated and purified, finally obtain quality height, high income, at
The finished product of this low Sorbus alnifolia Flavonoid substances.
The present embodiment does not have the well known conventional means of the detailed process step category industry, does not describe one by one here.
Claims (2)
1. a kind of ultrasonic wave couples the method for extracting Sorbus alnifolia flavones with double-aqueous phase system, it is characterized in that: this method is specific
Steps are as follows:
Step 1) Sorbus alnifolia leaf extracting flavonoids and separation obtain phase liquid and lower phase liquid using propyl alcohol-ammonium sulfate aqueous two-phase；
Lower phase liquid in step 1) is cooled down, crystallization, filtering, recycles ammonia sulfate crystal by step 2；
The finished product that upper phase liquid dehydrated alcohol in step 1) is purified, is concentrated, dried by step 3)；
The step 1) Sorbus alnifolia leaf extracting flavonoids and separation: fresh Sorbus alnifolia leaf is dried, and is crushed；First use ammonium sulfate
4.50-6.00g, propyl alcohol 6mL-7mL, water 10mL form stable double-aqueous phase system, Sorbus alnifolia are added in double-aqueous phase system
Leaf 0.5-0.7g carries out ultrasonic wave extraction 20-40min at power 300W, temperature 50 C, filters, and removes Sorbus alnifolia slag, filter
Liquid stands 1-3h, is layered as phase liquid and lower phase liquid, while hot separates upper phase liquid and lower phase liquid, obtains phase liquid and lower phase liquid；
The step 3) is by the upper phase liquid dehydrated alcohol purifying in step 1), concentration, dry finished product: upper phase liquid is added 3-5
After the dehydrated alcohol precipitating of times volume removes ammonium sulfate residual impurities, ethyl alcohol is recycled, it is true at 60 DEG C -70 DEG C after upper phase liquid concentration
Sky is dried to obtain Sorbus alnifolia leaf flavones finished product；
The upper phase liquid of the step 1) and lower phase liquid are by being cooled to room temperature, using rutin as standard specimen, using Al (NO3)3-NaNO2Than
Color method is respectively measured upper phase liquid and lower phase liquid, and flavones is greater than 12 in the distribution coefficient of upper phase liquid and lower phase liquid, returns
Yield is between 81.4-91.4%.
2. a kind of ultrasonic wave according to claim 1 couples the method for extracting Sorbus alnifolia flavones with double-aqueous phase system,
Be characterized in: the step 1) Sorbus alnifolia leaf extracting flavonoids and separation: fresh Sorbus alnifolia leaf is dried, and is crushed；First use sulfuric acid
Ammonium 5.25g, propyl alcohol 6mL, water 10mL form stable double-aqueous phase system, and Sorbus alnifolia leaf 0.5g is added in double-aqueous phase system,
Ultrasonic wave extraction 40min is carried out at power 300W, temperature 50 C, is filtered, Sorbus alnifolia slag is removed, and filtrate stands 2h, layering
For upper phase liquid and lower phase liquid, upper phase liquid and lower phase liquid are separated while hot, obtain phase liquid and lower phase liquid.
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| CN101396432B (en) * | 2008-10-13 | 2011-02-16 | 广西大学 | Method for concentrating and separating flavonoids from toona sinensis leaves |
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