CN102512959A - Method for separating enriched effective components from plant extract - Google Patents
Method for separating enriched effective components from plant extract Download PDFInfo
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- CN102512959A CN102512959A CN2011104486424A CN201110448642A CN102512959A CN 102512959 A CN102512959 A CN 102512959A CN 2011104486424 A CN2011104486424 A CN 2011104486424A CN 201110448642 A CN201110448642 A CN 201110448642A CN 102512959 A CN102512959 A CN 102512959A
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Abstract
The invention relates to a method for separating enriched effective components from plant extract, which is characterized in that a multi-stage tangential flow membrane filtration system consists of a first-stage tangential flow membrane ultrafiltration unit, a second-stage tangential flow membrane ultrafiltration unit and until an n-stage tangential flow membrane ultrafiltration unit which are sequentially connected in series. The method disclosed by the invention has the advantages of wide impurity removing range, high separation efficiency, less loss of effective components and small organic solvent and acid-base usage amount, and is easy and convenient to operate.
Description
Invention field
The present invention relates to a kind of from plant extraction liquid the method for separation and concentration active ingredient.
Background of invention
Plant extracts is to be raw material with the plant; According to needs to the purposes of the final products that extract; Extract separation process through physical chemistry; Orientation obtain and the plant of concentrating in a certain or plurality of active ingredients (like flavones, alkaloid, glucoside, acid, polyphenol, polysaccharide, terpene etc.), and do not change the product that its active ingredient structure forms.Plant extracts belongs to intermediate product, can be applied to the field such as raw material or auxiliary material of medicine, health food, tobacco, cosmetics, has extensive market prospects.At present, plant extract has developed into the new industry that an annual sales amount surpasses 10,000,000,000 dollars.Quality Control of Plant Extract usually adopts high performance liquid chromatography (HPLC), ultraviolet specrophotometer measuring apparatus percentage compositions a certain or several kinds of active ingredient monomers such as (UV) to confirm.How using the simplest method obtains highly purified plant extracts and is still the key issue in the commercial process.In the prior art, adopt technological means such as resin isolation, extraction to come active ingredient in the separation and concentration plant extracts liquid usually.The principle of resin isolation is through the active ingredient in the resin adsorption plant extracts liquid, through different solvents active ingredient dissolving of different nature is eluted, and realizes separating the purpose of different active ingredients.The defective of this method is: the one, and the organic solvent use amount is big; The 2nd, regeneration of resin need use soda acid and organic solvent, and is big for environment pollution, and the waste disposal energy resource consumption is big, cost is high; The 3rd, the solvent residual amount of finished product is high, influences the security that finished product uses.
Summary of the invention
The object of the present invention is to provide a kind of from plant extraction liquid the method for separation and concentration active ingredient.Separative efficiency is high, loss of effective components is few, the use amount of organic solvent and soda acid is few, simple to operation.
In order to achieve the above object, technical scheme of the present invention design is as follows:
A kind of from plant extraction liquid the method for separation and concentration active ingredient, it is characterized in that: adopt slipstream membrane filtration system classified filtering to separate.
Described a kind of from plant extraction liquid the method for separation and concentration active ingredient, it is characterized in that: multistage slipstream membrane filtration system is composed in series until n level slipstream film ultra filtration unit by one-level slipstream film ultra filtration unit, secondary slipstream film ultra filtration unit successively.
Described a kind of from plant extraction liquid the method for separation and concentration active ingredient, it is characterized in that: slipstream film ultra filtration unit comprises storage tank, slipstream film ultrafilter; Storage tank is connected with feed pipe, and the discharging opening of storage tank links to each other with the charging aperture of slipstream film ultrafilter through circulating pump; The trapped fluid outlet of slipstream film ultrafilter links to each other with the storage tank charging aperture through return duct; The filtrate (liquid of slipstream film ultrafilter links to each other through the charging aperture of discharge nozzle with next stage slipstream film ultra filtration unit.
Ultrafiltration is the relevant screening process of a kind of and membrane aperture size, is driving force with the pressure differential of film both sides, is filter medium with the milipore filter; Under certain pressure; When stoste flow through the film surface, the many tiny micropore that gathers in the milipore filter surface only allowed water and small-molecule substance through becoming through liquid, and volume then is trapped within the liquid feeding side of film in the stoste greater than the material in film surface micro aperture; Become concentrate, thus realize to stoste purification, separation and concentrated purpose.
Ultrafiltration stoste refers generally to need to purify, separate or concentrated solution, and by that part of liquid of the big molecule solute of filtering, concentrate then is because of isolating through the remaining highly concentrated solution of liquid in the stoste through liquid refers to see through milipore filter in the stoste.Ultrafiltration is one type that filters, and the pore diameter range that typically refers to filter membrane is 0.001-0.1um (1kD-1000kD), and this filter membrane aperture is little; Can improve the purity of filtered fluid, if but in the plant extracts suitability for industrialized production, directly adopt milipore filter vertically to filter, all fluids directly pass through filter membrane; The material that is trapped is piled up in the film surface, forms filter cake, stops up filter opening; Increase along with filter cake thickness; Flow through filter membrane descends rapidly until stopping fully, and filter efficiency is low, therefore in the plant extracts suitability for industrialized production, does not promote the use of milipore filter as yet.(Ultrafiltration is the method that the nano sized particles in the solution and shla molecule are separated UF), and this separation is mainly based on bulk of molecule, but the permeability of filter membrane medium also can receive the influence of chemistry, molecule and the charge characteristic of sample in ultrafiltration.Which size ultrafiltration can only separate usually differs the doubly above molecule of 3-5, and is not suitable for separating the little molecule of size differences.
The cross-flow ultrafiltration technology is an emerging technology of inventing in recent years; Principle is that liquid tangential (parallel) is in the milipore filter surface; Has tangential cleaning effect; This cleaning effect has avoided the material of membrane retention to form filter cake on the film surface, and promptly so-called " concentration polarization ", characteristics are effectively to keep the unimpeded state of filter opening.The cross-flow ultrafiltration technology is widely used in biological products, and from the clarification of bacterium and cell culture fluid with concentrate, the displacement of buffer solution and the separation of target molecule all are very crucial technology in the separation and purification process.Yet should technology in the plant extracts suitability for industrialized production, not use as yet, through twice filtration and slipstream technology milipore filter is used more widely in the plant extracts commercial production and becomes a reality, improve plant extracts extraction efficiency and quality, do not appear in the newspapers as yet.
The cross-flow ultrafiltration technology is a kind of membrane separation technique of present common employing, belongs to the tangential flow filtration of molecular weight level, usually molecular cut off scope: 1-1000kD.
Of the present invention a kind of from plant extraction liquid the method and technology effect of separation and concentration active ingredient following:
The one, the removal of impurities scope is wide, can hold back all materials bigger than milipore filter pore-size.
The 2nd, separative efficiency is high.The traditional filtering separation need regularly be removed filter cake, and workload is big, and downtime is long.Separation method according to the invention is owing to the slipstream effect, and the filter membrane surface can not produce filter cake, can realize continuing lock out operation, and separative efficiency is high.
The 3rd, loss of effective components is few.The prior resin separation at first is adsorbed on active ingredient on the resin, and then the active ingredient that will be adsorbed on the resin through solvent elutes.Because resin use amount restriction in the adsorption process, a collection of extract need be divided into repeatedly and adsorbing, and behind the wash-out, all has the active ingredient of 1-2% can remain in the resin at every turn, can not effectively reclaim, and accumulation causes loss of effective components bigger.Separation method according to the invention is owing to get trapped fluid in separation process and then do not have loss of effective components, and realizes continued operation, and disposal ability is big, gets the also loss of active ingredients of 1-2% for once of filtrating.
The 4th, the use amount of organic solvent and soda acid is few.Resin isolation need be used resin volume 2-4 organic solvent doubly during wash-out, need resin volume organic solvent and soda acid more than 2 times during regeneration.When method for separating and concentrating according to the invention filters; Extract directly separates through membrane filtration, has saved the organic solvent and the soda acid of wash-out and regenerating resin, has practiced thrift running cost; Reduced disposal of pollutants; Environmental pollution is little, and the finished product organic solvent residual is few, has improved the quality and the security of finished product.
The 5th, simple to operation.Resin isolation comprises absorption, wash-out, regeneration, and absorption needs the concentration of adjustment extract, to meet the resin adsorption requirement.Resin demand, solvent load etc. need strict calculating, and absorption, wash-out, regeneration can only intermittently operated.When method for separating and concentrating according to the invention filters, continued operation can be realized, certain concentration need be do not adjusted, simple to operation, less energy consumption.
Below through specifically describe technique effect of the present invention through contrast test.
Contrast test 1: separation and concentration total triterpene acid from the loguat leaf ethanol extract.
Get the dried loguat leaf of 1kg, process 20 liters of loguat leaf ethanol extracts, get 10 liters of loguat leaf ethanol extracts respectively, carry out the separation and concentration total triterpene acid with the absorption of Anhui Samsung D101 macroporous absorbent resin and the inventive method Germany Sai Duolisi milipore filter.Separating effect sees the following form:
Contrast test 2: separation and concentration total triterpene acid from the oldenlandia diffusa ethanol extract.
Get the 1kg oldenlandia diffusa, process 20 liters of oldenlandia diffusa ethanol extracts, get 10 liters of oldenlandia diffusa ethanol extracts respectively, rubbing with Shanghai, fast D101 macroporous absorbent resin adsorbs and the inventive method Germany Sai Duolisi milipore filter carries out the separation and concentration total triterpene acid.Separating effect sees the following form:
Contrast test 3: separation and concentration capsicim from the pimiento aqueous extract.
Get the dry pimiento of 1kg, process 20 liters of pimiento aqueous extracts, get 10 liters of pimiento aqueous extracts respectively, rubbing with Shanghai, fast D101 macroporous absorbent resin adsorbs and the inventive method Germany Sai Duolisi milipore filter carries out the separation and concentration capsicim.Separating effect sees the following form:
Contrast test 4: separation and concentration general flavone from bamboo leaf aqueous extract.
Get the dry bamboo leaf of 1kg, process 20 liters of bamboo leaf aqueous extracts, get 10 liters of bamboo leaf aqueous extracts respectively, rubbing with Shanghai, fast D101 macroporous absorbent resin adsorbs and the inventive method Germany Sai Duolisi milipore filter carries out the separation and concentration general flavone.Separating effect sees the following form:
Contrast test 5: separation and concentration anthocyanin from the perilla leaf ethanol extract.
Get the dry perilla leaf of 1kg, process 20 liters of perilla leaf ethanol extracts, get 10 liters of perilla leaf ethanol extracts respectively, rubbing with Shanghai, fast D101 macroporous absorbent resin adsorbs and the inventive method Germany Sai Duolisi milipore filter carries out the separation and concentration anthocyanin.Separating effect sees the following form:
Contrast test 6: separation and concentration phytochrome from the leaf of spinach ethanol extract.
Get the fresh the leaf of spinach of 1kg, process 20 liters of the leaf of spinach ethanol extracts, get 10 liters of the leaf of spinach ethanol extracts respectively, rubbing with Shanghai, fast D101 macroporous absorbent resin adsorbs and the inventive method Germany Sai Duolisi milipore filter carries out the separation and concentration phytochrome.Separating effect sees the following form:
Contrast test 7: separation and concentration cardigin from the digitalis folia ethanol extract.
Get the dry digitalis folia of 1kg, process 20 liters of digitalis folia ethanol extracts, get 10 liters of digitalis folia ethanol extracts respectively, rubbing with Shanghai, fast D101 macroporous absorbent resin adsorbs and the inventive method Germany Sai Duolisi milipore filter carries out the separation and concentration cardigin.Separating effect sees the following form:
Contrast test 8: the total naphthoquinones of separation and concentration Asian puccoon from the Asian puccoon ethanol extract.
Get the dry alkanet of 1kg, process 20 liters of Asian puccoon ethanol extracts, get 10 liters of alkanet ethanol extracts respectively, rubbing with Shanghai, fast D101 macroporous absorbent resin adsorbs and the inventive method Germany Sai Duolisi milipore filter carries out the total naphthoquinones of separation and concentration Asian puccoon.Separating effect sees the following form:
Contrast test 9: separation and concentration giant knotweed rhizome general anthraquinone from the perilla leaf ethanol extract.
Get the dry giant knotweed of 1kg, process 20 liters of perilla leaf ethanol extracts, get 10 liters of giant knotweed ethanol extracts respectively, rubbing with Shanghai, fast D101 macroporous absorbent resin adsorbs and the inventive method Germany Sai Duolisi milipore filter carries out the separation and concentration giant knotweed rhizome general anthraquinone.Separating effect sees the following form:
Contrast test 10: separation and concentration asiatic centella total saponins from the centella ethanol extract.
Get the 1kg centella, process 20 liters of centella ethanol extracts, get 10 liters of centella ethanol extracts respectively, rubbing with Shanghai, fast D101 macroporous absorbent resin adsorbs and the inventive method Germany Sai Duolisi milipore filter carries out the separation and concentration asiatic centella total saponins.Separating effect sees the following form:
Description of drawings
Accompanying drawing is multistage slipstream membrane filtration process principle figure
The implication of each label is following among the figure: A1-one-level slipstream film ultra filtration unit, A2-secondary slipstream film ultra filtration unit ... An-n level slipstream film ultra filtration unit.1-storage tank, 2-circulating pump, 3-slipstream film ultrafilter, 4-feed pipe, 5-discharge nozzle, 6-return duct.
The specific embodiment
Embodiment 1: from loguat leaf, extract the method for separating the total triterpene acid pregnant solution
First step water extracts: get dry loguat leaf meal 2kg, add 20L water, mix, be heated to 100 degree, boiled 60 minutes, be cooled to below 60 degree, discard the water extract, stay the dregs of a decoction subsequent use;
The second step alcohol extract: the dregs of a decoction and 95% ethanol are added in the reflux, and heating and extracting was taken out extract after 1 hour, and the dregs of a decoction are stayed in the reflux and extracted next time; So repetitive operation is 3 times; Each 95% ethanol 20L that adds, 3 times ethanol extracts merging is subsequent use, discard the dregs of a decoction;
The 3rd step coarse filtration: use industrial filter cloth ethanol extract to be filtered, discard filter residue, filtrate for later use as medium;
The once smart filter of the 4th step: it is that the sulfonated polysulfone membrane of 0.01 μ m adopts the tangential flow filtration mode to filter that filtrating is used the aperture, is trapped within mother liquor greater than the material of 10kD (kilodalton) and stays and use it for anything else, and filtrating is the total triterpene acid pregnant solution of 0.6mg/ml concentration;
The smart filter of the 5th step secondary: concentration is that to use the aperture be that the sulfonated polysulfone membrane of 0.003 μ m adopts the tangential flow filtration mode to filter to the total triterpene acid pregnant solution of 0.6mg/ml; Be trapped within mother liquor greater than the material of 3kD (kilodalton) and stay and use it for anything else, filtrating is the total triterpene acid pregnant solution of 1.2mg/ml concentration;
Embodiment 2: from oldenlandia diffusa, extract the method for separating the total triterpene acid pregnant solution
First step water extracts: get dry oldenlandia diffusa meal 2kg, add 20L water, mix, be heated to 100 degree, boiled 60 minutes, be cooled to below 60 degree, discard the water extract, stay the dregs of a decoction subsequent use;
The second step alcohol extract: the dregs of a decoction and 95% ethanol are added in the reflux, and heating and extracting was taken out extract after 1 hour, and the dregs of a decoction are stayed in the reflux and extracted next time; So repetitive operation is 3 times; Each 95% ethanol 20L that adds, 3 times ethanol extracts merging is subsequent use, discard the dregs of a decoction;
The 3rd step coarse filtration: use industrial filter cloth ethanol extract to be filtered, discard filter residue, filtrate for later use as medium;
The once smart filter of the 4th step: it is that the polyether-ketone film of 0.01 μ m adopts the tangential flow filtration mode to filter that filtrating is used the aperture, is trapped within mother liquor greater than the material of 10kD (kilodalton) and stays and use it for anything else, and filtrating is the total triterpene acid pregnant solution of 0.7mg/ml concentration;
The smart filter of the 5th step secondary: concentration is that to use the aperture be that the polyether-ketone film of 0.003 μ m adopts the tangential flow filtration mode to filter to the total triterpene acid pregnant solution of 0.7mg/ml; Be trapped within mother liquor greater than the material of 3kD (kilodalton) and stay and use it for anything else, filtrating is the total triterpene acid pregnant solution of 1.5mg/ml concentration.
Embodiment 3: the method for from pimiento, extracting capsicum red pigment and capsicim
First step water extracts: the pimiento meal 2kg and the water 20L of drying are added in the extractor, be heated to 100 degree, kept fluidized state 1 hour; Be cooled to 60 degree Celsius; Emit extract, the material slag stays in the jar and extracts next time, so repeats heating and extracting 3 times; 3 times aqueous extracts merging is subsequent use, discard the material slag;
The second step coarse filtration: use industrial filter cloth aqueous extract to be filtered, discard filter residue, filtrate for later use as medium;
The smart filter of the 3rd step: it is that the ceramic membrane of 0.003 μ m adopts the tangential flow filtration mode to filter that filtrating is used the aperture, is trapped within mother liquor greater than the capsicum red pigment of 3kD (kilodalton) and stays and use it for anything else, and filtrating is the capsicim pregnant solution of 1.3mg/ml concentration;
Embodiment 4: from the bamboo leaf, extract the method for separating general flavone
First step water extracts: the bamboo leaf meal 2kg and the water 20L of drying are added in the extractor, be heated to 100 degree, kept fluidized state 1 hour; Be cooled to 60 degree Celsius; Emit extract, the material slag stays in the jar and extracts next time, so repeats heating and extracting 3 times; 3 times aqueous extracts merging is subsequent use, discard the material slag;
The second step coarse filtration: use industrial filter cloth aqueous extract to be filtered, discard filter residue, filtrate for later use as medium;
The once smart filter of the 3rd step: it is that the copolyether sulfone film of 0.01 μ m adopts the tangential flow filtration mode to filter that filtrating is used the aperture, is trapped within mother liquor greater than the material of 10kD (kilodalton) and stays and use it for anything else, and filtrating is the general flavone pregnant solution of 0.5mg/ml concentration;
The smart filter of the 4th step secondary: it is that the copolyether film of 0.001 μ m adopts the tangential flow filtration mode to filter that filtrating is used the aperture, is trapped within mother liquor greater than the general flavone of 1kD (kilodalton), and filtrating is stayed and used it for anything else;
Embodiment 5: the method for from perilla leaf, extracting anthocyanin
First step alcohol extract: the perilla leaf meal 2kg and 90% ethanol of drying are added in the reflux; Heating and extracting was taken out extract after 1 hour; The dregs of a decoction are stayed in the reflux and are extracted next time, and so repetitive operation is 3 times, adds 90% ethanol 20L at every turn; 3 times ethanol extracts merging is subsequent use, discard the dregs of a decoction;
The second step coarse filtration: use industrial filter cloth ethanol extract to be filtered, discard filter residue, filtrate for later use as medium;
The once smart filter of the 3rd step: it is that the polyacrylonitrile film of 0.01 μ m adopts the tangential flow filtration mode to filter that filtrating is used the aperture, is trapped within mother liquor greater than the material of 10kD (kilodalton) and stays and use it for anything else, and filtrating is the anthocyanin pregnant solution of 0.6mg/ml concentration;
The smart filter of the 4th step secondary: concentration is that to use the aperture be that the polyacrylonitrile film of 0.001 μ m adopts the tangential flow filtration mode to filter to the anthocyanin pregnant solution of 0.6mg/ml; Be trapped within mother liquor greater than the material of 1kD (kilodalton) and stay and use it for anything else, filtrating is the anthocyanin pregnant solution of 1.3mg/ml concentration;
Instance 6: the method for from fresh spinach, extracting phytochrome
First step alcohol extract: fresh spinach fragment 2kg and 90% ethanol are added in the reflux; Heating and extracting was taken out extract after 1 hour; The dregs of a decoction are stayed in the reflux and are extracted next time, and so repetitive operation is 3 times, adds 90% ethanol 20L at every turn; 3 times ethanol extracts merging is subsequent use, discard the material slag;
The second step coarse filtration: use industrial filter cloth ethanol extract to be filtered, discard filter residue, filtrate for later use as medium;
The once smart filter of the 3rd step: it is that the polyethylene film of 0.01 μ m adopts the tangential flow filtration mode to filter that filtrating is used the aperture, is trapped within mother liquor greater than the material of 10kD (kilodalton) and stays and use it for anything else, and filtrating is the phytochrome pregnant solution of 0.004mg/ml concentration;
The smart filter of the 4th step secondary: concentration is that to use the aperture be that the polyethylene film of 0.001 μ m adopts the tangential flow filtration mode to filter to the phytochrome pregnant solution of 0.004mg/ml; Be trapped within mother liquor greater than the material of 1kD (kilodalton) and stay and use it for anything else, filtrating is the phytochrome pregnant solution of 0.007mg/ml concentration;
Instance 7: the method for from digitalis folia, extracting cardigin
First step alcohol extract: dry digitalis folia meal 2kg and 75% ethanol are added in the reflux; Heating and extracting was taken out extract after 1 hour; The dregs of a decoction are stayed in the reflux and are extracted next time, and so repetitive operation is 3 times, adds 75% ethanol 20L at every turn; 3 times ethanol extracts merging is subsequent use, discard the material slag;
The second step coarse filtration: use industrial filter cloth ethanol extract to be filtered, discard filter residue, filtrate for later use as medium;
The once smart filter of the 3rd step: it is that the polyethylene film of 0.01 μ m adopts the tangential flow filtration mode to filter that filtrating is used the aperture, is trapped within mother liquor greater than the material of 10kD (kilodalton) and stays and use it for anything else, and filtrating is the cardigin pregnant solution of 0.2mg/ml concentration;
The smart filter of the 4th step secondary: concentration is that to use the aperture be that the polyethylene film of 0.001 μ m adopts the tangential flow filtration mode to filter to total saponin(e pregnant solution of 0.2mg/ml; Be trapped within mother liquor greater than the material of 1kD (kilodalton) and stay and use it for anything else, filtrating is the cardigin pregnant solution of 0.5mg/ml concentration;
Instance 8: the method for from alkanet, extracting the total naphthoquinones of Asian puccoon
First step alcohol extract: dry alkanet meal 2kg and 90% ethanol are added in the reflux; Heating and extracting was taken out extract after 1 hour; The dregs of a decoction are stayed in the reflux and are extracted next time, and so repetitive operation is 3 times, adds 90% ethanol 20L at every turn; 3 times ethanol extracts merging is subsequent use, discard the material slag;
The second step coarse filtration: use industrial filter cloth ethanol extract to be filtered, discard filter residue, filtrate for later use as medium;
The once smart filter of the 3rd step: it is that the polyethylene film of 0.01 μ m adopts the tangential flow filtration mode to filter that filtrating is used the aperture, is trapped within mother liquor greater than the material of 10kD (kilodalton) and stays and use it for anything else, and filtrating is total naphthoquinones pregnant solution of 0.35mg/ml concentration;
The smart filter of the 4th step secondary: concentration is that to use the aperture be that the polyethylene film of 0.001 μ m adopts the tangential flow filtration mode to filter to total naphthoquinones pregnant solution of 0.35mg/ml; Be trapped within mother liquor greater than the material of 1kD (kilodalton) and stay and use it for anything else, filtrating is total naphthoquinones pregnant solution of 0.8mg/ml concentration;
Instance 9: the method for from giant knotweed, extracting giant knotweed rhizome general anthraquinone
First step alcohol extract: dry giant knotweed meal 2kg and 80% ethanol are added in the reflux; Heating and extracting was taken out extract after 1 hour; The dregs of a decoction are stayed in the reflux and are extracted next time, and so repetitive operation is 3 times, adds 80% ethanol 20L at every turn; 3 times ethanol extracts merging is subsequent use, discard the material slag;
The second step coarse filtration: use industrial filter cloth ethanol extract to be filtered, discard filter residue, filtrate for later use as medium;
The once smart filter of the 3rd step: it is that the polyethylene film of 0.01 μ m adopts the tangential flow filtration mode to filter that filtrating is used the aperture, is trapped within mother liquor greater than the material of 10kD (kilodalton) and stays and use it for anything else, and filtrating is the general anthraquinone pregnant solution of 0.8mg/ml concentration;
The smart filter of the 4th step secondary: concentration is that to use the aperture be that the polyethylene film of 0.001 μ m adopts the tangential flow filtration mode to filter to the general anthraquinone pregnant solution of 0.8mg/ml; Be trapped within mother liquor greater than the material of 1kD (kilodalton) and stay and use it for anything else, filtrating is the general anthraquinone pregnant solution of 1.6mg/ml concentration;
Instance 10: the method for extracting asiatic centella total saponins from centella
First step alcohol extract: dry centella herb meal 2kg and 75% ethanol are added in the reflux; Heating and extracting was taken out extract after 1 hour; The dregs of a decoction are stayed in the reflux and are extracted next time, and so repetitive operation is 3 times, adds 75% ethanol 20L at every turn; 3 times ethanol extracts merging is subsequent use, discard the material slag;
The second step coarse filtration: use industrial filter cloth ethanol extract to be filtered, discard filter residue, filtrate for later use as medium;
The once smart filter of the 3rd step: it is that the polyethylene film of 0.01 μ m adopts the tangential flow filtration mode to filter that filtrating is used the aperture, is trapped within mother liquor greater than the material of 10kD (kilodalton) and stays and use it for anything else, and filtrating is the asiatic centella total saponins pregnant solution of 1.8mg/ml concentration;
The smart filter of the 4th step secondary: concentration is that to use the aperture be that the polyethylene film of 0.001 μ m adopts the tangential flow filtration mode to filter to the asiatic centella total saponins pregnant solution of 1.4mg/ml; Be trapped within mother liquor greater than the material of 1kD (kilodalton) and stay and use it for anything else, filtrating is the asiatic centella total saponins pregnant solution of 3.0mg/ml concentration;
According to process principle figure the present invention is further specified below.
Shown in accompanying drawing, multistage slipstream membrane filtration system comprises one-level slipstream film ultra filtration unit A1, the secondary slipstream film ultra filtration unit A2......n level slipstream film ultra filtration unit An of series connection successively.
The slipstream membrane filtration system process structure of each grade is following: feed liquid gets into storage tank 1 through feed pipe 4, and the discharging opening of storage tank 1 links to each other with the charging aperture of slipstream film ultrafilter 3 through circulating pump 2.The trapped fluid outlet of slipstream film ultrafilter 3 links to each other with the storage tank charging aperture through return duct 6.The filtrate (liquid of slipstream film ultrafilter 3 links to each other with the charging aperture of next stage slipstream film ultra filtration unit.
Carrying out one-level through one-level slipstream film ultra filtration unit A1 filters.Plant extraction liquid enters into storage tank 1 through feed pipe 4 after the removal of impurities; ON cycle pump 2 pumps into slipstream film ultrafilter 3 with plant extraction liquid; Filtrating is through the storage tank 1 of discharge nozzle 5 entering next stage unit, and trapped fluid is carried back storage tank 1 through return duct 6, and carries out circulating filtration again through circulating pump 2; In trapped fluid, can leach with filtrating more than 98%, accomplish the ultrafiltration of one-level slipstream film through the material of milipore filter.Next, filtrating gets into secondary and carries out the ultrafiltration of secondary slipstream film to stream film ultra filtration unit A2, gets into n level slipstream film ultra filtration unit An until filtrating by that analogy and carries out the ultrafiltration of n level slipstream film.
Claims (3)
1. the method for a separation and concentration active ingredient from plant extraction liquid is characterized in that: adopt slipstream membrane filtration system classified filtering to separate.
2. according to claim 1 a kind of from plant extraction liquid the method for separation and concentration active ingredient, it is characterized in that: multistage slipstream membrane filtration system is composed in series until n level slipstream film ultra filtration unit (An) by one-level slipstream film ultra filtration unit (A1), secondary slipstream film ultra filtration unit (A2) successively.
3. according to claim 1 a kind of from plant extraction liquid the method for separation and concentration active ingredient, it is characterized in that: slipstream film ultra filtration unit comprises storage tank (1), slipstream film ultrafilter (3); Storage tank (1) is connected with feed pipe (4), and the discharging opening of storage tank (1) links to each other with the charging aperture of slipstream film ultrafilter (3) through circulating pump (2); The trapped fluid outlet of slipstream film ultrafilter (3) links to each other with storage tank (1) charging aperture through return duct (6); The filtrate (liquid of slipstream film ultrafilter (3) links to each other through the charging aperture of discharge nozzle (5) with next stage slipstream film ultra filtration unit.
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| CN110776138A (en) * | 2019-10-31 | 2020-02-11 | 南京工大膜应用技术研究所有限公司 | Membrane treatment device and method for steel pickling wastewater |
| CN111304049A (en) * | 2019-12-09 | 2020-06-19 | 华中科技大学 | Extracellular vesicle circulating separation and purification platform and method |
| WO2021209667A1 (en) * | 2020-04-15 | 2021-10-21 | Euromed, S.A. | Method for obtaining a botanical extract |
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| CN110776138B (en) * | 2019-10-31 | 2021-12-24 | 南京工大膜应用技术研究所有限公司 | Membrane treatment device and method for steel pickling wastewater |
| CN111304049A (en) * | 2019-12-09 | 2020-06-19 | 华中科技大学 | Extracellular vesicle circulating separation and purification platform and method |
| WO2021209667A1 (en) * | 2020-04-15 | 2021-10-21 | Euromed, S.A. | Method for obtaining a botanical extract |
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