CN105748580A - Low-temperature extraction device and method of active ingredients of natural products - Google Patents
Low-temperature extraction device and method of active ingredients of natural products Download PDFInfo
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- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
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Abstract
The invention provides a low-temperature extraction device and method of active ingredients of natural products.The low-temperature extraction device comprises a countercurrent extraction unit, an ultrasonic extraction unit, a membrane concentration unit and an enzyme adding unit, the enzyme adding unit is communicated with the countercurrent extraction unit, a residue outlet of the countercurrent extraction unit is connected with a to-be-extracted raw material feeding port of the ultrasonic extraction unit, an extract outlet of the ultrasonic extraction unit is connected with a to-be-separated liquid inlet of the membrane concentration unit, and a concentrate outlet of the membrane concentration unit is connected with a solvent inlet of the countercurrent extraction unit.Low-temperature enzymolysis technology is combined with countercurrent extraction and ultrasonic extraction, the extraction process is completed at low temperature (15-50 DEG C), extraction assisting effect of a biological active enzyme and concentration gradient increasing effect of countercurrent extraction jointly guarantee effective extraction rate of the active ingredients; ultrasonic extraction is performed on extraction residue of the natural products only, so that energy consumption is saved, recycling of the active enzyme is realized, and cost is lowered.
Description
Technical field
The invention belongs to the extraction and separation technology field of active component in natural prodcuts, relate to a kind of natural prodcuts
Low temperature (15-50 DEG C) extraction element of active component and method, particularly relate to the low of a kind of active ingredient of Chinese herbs
Temperature (15-50 DEG C) extraction element and method.
Background technology
Solvent extraction method is the most frequently used natural dynamic from Chinese herb, the natural plants of non-Chinese medicine, non-Chinese medicine
The method extracting active component in the solid natural prodcuts such as thing, natural minerals, edible fungus, according to active matter
The difference of matter, can select different solvents.Solvent extraction method is different with technique according to actual conditions, permissible
It is divided into infusion process, percolation, decocting method, reflux extraction, continuous extraction etc..Conventional natural products
The temperature that extraction process of active component typically uses close to solvent boiling carries out boiling, and follow-up employing high temperature steams
The method sent out realizes solvent and separates with active component.This method operation temperature is high, and extraction time is long, energy
Consumption is big, and most importantly high temperature extraction and concentration process can destroy the activity of active component.
The extracting method of the natural product active ingredient of the improvement occurred in recent years has ultrasound assisted extraction technique, surpasses and face
Boundary's fluid extraction technology, hot refluxed cryogenic extract, microwave abstracting, and counter current chromatography extracts, and biology enzyme assists
Extract.Wherein during Continuous Countercurrent Extraction, countercurrent movement the most in opposite directions made by material and solvent simultaneously, has
Effect improves extraction state, can significantly improve extraction efficiency；When ultrasound assisted extraction technique has shortening extraction
Between, improve active component recovery rate, save the energy, avoid high temperature on advantages such as the impacts of composition；Biology enzyme
By decomposition, destroy the shielding action of plant cell, there is good low temperature and extract performance.
The extracting method of the natural product active ingredient of above-described improvement can realize low to a certain extent
Temperature is extracted, but single counter-flow extraction and ultrasonic extraction are unable to reach the highest recovery rate at low temperatures, and
Biological enzyme can obtain good extraction performance at low temperatures, but there is the problem of high cost, solves
One of method be to realize recycling of enzyme, but there is presently no the circulation profit that can effectively realize enzyme
Report.
CN 102100712 A discloses a kind of ultrasonic extraction of continuous flow upstream and combines membrane technology extraction arasaponin
Method, the method mainly adds the temperature that the 40-90% ethanol of pseudo-ginseng meal weight 6-15 times is at 20-50 DEG C
Lower continuous flow upstream ultrasonic extraction 20-120min, supersonic frequency is 20-80KHz；Filtrate 1000-2500's
Milipore filter or 100-800 NF membrane are at 20-50 DEG C, and under 0.4-4.1MPa, film concentrates；It is evaporated to without alcohol taste
After be diluted with water or be directly diluted with water, macroporous absorbent resin in filtration, water elution is washed with 50-90% ethanol again
De-；Using 100-800 NF membrane after parlkaline resin anion (R.A.), under 0.4-4.1MPa, film concentrates, and subtracts after decolouring
Pressure concentrates, and is spray-dried.The arasaponin total recovery that the method obtains is 6.7-14.3%.CN
104857108 A disclose a kind of ultrasonic method preparing haw thorn extract of continuous flow upstream, and it includes walking as follows
Rapid: dry haw raw material is removed impurity pulverization process；Utilize continuous flow upstream ultrasonic device to hawthorn powder
End is extracted；Extract is concentrated, alcohol precipitation filtering；By film device, extract is separated
Purify, the haw thorn extract that purity is higher can be collected.But above two extracting method is just for a certain kind
Material, and its recovery rate is not high enough, the energy consumption during extraction is higher.
Summary of the invention
Long for the high-temperature operation time present in Conventional solvents extraction process, the energy consumption brought accordingly is high, lives
Property loses greatly, the invention provides a kind of low temperature extraction element and the method for natural prodcuts active component, described
Low temperature zymolysis technique is combined by device with counter-flow extraction and ultrasonic extraction process, makes extraction process at low temperature
Completing under (15-40 DEG C), the assisted extraction effect of bioactive enzyme and counter-flow extraction improve the work of concentration gradient
Effective recovery rate of active component by common guarantee；Owing to only the extraction residue of natural prodcuts being carried out ultrasonic
Extract, saved energy consumption, and be simultaneously achieved the recycling of organized enzyme, saved cost.
For reaching this purpose, the present invention by the following technical solutions:
A kind of extraction element of natural prodcuts active component, including counter-flow extraction unit, ultrasonic extraction unit and
Film upgrading unit, described device also includes that enzyme adds unit, and enzyme adds unit and connects with counter-flow extraction unit,
The solid discharge of counter-flow extraction unit is connected with the material inlet to be extracted of ultrasonic extraction unit, ultrasonic extraction
The extracting liquid outlet of unit is connected with the liquid import to be separated of film upgrading unit, and the concentrate of film upgrading unit goes out
Mouth is connected with the solvent inlet of counter-flow extraction unit.
Described counter-flow extraction unit refers to the equipment for counter-flow extraction natural prodcuts active component, described adverse current
Extraction unit one end is provided with material inlet to be extracted and extracting liquid outlet, and the other end is provided with solvent inlet
And solid discharge.Described raw material to be extracted enters counter-flow extraction unit through material inlet to be extracted, along adverse current
Extraction unit forward flow, solvent enters counter-flow extraction unit from solvent inlet, reverse along counter-flow extraction unit
Flowing, raw material to be extracted and solvent carry out counter current contacting, and the active component in raw material to be extracted enters solvent
In, extract is discharged from extracting liquid outlet, and the residue after extraction is discharged from solid discharge.
Low temperature of the present invention each means 15-50 DEG C if no special instructions.Enzyme adding apparatus of the present invention to
The organized enzyme put in counter-flow extraction unit has optimal performance at less than 50 DEG C, but active under this low temperature
Composition can be deteriorated from the diffusion effect of bulk to be extracted solvent phase in opposite directions.Therefore, what the present invention provided carries
Fetching puts the feature that can improve two-phase concentration gradient according to counter-flow extraction process, uses organized enzyme enzymolysis and inverse
Stream two kinds of Combination of Methods of extraction method use, and synergistic function occur, it is achieved that sky under the conditions of 15-50 DEG C
The purpose that so product active ingredient high-recovery extracts, meanwhile, counter-flow extraction is a continuous process, leading portion
Adsorptive enzyme in the residue extracted can desorb and extract for back segment, thus avoids raw material to be extracted
Mixed batch of problem；For the recovery of organized enzyme, have employed ultrasonic wave and extract and the technology of UF membrane coupling, utilize
Ultrasonic wave can occur the effects such as cavitation in plant cell and in solvent, the organized enzyme making absorption is fast from residue
Speed desorbs, and utilizes membrane process simultaneously, the organized enzyme continuous concentration of desorption is separated, makes ultrasonic extraction
Liquid phase organized enzyme in journey is maintained at the lowest level, and the biology enzyme being beneficial to desorb mutually from solid is rapidly to liquid
Spread mutually；On the other hand, ultrasonic procedure can also realize the depth extraction of residual activity composition in residue, super
Sound process is power consumption process, and it utilizes at the back segment extracted rather than all extracts process, also reduces ultrasonic
The cost increased.
The Extracting temperature of described extraction element is 15-50 DEG C.
The material inlet to be extracted of described counter-flow extraction unit is connected with reducing mechanism.Described raw material to be extracted
First pulverize and carry out counter-flow extraction again.
Preferably, the extracting liquid outlet of described counter-flow extraction unit is connected with concentrate drying unit, described concentration
Drying unit is for concentrating the active component in extract and being dried, thus obtains the active component being dried.
The temperature of described counter-flow extraction is 15-50 DEG C, and the time of described counter-flow extraction is 0.5-3 hour, described
During counter-flow extraction, raw material to be extracted is 1:1-1:20 with the mass ratio of solvent.
Preferably, described enzyme addition unit is connected to the solvent in the middle part of counter-flow extraction unit with counter-flow extraction unit
Between inducer, preferably it is connected to the middle part of counter-flow extraction unit.Described enzyme adds unit for adverse current
Adding organized enzyme in extraction unit, organized enzyme solvent with counter-flow extraction unit in the middle part of counter-flow extraction unit enters
There was added beneficially organized enzyme between mouth section to be fully contacted with raw material to be extracted, give full play to the effect of organized enzyme.
Preferably, between described ultrasonic extraction unit and film upgrading unit, it is provided with pretreatment unit, described pre-
Processing unit is for removing the solid impurity in the extract that ultrasonic extraction unit obtains, it is ensured that film upgrading unit
Normal work, and reduce the replacing number of times of separation film therein.
Preferably, described pretreatment unit is centrifuge, micro-filtration or plate filter, is preferably centrifugal
Machine.
Preferably, the permeate outlet of described film upgrading unit is connected with the solvent inlet of ultrasonic extraction unit.
Thus realize the recycling of permeate, reduce the addition of fresh solvent.
Described counter-flow extraction unit be duct type counterflow extraction apparatus and/or dynamically continuously pot group type counter-flow extraction set
Standby, preferably duct type counterflow extraction apparatus.
Preferably, described ultrasonic extraction unit is ultrasonic extractor.Described ultrasonic wave extraction unit extracts temperature
Degree is 15-50 DEG C, preferably 50 DEG C；The ultrasonic frequency range of described ultrasonic wave extraction unit is
20-100kHz, preferably 40kHz.The time that ultrasonic wave extracts is 10 minutes-2 hours.Described ultrasonic wave carries
During taking, residue is 1:1-1:20 with the mass ratio of solvent.
Preferably, it is enzyme solutions material-compound tank and feed pump that described enzyme adds unit, and described feed pump carries with adverse current
Take unit to be connected.Organized enzyme assisted extraction process in the present invention is the process of a low temperature, and hydrolysis temperature exists
Less than 50 DEG C.The temperature of described enzymolysis and extraction is 15-50 DEG C, preferably 50 DEG C；Described organized enzyme addition
It is 0.1-2% with the mass ratio of raw material to be extracted, preferably 0.6%.Described organized enzyme is cellulase, pectin
Any one or the mixture of at least two, the nonrestrictive reality of described mixture in enzyme, papain
Such as: cellulase and the mixture of pectase；Pectase and the mixture of papain；Cellulose
The mixture of enzyme, pectase and papain.Cellulase as organized enzyme can be by plant cell wall
Cellulose is hydrolyzed into water-soluble sugar, and the plant cell wall hydrolysis after cellulase processes ruptures, beneficially intracellular
The dissolution of active compound component；Pectase can make intercellular pectic substance degrade, cell in tissue
Separate；Papain can be with decomposing protein, and therefore, the addition of organized enzyme can be effectively improved
The extraction effect of plant containing natural product.
Preferably, described film upgrading unit is that rolling diaphragm separator, tubular membrane separator or hollow-fibre membrane divide
Any one or the combination of at least two, preferably rolling diaphragm separator in device.Typical case but non-limiting
Be combined as rolling diaphragm separator and tubular membrane separator, rolling diaphragm separator and hollow fiber membrane separator,
Rolling diaphragm separator, tubular membrane separator and hollow fiber membrane separator.
Separation film in described film upgrading unit is organic nanofiltration membrane and/or organic reverse osmosis membrane, the most organic
NF membrane.Described separation film has cutoff performance to the active component extracted.
Preferably, the molecular cut off of described organic nanofiltration membrane is 200-400.
Preferably, the material of described separation film be cellulose, cellulose acetate, SPSF, polyamide,
Any one or at least two in polyimides, polyether sulfone, sulfonated polyether sulfone, poly-piperazine or polyvinyl alcohol
Combination.Typical but non-limiting combination is such as: cellulose and cellulose acetate, SPSF and polyamides
Amine, poly-piperazine and polyvinyl alcohol, polyimides, polyether sulfone and sulfonated polyether sulfone, cellulose acetate, sulfonation
Polysulfones and polyamide, polyether sulfone, sulfonated polyether sulfone, poly-piperazine and polyvinyl alcohol.
The operation pressure of described film upgrading unit is 0.5-6.0MPa, as 0.5MPa, 1.0MPa, 1.5MPa,
1.8MPa、2.0MPa、2.5MPa、2.8MPa、3.0MPa、3.2MPa、3.5MPa、4.0MPa、
4.2MPa, 4.5MPa, 5.0MPa, 5.5MPa or 6.0MPa etc., temperature is 15-50 DEG C, as 15 DEG C,
18 DEG C, 20 DEG C, 22 DEG C, 25 DEG C, 28 DEG C, 30 DEG C, 32 DEG C, 35 DEG C, 38 DEG C, 40 DEG C, 42 DEG C,
45 DEG C, 48 DEG C or 50 DEG C etc..
The two of the purpose of the present invention are that providing one to utilize device as above to extract natural prodcuts activity becomes
The method divided, described method comprises the steps:
(1) by raw material to be extracted and solvent counter current contacting under the effect of organized enzyme, extract in raw material to be extracted
Active component, obtain the extract containing active component and residue；
(2) active component in ultrasonic extraction residue, the organized enzyme of absorption on desorption residue, is contained simultaneously
Active composition and the ultrasonic extract of organized enzyme；
(3) ultrasonic extract is carried out membrane separation concentration, obtain organized enzyme and the concentrate of active component and
Permeate, described concentrate is for completely or partially replacing the solvent in step (1).
Described extracting method is suitable under the conditions of 15-50 DEG C extracting the active component in natural prodcuts, it is possible to real
The low temperature of existing natural prodcuts active component extracts.
Organized enzyme of the present invention has optimal performance at less than 50 DEG C, but active matter under this low temperature
Matter can be deteriorated from the diffusion effect of medicinal material main body solvent phase in opposite directions.The present invention can carry according to counter-flow extraction process
The feature of high two-phase concentration gradient, uses biology enzyme enzymolysis and two kinds of Combination of Methods of counter-flow extraction method to use, its
Synergistic function can occur, it is achieved that natural prodcuts active component high-recovery extracts under cryogenic
Purpose, meanwhile, counter-flow extraction is a continuous process, the adsorptive enzyme in the natural prodcuts residue that leading portion extracts
Can desorb and extract for rear end, thus avoid mixed batch of problem of raw material；For the recovery of biology enzyme,
Have employed ultrasonic wave and the technology of UF membrane coupling, utilize ultrasonic wave can occur in plant cell and in solvent
Cavitations etc. act on, and make organized enzyme fast desorption from natural prodcuts residue of absorption out, utilize film mistake simultaneously
Journey, separates the biology enzyme continuous concentration of desorption, makes the liquid phase biology enzyme during ultrasonic extraction be maintained at
The lowest level, is beneficial to the biology enzyme from solid desorbs mutually and spreads to liquid phase rapidly；On the other hand, ultrasonic mistake
Journey can also realize the depth extraction of residual activity composition in residue, and ultrasonic procedure is power consumption process, and it utilizes
Extract rear end rather than all extract process, also reduce the cost of ultrasonic increase.
The described raw material to be extracted of step (1) is natural prodcuts, preferably Chinese medicine.
Preferably, the described raw material to be extracted of step (1) contacts with solvent counter current the most again.Treat to increase
Extract the contact area of raw material and solvent, improve extraction efficiency.
Step (1) described counter current contacting carries at duct type counterflow extraction apparatus and/or the most continuous pot group type adverse current
Taking equipment is carried out, preferably duct type counterflow extraction apparatus.
Preferably, the mass ratio of the described raw material to be extracted of step (1) and solvent is 1:1-1:20, as 1:2,
1:3,1:5,1:8,1:10,1:12,1:15,1:18 or 1:19 etc., preferably 1:5.
Preferably, the addition of step (1) described organized enzyme with the mass ratio of raw material to be extracted is
0.1-2%, such as 0.1%, 0.2%, 0.5%, 0.8%, 1.0%, 1.2%, 1.5%, 1.8% or 2.0% etc.,
Preferably 0.6%.
Preferably, the organized enzyme described in step (1) is appointing in cellulase, pectase or papain
Anticipate a kind of or mixture of at least two.The nonrestrictive example of described mixture is such as: cellulase and pectin
The mixture of enzyme；Pectase and the mixture of papain；Cellulase, pectase and papain
Mixture.The cellulose of plant cell wall can be hydrolyzed into water-soluble sugar, at cellulase by cellulase
Plant cell wall hydrolysis after reason ruptures, the beneficially dissolution of intracellular activity component cpd；Pectase can make
Intercellular pectic substance is degraded, and cell is separated in tissue；Papain can be with decomposition of protein
Matter, therefore, the addition of bioactive enzyme can be effectively improved the extraction effect of plant containing natural product.
Preferably, step (1) described organized enzyme adds at the leading portion extracted, and is preferably the stage casing extracting and adds
Enter.Described extraction process can be divided into extraction leading portion and extract back segment, and extracting leading portion is that raw material to be extracted is just with molten
Agent contact, to about the 1/2 of extraction time, is extracted about the 1/2 extremely extraction that back segment is extraction time and is terminated, carry
Take liquid to discharge.Extract leading portion addition organized enzyme beneficially organized enzyme to be fully contacted with raw material to be extracted, preferably
Play the effect of organized enzyme.
Preferably, step (1) described organized enzyme is added in raw material to be extracted and solvent by feed pump.
Preferably, the temperature of step (1) described extraction is 15-50 DEG C, as 15 DEG C, 18 DEG C, 20 DEG C,
22 DEG C, 25 DEG C, 28 DEG C, 30 DEG C, 32 DEG C, 35 DEG C, 38 DEG C, 40 DEG C, 42 DEG C, 45 DEG C or 50 DEG C etc.,
Preferably 50 DEG C.
Preferably, the time of step (1) described extraction is 0.5-3 hour, as 0.8 hour, 1.0 hours,
1.2 hours, 1.5 hours, 1.8 hours, 2.0 hours, 2.2 hours, 2.5 hours or 2.8 hours etc., preferably
It it is 2 hours.
Preferably, step (1) described extract carries out concentrate drying process, obtains active component.
Described ultrasonic being extracted on ultrasonic extractor of step (2) is carried out.
Preferably, the ultrasonic frequency range of the described ultrasonic extraction of step (2) is 20-100kHz, as
20kHz、25kHz、30kHz、35kHz、40kHz、45kHz、50kHz、55kHz、60kHz、
65kHz, 70kHz, 75kHz, 80kHz, 85kHz, 90kHz, 95kHz or 100kHz etc., preferably
40kHz。
Preferably, the temperature of the described ultrasonic extraction of step (2) is 15-50 DEG C, as 15 DEG C, 18 DEG C, 20 DEG C,
22 DEG C, 25 DEG C, 28 DEG C, 30 DEG C, 32 DEG C, 35 DEG C, 38 DEG C, 40 DEG C, 42 DEG C, 45 DEG C or 50 DEG C etc.,
Preferably 50 DEG C.
Preferably, the time of the described ultrasonic extraction of step (2) is 10 minutes-2 hours, as 0.5 hour, 0.8
Hour, 1.0 hours, 1.2 hours, 1.5 hours or 1.8 hours etc., preferably 1 hour.
Preferably, in the described ultrasonic extraction of step (2), the mass ratio of residue and solvent is 1:1-1:20, as 1:2,
1:3,1:5,1:8,1:10,1:12,1:15,1:18 or 1:19 etc., preferably 1:5.
Ultrasonic wave can occur the effects such as cavitation in plant cell and in solvent, makes the organized enzyme of absorption from residue
Upper fast desorption out, utilizes membrane process simultaneously, the biology enzyme continuous concentration of desorption is separated, makes ultrasonic carrying
Liquid phase biology enzyme during taking is maintained at the lowest level, and the biology enzyme being beneficial to desorb mutually from solid is rapid
Spread to liquid phase；On the other hand, ultrasonic procedure can also realize the degree of depth of residual activity composition in residue and carries
Taking, ultrasonic procedure is power consumption process, and it utilizes in the rear end extracted rather than all extracts process, also reduces
The cost of ultrasonic increase.
Ultrasonic extract first carries out pre-processing the membrane separation concentration carried out again described in step (3), described pre-place
Reason is any one in centrifugal treating, micro-filtration or plate-frame filtering or the combination of at least two, is preferably centrifugal
Process.Pretreatment it is advantageously ensured that being normally carried out of membrane separating process, reduces the replacing time separating film simultaneously
Number, reduces cost.
Preferably, step (3) described membrane separation concentration is in rolling diaphragm separator, tubular membrane separator or hollow
Carry out in any one or the combination of at least two in tunica fibrosa separator, be preferably at rolling diaphragm separator
On carry out.Typical but non-limiting rolling diaphragm separator and the tubular membrane separator of being combined as, rolled film separation
Device and hollow fiber membrane separator, rolling diaphragm separator, tubular membrane separator and hollow fiber membrane separator.
Preferably, the membrane separation concentration described in step (3) is carried out under the pressure of 0.5-6.0MPa, as
0.5MPa、1.0MPa、1.5MPa、1.8MPa、2.0MPa、2.5MPa、2.8MPa、3.0MPa、
3.2MPa, 3.5MPa, 4.0MPa, 4.2MPa, 4.5MPa, 5.0MPa, 5.5MPa or 6.0MPa
Deng.
Preferably, the membrane separation concentration described in step (3) is carried out under conditions of 15-50 DEG C, as 15 DEG C,
18 DEG C, 20 DEG C, 22 DEG C, 25 DEG C, 28 DEG C, 30 DEG C, 32 DEG C, 35 DEG C, 38 DEG C, 40 DEG C, 42 DEG C,
45 DEG C, 48 DEG C or 50 DEG C etc..
Preferably, the separation film that step (3) described membrane separation concentration uses is organic nanofiltration membrane or organic reverse osmosis
Permeable membrane, preferably organic nanofiltration membrane.Described separation film is used for retaining organized enzyme and active component, thus obtains
Containing organized enzyme and the ultrasonic extract of active component.
Preferably, the molecular cut off of described organic nanofiltration membrane is 200-400.
Preferably, the material of described separation film be cellulose, cellulose acetate, SPSF, polyamide,
Any one or at least two in polyimides, polyether sulfone, sulfonated polyether sulfone, poly-piperazine or polyvinyl alcohol
Combination.Typical but non-limiting combination is such as: cellulose and cellulose acetate, SPSF and polyamides
Amine, poly-piperazine and polyvinyl alcohol, polyimides, polyether sulfone and sulfonated polyether sulfone, cellulose acetate, sulfonation
Polysulfones and polyamide, polyether sulfone, sulfonated polyether sulfone, poly-piperazine and polyvinyl alcohol.
Preferably, the permeate described in step (3) returns step (2).Make realizing the circulation of permeate
With, reduce the consumption of fresh solvent.
As preferred technical scheme, described method comprises the steps:
(1) raw material to be extracted mixes with solvent after crushing, to be extracted former subsequently into counterflow extraction apparatus
Material charging aperture, along counterflow extraction apparatus forward flow under additional power drive, fresh solvent is from counter-flow extraction
The solvent inlet of equipment opposite side enters, solvent and raw material counter current contacting mass transfer to be extracted, raw material to be extracted with
The mass ratio of solvent total amount is 1:1-1:20, and organized enzyme is from the middle part of counterflow extraction apparatus and counter-flow extraction unit
Solvent inlet section between position add counter-flow extraction unit, Extracting temperature is 15-50 DEG C, and organized enzyme adds
The mass ratio entering amount and raw material inlet to be extracted is 0.1-2%, and extraction time is 0.5-3 hour, is extracted
Liquid and residue, extract, after the extracting liquid outlet of counterflow extraction apparatus is discharged, carries out concentrate drying, obtains
Active component；
(2) ultrasonic extractor is used to extract the active component in residue further and desorb absorption at residue
On organized enzyme, the mass ratio of the residue in ultrasonic extractor and solvent is 1:1-1:20, and ultrasonic wave extracts
Temperature be 15-50 DEG C, ultrasonic wave extract ultrasonic frequency range be 20-100kHz, ultrasonic wave extract
Time is 10 minutes-2 hours, obtains the ultrasonic extract containing active component and organized enzyme；
(3) ultrasonic extract is after centrifugal treating, enters membrane separator, and the pressure at 0.5-6.0MPa drives
Move and at a temperature of 15-50 DEG C, by membrane separator separation concentrated active ingredients and organized enzyme, contained
Active enzyme and the concentrate of active component and permeate, concentrate is for completely or partially replacing step
(1) fresh solvent in, permeate returns in the ultrasonic wave extraction equipment described in step (2) continuously.
Compared with prior art, the invention have the benefit that
The extraction element of the natural prodcuts active component that the present invention provides is by low temperature zymolysis technique and counter-flow extraction mistake
Journey combines, and makes extraction process complete under low temperature (15-40 DEG C), and the assisted extraction of bioactive enzyme is made
With the effect common guarantee effective recovery rate of active component improving concentration gradient with counter-flow extraction.
The extraction element of the natural prodcuts active component that the present invention provides uses in ultrasound assisted extraction natural prodcuts
Active component, it is achieved the depth extraction of residual activity composition in the desorption of organized enzyme and residue, solve
Organized enzyme adsorption loss problem on natural prodcuts residue and the high problem of energy consumption.
The extraction element of the natural prodcuts active component that the present invention provides uses membrane process continuously to ultrasonic extract
Concentrating, the organized enzyme solution after concentration completely or partially replaces the solvent of counter-flow extraction, thus improves
The utilization rate of organized enzyme, reduces extraction cost；It addition, the organized enzyme of this mode reclaims, can avoid
The enzyme that other methods reclaiming enzyme obtain extracts mixed batch of the different batches raw material brought for next group natural prodcuts
Problem.
Accompanying drawing explanation
The low temperature extraction element signal of the natural prodcuts active component that Fig. 1 provides for one embodiment of the present invention
Figure；
Wherein, 1-disintegrating apparatus, 2-counterflow extraction apparatus, the ultrasonic extractor of 3-, 4-ultrasonic probe, 5-locates in advance
Reason equipment, 6-film concentrator, 7-enzyme adding apparatus.
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be further described.Theme protection domain involved in the present invention is also
Non-it is only limitted to these embodiments.
As it is shown in figure 1, be the low temperature extraction of the natural prodcuts active component that one embodiment of the present invention provides
Device.Disintegrating apparatus 1 that described device includes being sequentially connected, counterflow extraction apparatus 2, ultrasonic extractor 3,
Pre-processing device 5 and film concentrator 6, described device also includes enzyme adding apparatus 7, described enzyme adding apparatus
7 are connected with counterflow extraction apparatus 2；Permeate outlet and the ultrasonic extractor 3 of described film concentrator 6
Colvent inlet is connected, the solvent inlet phase of the concentrated solution outlet of described membrane concentrator and counterflow extraction apparatus 2
Even, described ultrasonic extractor 3 is provided with ultrasonic probe 4.
The process utilizing described extraction element to extract natural prodcuts active component is:
(1) natural prodcuts mix with solvent, subsequently into counterflow extraction apparatus 2 after disintegrating apparatus 1 is broken
Charging aperture, along counterflow extraction apparatus 2 forward flow under additional power drive, fresh solvent from adverse current carry
The solvent inlet of taking equipment 2 opposite side enters, and solvent and natural prodcuts counter current contacting mass transfer, organized enzyme is inverse
The middle part of stream extraction equipment 2 adds, and obtains extract and residue, and extract carries from counterflow extraction apparatus 2
After taking liquid outlet discharge, carry out concentrate drying, obtain active component；
(2) ultrasonic extraction tank is used to extract the active component in residue further and desorb absorption at residue
On organized enzyme, obtain the ultrasonic extract containing active component and organized enzyme；
(3) ultrasonic extract is after centrifugal treating, enters film concentrator 6, by film concentrator 6
Concentrated active ingredients and organized enzyme, obtain containing organized enzyme and the concentrate of active component and permeate, dense
Contracting liquid is for completely or partially replacing the fresh solvent in step (1), and permeate returns to step (2) continuously
In described ultrasonic wave extraction equipment.
Embodiment 1:
200g rabdosia lophanthide raw material enters counterflow extraction apparatus after broken, and Materials Solvents ratio is for 1:5, and water is pre-
Heat to 40 DEG C entrance counterflow extraction apparatus, cellulase addition 1g, counter-flow extraction time 2 h, ultrasonic
Extractor installs the water of 1000g in advance, is preheating to 40 DEG C, after having residue to enter ultrasonic extractor, opens
Ultrasonic probe, ultrasonic frequency is 40kHz, after 10min, is taken by extract bottom ultrasonic extraction device
Go out, be centrifuged off suspended particulate through filtration laggard, be pressurized to 3.0MPa and enter membrane module.Membrane module is selected
Have the reverse osmosis membrane of high cutoff performance to rabdosia lophanthide active component, under pressure-driven, moisture is through separating
Film, organized enzyme and rabdosia lophanthide active component in extract retained the most completely, and permeate solid content is less than
0.001%.
Control the operating parameter of membrane separating process, make the concentration of concentrate reach to feed the 5 of extract concentration
Times, concentrate enters countercurrent extractor, and fresh solvent enters ultrasonic extractor, and permeate returns to extract
Tank.Obtaining extract about 1800mL after extracting, in concentrate, solid content is 1.5%, and total solid is received
Rate (soluble solids thing total amount and the ratio of material quantity) is about 13.5%.
Result shows, the extracting method that the present embodiment provides can realize extracting operation, cellulose at low temperatures
Enzyme and counter-flow extraction are used in combination and can obtain higher rabdosia lophanthide activated product recovery rate.
Embodiment 2:
200g bletilla striata raw material enters counterflow extraction apparatus after broken, and Materials Solvents ratio is for 1:5, and water preheats
Entering counterflow extraction apparatus, cellulase and pectase addition 1g altogether to 40 DEG C, the counter-flow extraction time 2 is little
Time, ultrasonic extractor installs the water of 1000g in advance, is preheating to 40 DEG C, enters ultrasonic extractor when there being residue
After, open ultrasonic probe, ultrasonic frequency is 40kHz, after 10min, will bottom ultrasonic extraction device
Extract takes out, and is centrifuged off suspended particulate through filtration laggard, is pressurized to 3.0MPa and enters membrane module.Film group
Part is selected the reverse osmosis membrane to rabdosia lophanthide active component with high cutoff performance, under pressure-driven, moisture
Through separating film, organized enzyme and bletilla striata active component in extract are retained the most completely, contain through liquid-solid
Amount is less than 0.001%.
Control the operating parameter of membrane separating process, make the concentration of concentrate reach to feed the 5 of extract concentration
Times, concentrate enters countercurrent extractor, and fresh solvent enters ultrasonic extractor, and permeate returns to extract
Tank.Obtaining extract about 1850mL after extracting, in concentrate, solid content is 1.4%, and total solid is received
Rate (soluble solids thing total amount and the ratio of material quantity) is about 13.53%.
Result shows, the extracting method that the present embodiment provides can realize extracting operation, cellulose at low temperatures
Enzyme and counter-flow extraction are used in combination and can obtain higher bletilla striata activated product recovery rate.
Embodiment 3:
200g glossy ganoderma raw material enters counterflow extraction apparatus after broken, and Materials Solvents ratio is for 1:6, and water preheats
Counterflow extraction apparatus is entered to 50 DEG C, cellulase, pectase, papain addition 1.2g altogether, inverse
2 hours extraction times of stream, ultrasonic extractor installs the water of 1200g in advance, is preheating to 50 DEG C, when there being residue
After entering ultrasonic extractor, opening ultrasonic probe, ultrasonic frequency is 40kHz, after 10min, ultrasonic
Bottom extraction equipment, extract is taken out, after filtering and being centrifuged off suspended particulate, be pressurized to 3.0MPa and enter
Membrane module.Membrane module is selected the reverse osmosis membrane to active components of glossy ganoderma with high cutoff performance, drives at pressure
Under Dong, moisture is through separating film, and organized enzyme and active component in extract are retained the most completely, pass through
Fluid solid content is less than 0.001%.
Control the operating parameter of membrane separating process, make the concentration of concentrate reach to feed the 5 of extract concentration
Times, concentrate enters countercurrent extractor, and fresh solvent enters ultrasonic extractor, and permeate returns to extract
Tank.Obtaining extract about 2200mL after extracting, in concentrate, solid content is 1.5%, and total solid is received
Rate (soluble solids thing total amount and the ratio of material quantity) is about 16.5%.
Result shows, the extracting method that the present embodiment provides can realize extracting operation, cellulose at low temperatures
Enzyme and counter-flow extraction are used in combination and can obtain higher ganoderma active product recovery rate.
Embodiment 4:
200g raspberry raw material enters counterflow extraction apparatus after broken, and Materials Solvents ratio is for 1:6, and water is pre-
Heat to 50 DEG C enters counterflow extraction apparatus, cellulase, pectase, papain addition 1.2g altogether,
Counter-flow extraction time 2 h, ultrasonic extractor installs the water of 1200g in advance, is preheating to 50 DEG C, residual when having
After slag enters ultrasonic extractor, opening ultrasonic probe, ultrasonic frequency is 50kHz, after 10min, super
Bottom sound extraction equipment, extract is taken out, after filtering and being centrifuged off suspended particulate, be pressurized to 1.5MPa and enter
Enter membrane module.Membrane module is selected the NF membrane to raspberry active component with high cutoff performance, at pressure
Under driving, moisture is through separating film, and organized enzyme and active component in extract are retained, thoroughly the most completely
Cross fluid solid content less than 0.003%.
Control the operating parameter of membrane separating process, make the concentration of concentrate reach to feed the 5 of extract concentration
Times, concentrate enters countercurrent extractor, and fresh solvent enters ultrasonic extractor, and permeate returns to extract
Tank.Obtaining extract about 2200mL after extracting, in concentrate, solid content is 1.3%, and total solid is received
Rate (soluble solids thing total amount and the ratio of material quantity) is about 14.3%.
Result shows, the extracting method that the present embodiment provides can realize extracting operation, cellulose at low temperatures
Enzyme and counter-flow extraction are used in combination and can obtain higher raspberry activated product recovery rate.
Embodiment 5
200g raspberry raw material enters counterflow extraction apparatus after broken, and Materials Solvents ratio is for 1:1, and water is pre-
Heat to 15 DEG C enters counterflow extraction apparatus, and papain addition 0.2g, the counter-flow extraction time 0.5 is little
Time, ultrasonic extractor installs water so that residue is 1:1 with the mass ratio of water, is preheating to 15 DEG C, residual when having
After slag enters ultrasonic extractor, opening ultrasonic probe, ultrasonic frequency is 100kHz, after 2 hours, super
Bottom sound extraction equipment, extract is taken out, after filtering and being centrifuged off suspended particulate, be pressurized to 6.0MPa and enter
Enter membrane module.Membrane module is selected the reverse osmosis membrane to raspberry active component with high cutoff performance, in pressure
Under the conditions of power driving and temperature are 15 DEG C, moisture is through separating film, the organized enzyme in extract and active component
Being retained the most completely, permeate solid content is less than 0.001%.
Control the operating parameter of membrane separating process, make the concentration of concentrate reach to feed the 5 of extract concentration
Times, concentrate enters countercurrent extractor, and fresh solvent enters ultrasonic extractor, and permeate returns to extract
Tank.Obtaining extract about 2200mL after extracting, in concentrate, solid content is 1.4%, and total solid is received
Rate (soluble solids thing total amount and the ratio of material quantity) is about 14.66%.
Result shows, the extracting method that the present embodiment provides can realize extracting operation, cellulose at low temperatures
Enzyme and counter-flow extraction are used in combination and can obtain higher raspberry activated product recovery rate.
Embodiment 6
200g raspberry raw material enters counterflow extraction apparatus after broken, and Materials Solvents ratio is for 1:20, and water is pre-
Heat to 50 DEG C enters counterflow extraction apparatus, cellulase, pectase, papain addition 4g altogether, inverse
3 hours extraction times of stream, ultrasonic extractor installs water so that residue is 1:20 with the mass ratio of water, preheating
To 50 DEG C, after having residue to enter ultrasonic extractor, opening ultrasonic probe, ultrasonic frequency is 100kHz,
After 1 hour, bottom ultrasonic extraction device, extract is taken out, after filtering and being centrifuged off suspended particulate,
It is pressurized to 0.5MPa and enters membrane module, membrane module is selected raspberry active component is had high cutoff performance
NF membrane, under the conditions of pressure-driven and temperature are 50 DEG C, moisture is through separating film, the activity in extract
Enzyme and active component are retained the most completely, and permeate solid content is less than 0.003%.
Control the operating parameter of membrane separating process, make the concentration of concentrate reach to feed the 5 of extract concentration
Times, concentrate enters countercurrent extractor, and fresh solvent enters ultrasonic extractor, and permeate returns to extract
Tank.Obtaining extract about 2200mL after extracting, in concentrate, solid content is 1.5%, and total solid is received
Rate (soluble solids thing total amount and the ratio of material quantity) is about 15.95%.
Result shows, the extracting method that the present embodiment provides can realize extracting operation, cellulose at low temperatures
Enzyme and counter-flow extraction are used in combination and can obtain higher raspberry activated product recovery rate.
Comparative example 1:
200g rabdosia lophanthide raw material, through broken, enters pot type extraction equipment after sieving, water is preheating to 90 DEG C of entrance
Extraction equipment, Materials Solvents ratio for 1:5,2 hours extraction times, obtains extract about after extracting
1800mL, in concentrate, solid content is 0.8%, total solid yields (soluble solids thing total amount and material quantity
Ratio) it is about 7.2%.
Result shows, the conventional high temperature that this comparative example provides extracts the yield extraction less than embodiment 1 of process
Process.
Comparative example 2:
200g rabdosia lophanthide raw material, through broken, enters pot type extraction equipment after sieving, water is preheating to 40 DEG C of entrance
Extraction equipment, Materials Solvents ratio is for 1:5, and cellulase addition 1g, after 2 hours extraction times, water heats
Continuing to extract 1 hour to 90 DEG C, obtain extract about 1800mL after extracting, in concentrate, solid content is
1.0%, total solid yields (soluble solids thing total amount and the ratio of material quantity) is about 9%.
Result shows, the yield of the extraction process that this comparative example provides is less than the extraction process of embodiment 1.
Comparative example 3:
200g rabdosia lophanthide raw material, through broken, sieves, presoak laggard enter ultrasonic pot type extraction equipment, water preheats
Entering extraction equipments to 40 DEG C, Materials Solvents ratio is for 1:5, cellulase addition 1g, and extraction time 2 is little
Time, ultrasonic extractor installs the water of 1000g in advance, opens ultrasonic probe, and ultrasonic frequency is 40kHz,
After 10min, obtaining extract about 1800mL, in concentrate, solid content is 0.92%, and total solid yields (can
Molten solids total amount and the ratio of material quantity) it is about 10.35%.
Result shows, the yield of the extraction process that this comparative example provides is less than the extraction process of embodiment 1.
Comparative example 4:
200g rabdosia lophanthide raw material enters counterflow extraction apparatus after broken, and Materials Solvents ratio is for 1:5, and water is pre-
Heat to 40 DEG C enters counterflow extraction apparatus, cellulase addition 1g, counter-flow extraction time 2 h, passes through
Obtaining extract about 1800mL after extraction, in concentrate, solid content is 0.96%, and total solid yields is (solvable
Solids total amount and the ratio of material quantity) it is about 8.64%.
Result shows, the yield of the extraction process that this comparative example provides is less than the extraction process of embodiment 1.
Comparative example 5
In addition to counterflow extraction apparatus is replaced with pot type extraction equipment, remaining is same as in Example 1.
Obtaining extract about 1800mL after extracting, in concentrate, solid content is 0.9%, and total solid is received
Rate (soluble solids thing total amount and the ratio of material quantity) is about 8.1%.
Result shows, the yield of the extraction process that this comparative example provides is less than the extraction process of embodiment 1.
Comparative example 6
Except being not added with cellulase during extracting, remaining is same as in Example 1.
Obtaining extract about 1800mL after extracting, in concentrate, solid content is 0.85%, and total solid is received
Rate (soluble solids thing total amount and the ratio of material quantity) is about 7.65%.
Result shows, the yield of the extraction process that this comparative example provides is less than the extraction process of embodiment 1.
Owing to comparative example 1 is to use high temperature to extract, comparative example 2 is to use enzymolysis and extraction to combine high temperature to extract,
Comparative example 3 is low temperature ultrasonic enzymolysis assisted extraction, and comparative example 4 is low temperature adverse current enzymolysis assisted extraction, contrast
Example 5 is that low temperature ultrasonic enzymolysis film concentrates assisted extraction, and comparative example 6 is that low temperature adverse current ultrasonic film concentration auxiliary carries
Taking, after testing, in its concentrate obtained after finally concentrating, solid content and total solid yields will be the lowest
In embodiment 1.Thus can also illustrate that the natural prodcuts novel technology for extracting in the present invention achieves collaborative
Synergistic effect, and achieve the purpose that under cryogenic conditions, natural prodcuts active component high-recovery extracts.
Applicant states, the foregoing is only the detailed description of the invention of the present invention, but protection scope of the present invention
Being not limited thereto, person of ordinary skill in the field is it will be clearly understood that any skill belonging to the art
Art personnel in the technical scope that the invention discloses, the change that can readily occur in or replacement, all fall within the present invention
Protection domain and open within the scope of.
Claims (10)
1. a natural prodcuts active component extraction element, including counter-flow extraction unit, ultrasonic extraction unit
With film upgrading unit, it is characterised in that described device also includes that enzyme adds unit, enzyme adds unit and adverse current
Extraction unit connects, the solid discharge of counter-flow extraction unit and the material inlet to be extracted of ultrasonic extraction unit
Being connected, the extracting liquid outlet of ultrasonic extraction unit is connected with the liquid import to be separated of film upgrading unit, and film concentrates
The concentrated solution outlet of unit is connected with the solvent inlet of counter-flow extraction unit.
Device the most according to claim 1, it is characterised in that the waiting of described counter-flow extraction unit carries
Take material inlet to be connected with reducing mechanism；
Preferably, the extracting liquid outlet of described counter-flow extraction unit is connected with concentrate drying unit, described concentration
Drying unit is for concentrating the active component in extract and being dried；
Preferably, described enzyme addition unit is connected to the solvent in the middle part of counter-flow extraction unit with counter-flow extraction unit
Between inducer, preferably it is connected to the middle part of counter-flow extraction unit；
Preferably, between described ultrasonic extraction unit and film upgrading unit, it is provided with pretreatment unit, described pre-
Processing unit is for removing the solid impurity in the extract that ultrasonic extraction unit obtains；
Preferably, described pretreatment unit is centrifuge, micro-filtration or plate filter, is preferably centrifugal
Machine；
Preferably, the permeate outlet of described film upgrading unit is connected with the solvent inlet of ultrasonic extraction unit.
Device the most according to claim 1 and 2, it is characterised in that described counter-flow extraction unit is pipe
Road formula counterflow extraction apparatus and/or the most continuously pot group type counterflow extraction apparatus, preferably duct type adverse current carries
Taking equipment；
Preferably, described ultrasonic extraction unit is ultrasonic extractor；
Preferably, it is enzyme solutions material-compound tank and feed pump that described enzyme adds unit, and described feed pump carries with adverse current
Take unit to be connected；
Preferably, described film upgrading unit is that rolling diaphragm separator, tubular membrane separator or hollow-fibre membrane divide
Any one or the combination of at least two, preferably rolling diaphragm separator in device.
4. according to the device one of claim 1-3 Suo Shu, it is characterised in that in described film upgrading unit
Separating film is organic nanofiltration membrane and/or organic reverse osmosis membrane, preferably organic nanofiltration membrane；
Preferably, the molecular cut off of described organic nanofiltration membrane is 200-400；
Preferably, the material of described separation film be cellulose, cellulose acetate, SPSF, polyamide,
Any one or at least two in polyimides, polyether sulfone, sulfonated polyether sulfone, poly-piperazine or polyvinyl alcohol
Combination.
5. the method that the device utilizing one of claim 1-4 described extracts natural prodcuts active component, it is special
Levying and be, described method comprises the steps:
(1) by raw material to be extracted and solvent counter current contacting under the effect of organized enzyme, extract in raw material to be extracted
Active component, obtain the extract containing active component and residue；
(2) active component in ultrasonic extraction residue, the organized enzyme of absorption on desorption residue, is contained simultaneously
Active composition and the ultrasonic extract of organized enzyme；
(3) ultrasonic extract is carried out membrane separation concentration, obtain organized enzyme and the concentrate of active component and
Permeate, described concentrate is for completely or partially replacing the solvent in step (1).
Method the most according to claim 5, it is characterised in that the described raw material to be extracted of step (1)
For natural prodcuts, preferably Chinese medicine；
Preferably, the described raw material to be extracted of step (1) contacts with solvent counter current the most again.
7. according to the method described in claim 5 or 6, it is characterised in that step (1) described adverse current connects
Touch and carry out in duct type counterflow extraction apparatus and/or the most continuous pot group type counterflow extraction apparatus, be preferably
Duct type counterflow extraction apparatus；
Preferably, the described raw material to be extracted of step (1) is 1:1-1:20, preferably 1:5 with the mass ratio of solvent；
Preferably, the addition of step (1) described organized enzyme with the mass ratio of raw material to be extracted is
0.1-2%, preferably 0.6%；
Preferably, the organized enzyme described in step (1) is appointing in cellulase, pectase or papain
Anticipate a kind of or mixture of at least two；
Preferably, step (1) described organized enzyme adds at the leading portion extracted, and is preferably the stage casing extracting and adds
Enter；
Preferably, step (1) described organized enzyme is added in raw material to be extracted and solvent by feed pump；
Preferably, the temperature of step (1) described extraction is 15-50 DEG C, preferably 50 DEG C；
Preferably, the time of step (1) described extraction is 0.5-3 hour, preferably 2 hours；
Preferably, step (1) described extract carries out concentrate drying process, obtains active component.
8. according to the method one of claim 5-7 Suo Shu, it is characterised in that step (2) is described ultrasonic
It is extracted on ultrasonic extractor and carries out；
Preferably, the ultrasonic frequency range of the described ultrasonic extraction of step (2) is 20-100kHz, is preferably
40kHz；
Preferably, the temperature of the described ultrasonic extraction of step (2) is 15-50 DEG C, preferably 50 DEG C；
Preferably, the time of the described ultrasonic extraction of step (2) is 10 minutes-2 hours, preferably 1 hour；
Preferably, in the described ultrasonic extraction of step (2), residue is 1:1-1:20 with the mass ratio of solvent, preferably
For 1:5.
9. according to the method one of claim 5-8 Suo Shu, it is characterised in that first ultrasonic extract is carried out
Pretreatment carries out the membrane separation concentration described in step (3) again, and described pretreatment is centrifugal treating, micro-filtration or plate
Frame filter in any one or the combination of at least two, preferably centrifugal treating；
Preferably, step (3) described membrane separation concentration is in rolling diaphragm separator, tubular membrane separator or hollow
Carry out in any one or the combination of at least two in tunica fibrosa separator, be preferably at rolling diaphragm separator
On carry out；
Preferably, the membrane separation concentration described in step (3) is carried out under the pressure of 0.5-6.0MPa；
Preferably, the membrane separation concentration described in step (3) is carried out under conditions of 15-50 DEG C；
Preferably, the separation film that step (3) described membrane separation concentration uses is organic nanofiltration membrane or organic reverse osmosis
Permeable membrane, preferably organic nanofiltration membrane；
Preferably, the molecular cut off of described organic nanofiltration membrane is 200-400；
Preferably, the material of described separation film be cellulose, cellulose acetate, SPSF, polyamide,
Any one or at least two in polyimides, polyether sulfone, sulfonated polyether sulfone, poly-piperazine or polyvinyl alcohol
Combination；
Preferably, the permeate described in step (3) returns step (2).
10. according to the method one of claim 5-9 Suo Shu, it is characterised in that described method includes as follows
Step:
(1) raw material to be extracted mixes with solvent after crushing, to be extracted former subsequently into counterflow extraction apparatus
Material charging aperture, along counterflow extraction apparatus forward flow under additional power drive, fresh solvent is from counter-flow extraction
The solvent inlet of equipment opposite side enters, solvent and raw material counter current contacting mass transfer to be extracted, raw material to be extracted with
The mass ratio of solvent total amount is 1:1-1:20, and organized enzyme is from the middle part of counterflow extraction apparatus and counter-flow extraction unit
Solvent inlet section between position add counter-flow extraction unit, Extracting temperature is 15-50 DEG C, and organized enzyme adds
The mass ratio entering amount and raw material inlet to be extracted is 0.1-2%, and extraction time is 0.5-3 hour, is carried
Taking liquid and residue, extract, after the extracting liquid outlet of counterflow extraction apparatus is discharged, carries out concentrate drying,
To active component；
(2) ultrasonic extractor is used to extract the active component in residue further and desorb absorption at residue
On organized enzyme, the mass ratio of the residue in ultrasonic extractor and solvent is 1:1-1:20, and ultrasonic wave extracts
Temperature be 15-50 DEG C, ultrasonic wave extract ultrasonic frequency range be 20-100kHz, ultrasonic wave extract
Time is 0.5-2 hour, obtains the ultrasonic extract containing active component and organized enzyme；
(3) ultrasonic extract is after centrifugal treating, enters membrane separator, at the pressure of 0.5-6.0MPa
Drive and at a temperature of 15-50 DEG C, by membrane separator separation concentrated active ingredients and organized enzyme, obtain
Containing organized enzyme and the concentrate of active component and permeate, concentrate is for completely or partially replacing step
(1) fresh solvent in, permeate returns in the ultrasonic wave extraction equipment described in step (2) continuously.
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