CN104151380A - Preparation method of high-purity rutin - Google Patents
Preparation method of high-purity rutin Download PDFInfo
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- CN104151380A CN104151380A CN201410281429.2A CN201410281429A CN104151380A CN 104151380 A CN104151380 A CN 104151380A CN 201410281429 A CN201410281429 A CN 201410281429A CN 104151380 A CN104151380 A CN 104151380A
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Abstract
The invention provides a preparation method of high-purity rutin. The method comprises the following steps: grinding a rutin-containing raw material, enzymatically hydrolyzing, filtering, performing stirring extraction on filter residues at a certain temperature by using alcohol, and filtering to obtain rutin extract liquid; adsorbing the rutin-containing extract liquid by using a separation medium, eluting, collecting rutin-containing fraction, concentrating, and filtering to obtain a high-purity rutin product. The used production process is nontoxic, safe, short in process time, free of environmental pollution, simple and convenient to operate and easy for industrialization; the product is high in yield and good in purity; the development needs of drugs taking various kinds of rutin as raw materials can be met.
Description
Technical field
The present invention relates to a kind of preparation method of high-purity rutoside, more specifically, the present invention relates to extract the method for preparing high-purity rutoside from vegetable material.
Background technology
Rutin (Rutin) claim again violaguercitrin, for buff powder or superfine needle crystal, the crystal water that contains 3 molecules, fusing point is 174～178 DEG C, and 188～190 DEG C of anhydrides, are extensively present in vegitabilia, rutin raw material sources can be from Remote Lemongrass Herb, buckwheat (comprising cauline leaf, flower), Herba Hyperici, cursor hooks youngster rattan, Cortex malloti japonici leaf, Chinese ilex, the capsule of weeping forsythia, the sophora bud, the plants such as outstanding graceful eucalyptus leaves, especially the highest taking content in Flos Sophorae Immaturus (as the unopened bud of plant SophorajaponicaL) and buckwheat, can be used as the raw materials of a large amount of extraction rutins.The structure of rutin is as follows:
At present, China rutin produces and mainly extracts taking the sophora bud (bud of sophora flower) as raw material.Because rutin is in all kinds of SOLVENTS, solvability is very poor, is soluble in alkali lye and is yellow, after acidifying, separates out again.And other composition trochols in the sophora bud, sophoradiol, Flos Sophorae Immaturus first element, second element, the third element is without phenolic hydroxyl group, so do not dissolve in alkali lye, other polyoses in the sophora bud also do not dissolve.Therefore the topmost method of extracting rutin from the sophora bud is that thermokalite extracts acid precipitation method, exactly thick sophora bud powder is added to borax, S-WAT, enough saturated limewaters, pH value is adjusted to 8～9, is heated to boil, keep 50min, maintain pH=7, after heat filter, filtrate is adjusted to pH=4 with hydrochloric acid, leaves standstill 5 hours, suction filtration, be washed to neutrality, 70～80 DEG C dry, makes rutin.But its environment protection treating expense is large, and earning rate is low, yield low (8-12%), serious waste sophora bud resource.Be regarded as for many years comparatively ideal method always.And this technique needs to use a large amount of saturated limewater (buck) and hydrochloric acid in leaching process, and extract after acid-base waste fluid can not reclaim, need to administer, and then can produce huge wastewater treatment expense, do not administer and can cause great destruction to environment.According to the preliminary statistics for industrial scale generally the 1000 tons of sophora bud/years, produce the rutin producer of 200 tons of left and right, the waste water that produce every day is about more than 30 tons, annual sewage disposal expense is just up to units up to a million.
Along with country is more and more higher to the requirement of environmental protection, and the appearance of Extraction of rutin new technology, original extractive technique has gradually become a relative backward technology.Extract in order to solve industrialization the serious negative impact that rutin brings to environment, reduce the discharge of the three wastes, extract in the industry expert and also want to have use up various ways, but be all after obtaining rutin crude product substantially, then be further purified.But because the limitation of rutin solubleness, then dissolving is very difficult, need to expend a large amount of solvents and the energy.Production rutin technique is being explored by my company, when overcoming the defect of technique in the past, utilize enzyme engineering technology, by enzyme reaction gentleness plant tissue is decomposed, accelerating the release of effective constituent extracts, select suitable enzyme the impurity that affects liquid preparation clarity can be decomposed and removes as starch, protein, pectin etc., and many for part fat-soluble component, by glucuroide or transglucosidase, make fat-soluble component change into water-soluble glycoside, rutin as solid filtering out, obtains liquid glucose after filtration; The concentrated solid substance of useless sugar after filtration reaches the 30-50% of raw material, whole production technique is only solvent with alcohol and water, adopt separating medium to remove this thinking of impurity purifying, not only more than extraction rate reached to 20%, the rate of recovery reaches more than 85%, content is more than 95% rutin crystallization, but also overcome the pollution problem to environment of the three wastes that alkali extraction and acid precipitation technique produces.And solvent can completely reclaim and reuse, not only reduce production cost, and welding not, really realize the new situation processing of economy and environment harmonious development.
Summary of the invention
The object of the present invention is to provide a kind of method of efficient low-consume, extraction purifying high-purity rutin easy and simple to handle.
Another object of the present invention is to provide a kind of high-content rutin product, its content is greater than 98%, and residue on ignition is less than 2%, and Quercetin is less than 2%, and the rate of recovery is more than 85%, and yield is more than 20%.
Another object of the present invention is to overcome the defect of prior art, behave and provide a kind of raw material to be easy to get, product, without complex steps such as recrystallization processing, directly obtains rutin sterling more than GB.Whole production process, yield is high, good product purity, production technique is nontoxic, safety, the process time is short, non-environmental-pollution.Meanwhile, the waste saccharide liquid after enzymolysis transforms into nutrient fodder after reclaiming, and sells feed producer, does forage feed domestic animal, and sophora bud resource is fully utilized, and without three industrial wastes, has really accomplished recycling economy, the object of Sustainable development.
For achieving the above object, the present invention realizes by following technical proposals.The processing method of extraction rutin of the present invention comprises:
A. obtain Extraction of rutin liquid.
B. use separating medium to carry out fractionation by adsorption to described containing Extraction of rutin liquid, with the alcohol wash-out separating medium of 1-8 times of volume, collect and merge stream part of containing rutin, obtain elutriant.
C. concentrate eluant, filters, dry, obtains rutin sterling.
The Extraction of rutin liquid of mentioning in the present invention obtains in the following manner: will contain rutin raw material pulverizing, sieve, raw material powder adds distilled water, regulates pH to 4.0-6.0, add a certain amount of compound enzymic preparation, at 40-60 DEG C of enzymolysis 1-6 hour, filter, then filter residue is according to raw material: the weight/volume of alcohol=1:5～20, at a certain temperature, stir and extract, filter, obtain Extraction of rutin liquid.
In the present invention, a kind of compound enzymic preparation of mentioning, is characterized in that: the component that comprises following weight part:
Cellulase 1-5 part
Proteolytic enzyme 1-5 part
Amylase 1-5 part
Described proteolytic enzyme is selected at least one in papoid, Sumizyme MP, neutral protease.Described amylase is selected at least one in mesophilicα-diastase and beta-amylase.
The application of above-mentioned prozyme for extracting rutin flavones.
In extraction rutin Flavonoids Method above-mentioned, described plant is pulverized at 40-100 order, and vegetable material is 1:8-30 with the mass ratio of the distilled water adding.
Enzyme addition described in steps A is the 0.01-1% of plant material addition.
The present invention selects the principle of zymin to be: the net effect of these several enzyme interactings, can destroy the fibrous texture of plant cell wall, and even resolve into small-molecule substance, reduce and extract resistance to mass transfer, effectively make rutin molecule exposed outside plant tissue; Say according to convention, under the condition of enzymic hydrolysis under 40-60 DEG C of condition, rue enzyme in raw material can destroy the structure of rutin, and yield can be lower, but from experiment, the combination of these several enzymes, suppress on the contrary the hydrolysis of rue enzyme to rutin, found unexpectedly, added this prozyme, suppressed the hydrolysis of rue enzyme to rutin, this is that we are quite unexpected.Remove merely in the test of combination enzyme, have the rutin of 30-50% to be broken off, and after having added combination enzyme, be almost broken off without any rutin.
In one embodiment of the invention, the method for described extraction rutin, is characterized in that, described A step Extraction of rutin liquid is by using the first alcohol solution that the enzymolysis filter residue that contains rutin is extracted and obtained.
In one embodiment of the invention, the method for described extraction rutin, is characterized in that: described the first alcohol solution is the group that is selected from 1～20 fat of carbon atom alcohol composition.
In one embodiment of the invention, the method for described extraction rutin, the alcohol of the first alcohol solution used is selected from methyl alcohol, ethanol, butanols, a kind of in amylalcohol or wherein two kinds, three kinds.Described determining alcohol is 20-90 volume %, comprising: 20-30 volume %, 30-40 volume %, 40-50 volume %, 50-60 volume %, 60-70 volume %, 70-80 volume %, 80-90 volume %; Also comprise: 25-35 volume %, 35-45 volume %, 45-55 volume %, 55-65 volume %, 65-75 volume %, 75-85 volume % simultaneously.In one embodiment of the present of invention, extracting the method for rutin, is to be 50-80 volume % by the first alcohol water concentration ethanol carries out; And at a preferred preferred version of the present invention be: the first alcohol water concentration used is 60-70% volume % ethanol.
In one embodiment of the invention, the group that in described the second alcohol solution, contained alcohol selects the fatty alcohol that freely contains 1～3 carbon atom to form, comprises methyl alcohol, ethanol, and the group of propyl alcohol, or one of them.In one embodiment of the invention, the method of described extraction rutin, the second alcohol solution determining alcohol of wash-out separating medium is 30 volume %～100 volume %, comprise: 30-40 volume %, 40-50 volume %, 50-60 volume %, 60-70 volume %, 70-80 volume %, 80-90 volume %, 90-100 volume %; Also comprise simultaneously, 35-45 volume %, 45-55 volume %, 55-65 volume %, 65-75 volume %, 75-85 volume %, 85-95 volume %, is preferably 50-80 volume %; In a more preferred scheme of the present invention, the determining alcohol of the second alcohol solution is 60-70 volume %; In another one preferred version of the present invention, the determining alcohol of the second alcohol solution is 70-80 volume %.
In the present invention, the separating medium of use is ion exchange resin, and absorption with macroporous adsorbent resin post carries out fractionation by adsorption, and carries out wash-out.Contriver finds, by making spent ion exchange resin or macroporous adsorbent resin, can reach extraordinary effect, can remove a large amount of chlorophyll, the impurity such as betula camphor and Quercetin simultaneously.To described Extraction of rutin liquid A, B step alcohol kind used and determining alcohol, can be identical, also can be different.
In one embodiment of the invention, use separating medium, its specific surface area 500m
2more than/g, aperture is more than 50 dusts.Extraordinary effect can be reached, a large amount of chlorophyll, the impurity such as betula camphor and Quercetin can be removed simultaneously.
In one embodiment of the invention, use separating medium, its specific surface area 500-1500m
2/ g, aperture is 50-300 dust.Extraordinary effect can be reached, a large amount of chlorophyll, the impurity such as betula camphor and Quercetin can be removed simultaneously.
In one embodiment of the invention, use separating medium, its specific surface area 500-1500m
2/ g, aperture is 50-150 dust.Extraordinary effect can be reached, a large amount of chlorophyll, the impurity such as betula camphor and Quercetin can be removed simultaneously.
In one embodiment of the invention, make spent ion exchange resin, its specific surface area 500m
2more than/g, aperture is more than 50 dusts.Extraordinary effect can be reached, a large amount of chlorophyll, the impurity such as betula camphor and Quercetin can be removed simultaneously.
In one embodiment of the invention, make spent ion exchange resin, its specific surface area 500-1500m
2/ g, aperture is 50-300 dust.Extraordinary effect can be reached, a large amount of chlorophyll, the impurity such as betula camphor and Quercetin can be removed simultaneously.
In one embodiment of the invention, make spent ion exchange resin, its specific surface area 500-1500m
2/ g, aperture is 50-150 dust.Extraordinary effect can be reached, a large amount of chlorophyll, the impurity such as betula camphor and Quercetin can be removed simultaneously.
In one embodiment of the invention, using anionite-exchange resin is D301R, can reach extraordinary effect, can remove a large amount of chlorophyll, the impurity such as betula camphor and Quercetin simultaneously.
In one embodiment of the invention, use macroporous adsorbent resin, its specific surface area 500m
2more than/g, aperture is more than 50 dusts.Extraordinary effect can be reached, a large amount of chlorophyll, the impurity such as betula camphor and Quercetin can be removed simultaneously.
In one embodiment of the invention, use macroporous adsorbent resin, its specific surface area 500-1500m
2/ g, aperture is 50-300 dust.Extraordinary effect can be reached, a large amount of chlorophyll can be removed, the impurity such as betula camphor.Can remove a large amount of chlorophyll, the impurity such as betula camphor and Quercetin simultaneously.
In one embodiment of the invention, use macroporous adsorbent resin, its specific surface area 500-1500m
2/ g, aperture is 50-150 dust.Extraordinary effect can be reached, a large amount of chlorophyll, the impurity such as betula camphor and Quercetin can be removed simultaneously.
In one embodiment of the invention, use nonpolar or low-pole macroporous adsorbent resin, its specific surface area 500m
2more than/g, aperture is more than 50 dusts.Extraordinary effect can be reached, a large amount of chlorophyll, the impurity such as betula camphor and Quercetin can be removed simultaneously.
In one embodiment of the invention, using macroporous adsorbent resin is nonpolar or low-pole, its specific surface area 500-1500m
2/ g, aperture is 50-300 dust.Extraordinary effect can be reached, a large amount of chlorophyll, the impurity such as betula camphor and Quercetin can be removed simultaneously.
In one embodiment of the invention, using macroporous adsorbent resin is nonpolar or low-pole, its specific surface area 500-1500m
2/ g, aperture is 50-150 dust.Extraordinary effect can be reached, a large amount of chlorophyll, the impurity such as betula camphor and Quercetin can be removed simultaneously.
In one embodiment of the invention, use nonpolar macroporous adsorption resin, its specific surface area 500-1500m
2/ g, aperture is 50-300 dust.Extraordinary effect can be reached, a large amount of chlorophyll, the impurity such as betula camphor and Quercetin can be removed simultaneously.
In one embodiment of the invention, use low-pole macroporous adsorbent resin, its specific surface area 500m
2more than/g, aperture is more than 50 dusts.Extraordinary effect can be reached, a large amount of chlorophyll, the impurity such as betula camphor and Quercetin can be removed simultaneously.
In one embodiment of the invention, use low-pole macroporous adsorbent resin, its specific surface area 500-1500m
2/ g, aperture is 50-150 dust.Extraordinary effect can be reached, a large amount of chlorophyll, the impurity such as betula camphor and Quercetin can be removed simultaneously.
In one embodiment of the invention, use intermediate-polarity macroporous adsorption resin, its specific surface area 500m
2more than/g, aperture is more than 50 dusts.Extraordinary effect can be reached, a large amount of chlorophyll, the impurity such as betula camphor and Quercetin can be removed simultaneously.
In one embodiment of the invention, use intermediate-polarity macroporous adsorption resin, its specific surface area 500-1500m
2/ g, aperture is 50-300 dust.Extraordinary effect can be reached, a large amount of chlorophyll, the impurity such as betula camphor and Quercetin can be removed simultaneously.
In one embodiment of the invention, use intermediate-polarity macroporous adsorption resin, its specific surface area 500-1500m
2/ g, aperture is 50-150 dust.Extraordinary effect can be reached, a large amount of chlorophyll, the impurity such as betula camphor and Quercetin can be removed simultaneously.
In the present invention, be by using 1-8BV column volume alcohol wash-out separating medium (comprising nonpolar or low-pole macroporous adsorbent resin and resin anion(R.A)), collect and merge stream part of containing rutin, obtain elutriant.In another embodiment of the present invention, use 2-4BV column volume alcohol wash-out separating medium, collect and merge stream part of containing rutin, obtain elutriant.In another embodiment of the present invention, use 2-3BV column volume alcohol wash-out separating medium, collect and merge stream part of containing rutin, obtain elutriant.The rutin rate of recovery is increased considerably.
In another embodiment of the present invention, obtain elutriant by concentrating and separating medium, reclaim alcohol, crystallization, filters, and obtains rutin crystallization, and the rate of recovery reaches more than 85%, and product content reaches more than 95%.
In a comparative example of the present invention, do not use prozyme and resin treatment step, rutin content only arrives 70% left and right, does not reach standard.
Technique scheme is that contriver gropes to sum up technical scheme out by long-term practice repeatedly, and raw materials used being easy to get, can solve the huge waste of acid-alkali treatment method to environment and resource.The present invention is a kind of high efficiency extraction isolation technique, highly effective from the plant material that contains rutin as separated rutin the sophora bud, the rate of recovery reaches 85%-95%, product content reaches more than 95%.
Solvent for use all can be recycled, and the plant material (as sophora bud slag) that contains rutin can be for organic composite fertilizer or feed, and whole industrial production is a green cleaning technology process of typical case.Life cycle of the product is short, and production cost is low, and production technique is nontoxic, safety, non-environmental-pollution.
The aspect that the present invention is additional and advantage in the following description part provide, and part will become obviously from the following description, or recognize by practice of the present invention.
Embodiment
To describe the specific embodiment of the present invention below in detail, this is only for explaining the present invention, and can not be interpreted as limitation of the present invention.
It should be noted that, the numerical range that used in the present invention has not only comprised all concrete numerical point in described scope, and having comprised the random subset in this numerical range, the fatty alcohol that contains 1～20 carbon atom that for example used in the present invention comprises the fatty alcohol that contains 1,2,3,4,5,6,7,8,9,10,11,12,13,14,15,16,17,18,19 or 20 carbon atom, the fatty alcohol that contains 1～3 carbon atom using in the present invention comprises and contains 1,2, the fatty alcohol of 3 carbon atoms, the concentration of the alcohol solution that used is in the present invention 30 volume %～100 volume %, comprise that concentration is 30 volume %, 40 volume %, 50 volume %, 60 volume %, 70 volume %, 80 volume %, 90 volume %, the alcohol solution of 100 volume %, but also be included in the random subset within the scope of 30 volume %～80 volume %, for example 30 volume %～80 volume %, 40 volume %～80 volume %, 50 volume %～60 volume %, 60 volume %～70 volume %, 70 volume %～80 volume %, and 65 volume %～80 volume %, 65 volume %～75 volume %, 75～85 volume %, 85～95 volume %, for example use 1-8BV (BV represents column volume, and separating medium is filled in the volume occupying in chromatography column) column volume alcohol wash-out separating medium, 1-8BV includes 1BV, 2BV, 3BV, 4BV, 5BV, 6BV, 7BV, any one of 8BV, the specific surface area 500-1500m of the separating medium that for example the present invention uses
2/ g, comprises specific surface area 500-550m
2/ g, 550-600m
2/ g, 600-650m
2/ g, 65-700m
2/ g,, 700-750m
2/ g, 750-800m
2/ g, 800-850m
2/ g, 850-900m
2/ g, 900-950m
2/ g, 950-1000m
2/ g,, 1000-1050m
2/ g, 1050-1100m
2/ g, 1100-1150m
2/ g, 1150-1200m
2/ g, 1200-1250m
2/ g, 1250-1300m
2/ g, 1300-1350m
2/ g, 1350-1400m
2/ g, 1400-1450m
2/ g, 1450-1500m
2/ g, also comprises 500-600m simultaneously
2/ g, 600-700m
2/ g, 700-800m
2/ g, 800-900m
2/ g, 900-1000m
2/ g, 1000-1100m
2/ g, 1100-1200m
2/ g, 1200-1300m
2/ g, 1300-1400m
2/ g, 1400-1500m
2/ g.The aperture 50-300 dust of the separating medium that for example the present invention uses, comprise 50-60 dust, 60-70 dust, 70-80 dust, 80-90 dust, 90-100 dust, 100-110 dust, 110-120 dust, 120-130 dust, 130-140 dust, 140-150 dust, 150-160 dust, 160-170 dust, 170-180 dust, 180-190 dust, 190-200 dust, 200-210 dust, 220-230 dust, 240-250 dust, 260-270 dust, 270-280 dust, 280-290 dust, 290-300 dust, also comprise 50-55 dust simultaneously, 55-60 dust, 60-65 dust, 65-70 dust, 70-75 dust, 75-80 dust, 80-85 dust, 85-90 dust, 90-95 dust, 95-100 dust, 105-110 dust, 110-115 dust, 115-120 dust, 120-125 dust, 125-130 dust, 130-135 dust, 135-140 dust, 140-145 dust, 145-150 dust, 185-195 dust, 265-275 dust, 285-295 dust etc., here just do not enumerate one by one.Separating medium used in the present invention, its specific surface area and aperture are the arbitrary combination from above-mentioned specific surface area and aperture random subset the inside.
In an embodiment of the invention, provide a kind of method of preparing high-purity rutoside, it comprises the following steps:
A. obtain Extraction of rutin liquid.
B. use separating medium to carry out fractionation by adsorption to described containing Extraction of rutin liquid, with the alcohol wash-out separating medium of 1-8 times of volume, collect and merge stream part of containing rutin, obtain elutriant.
C. concentrate eluant, filters, dry, obtains rutin sterling.
The Extraction of rutin liquid of mentioning in the present invention obtains in the following manner: will contain rutin raw material pulverizing, sieve, raw material powder adds distilled water, regulates pH to 4.0-6.0, add a certain amount of compound enzymic preparation, at 40-60 DEG C of enzymolysis 1-6 hour, filter, then filter residue is according to raw material: the weight/volume of alcohol=1:5～20, at a certain temperature, stir and extract, filter, obtain Extraction of rutin liquid.
In the present invention, described a kind of compound enzymic preparation, is characterized in that: the component that comprises following weight part:
Cellulase 1-5 part
Proteolytic enzyme 1-5 part
Amylase 1-5 part
Described proteolytic enzyme is selected at least one in papoid, Sumizyme MP, neutral protease.Described amylase is selected at least one in mesophilicα-diastase and beta-amylase.
In extraction rutin Flavonoids Method above-mentioned, described plant is pulverized at 40-100 order, and vegetable material is 1:8-30 with the mass ratio of the distilled water adding.The addition of enzyme is the 0.01-1% of plant material addition.
In the present invention, separating medium absorption can be placed in chromatography column to be carried out, and also can whip attachment carry out.After absorption, with this separating medium of alcohol wash-out with being equivalent to separating medium 1-8 times column volume, collect and merge stream part of containing rutin, obtaining elutriant.Wash-out object is the rate of recovery in order to increase rutin, makes rutin and impurity separately.
Traditional method, because the limitation of rutin solubleness, adopt alkali to put forward the sour heavy mode that to obtain, add a lot of picture boraxs, lime toward contact, hydrochloric acid etc. are unfavorable for the chemical reagent of environmental protection, often, after acid is heavy, through repeatedly refining recrystallize, could meet the requirement of rutin content, cause the huge pollution of environment simultaneously, therefore in application, be restricted.And in the present invention, utilize the method for enzyme process and resin-phase combination, can reach the effect of purifying and raising rutin content simultaneously, can exempt applied chemistry reagent on the one hand, on the other hand, in conjunction with complex enzyme hydrolysis, decon, ethanol-extracted, resin is removed impurity, concentrated, the means of recovery alcohol, obtain high-content rutin finished product.In addition, the material price that the method is used is cheap, and separating medium also can repeat regeneration and use, and greatly reduces production cost, is applicable to large-scale industrial production.
Can take in the present invention any known method to obtain Extraction of rutin thing solution, for example, include but not limited to by using enzyme extraction, the first alcohol solution extracts acquisition to the filter residue of enzyme extraction.Can adopt in the present invention any material that contains rutin as the raw material that extracts rutin.Adopt in one embodiment of the invention the sophora bud as raw material.In another embodiment of the present invention, the raw material adopting is bitter buckwheat.It will be understood by those skilled in the art that and can adopt a kind of plant origin as raw material, also can adopt the combination in various plants source to be used as raw material.In one embodiment of the invention, before extracting, be powder by raw material pulverizing, can improve like this extraction efficiency.
For the selection of alcohol in the first alcohol solution, be not subject to any restriction, as long as can extract rutin from raw material.In one embodiment of the invention, alcohol is the fatty alcohol that contains 1～20 carbon atom.Like this, can make the residual little of alcohol in product, toxicological harmless effect.In another embodiment of the present invention, due to the preferred self-contained methyl alcohol of described alcohol, the group of ethanol, propyl alcohol, Virahol, butanols, isopropylcarbinol, can make the residual little of alcohol in product like this, toxicological harmless effect, and the efficiency of extracting obtains greatly must improving.In one embodiment of the invention, the concentration of described the first alcohol solution is 50 volume %～80 volume %; In another preferred version of the present invention, the concentration of the first alcohol solution is 60 volume %～70 volume %, can further improve like this extraction efficiency, and extraction time shortens.It will be understood by those skilled in the art that in alcohol solution and both can select independent a kind of alcohol, also can select the combination of two kinds or more kinds of alcohol.
At use separating medium, described Extraction of rutin liquid is carried out in the step of fractionation by adsorption and wash-out, the eluent adopting is not restricted.In one embodiment of the invention, wash-out uses the second alcohol solution to carry out.For the selection of alcohol in the second alcohol solution, be not subject to any restriction.The selection of the first alcohol solution and the second alcohol solution is independently, can use identical alcohol solution, also can use different alcohol solutions.In one embodiment of the invention, alcohol is the fatty alcohol that contains 1～3 carbon atom.Like this, can make the residual little of alcohol in product, toxicological harmless effect.In another embodiment of the present invention, due to the preferred self-contained methyl alcohol of described alcohol, the group of ethanol, propyl alcohol, can make the residual little of alcohol in product like this, toxicological harmless effect, and the efficiency of extracting obtains greatly must improving.In one embodiment of the invention, the concentration of described the second alcohol solution is 30 volume %～100 volume %, is preferably 50 volume %～80 volume %, further preferred volume 60%～70 volume %.Can further improve like this extraction efficiency, extraction time shortens.It will be understood by those skilled in the art that in the second alcohol solution and both can select independent a kind of alcohol, also can select the combination of two kinds or more kinds of alcohol.
Rutin, Quercetin, chlorophyll, when betula camphor etc. mix, general by the method for recrystallization, in mother liquor, contain a large amount of rutins, suitable low of the yield of rutin, general yield is 12-13%.When the present invention passes through to explore a series of separating medium, through a large amount of experiments, by attempting various specific surface areas, the macroporous adsorbent resin in various apertures, in vast as the open sea separating medium, find specific separating medium (as nonpolar or low-pole polymeric adsorbent or resin anion(R.A)), there is specific specific surface area (500-1500m
2/ g), specific resin aperture (50-300 dust), reaches and removes Quercetin simultaneously, chlorophyll, the object of these impurity of betula camphor.In comparative example 9,17, a large amount of impurity, not within this scope, is not removed in the resin specific surface area of using or aperture, finally causes rutin product purity not high.
The present invention also provides the rutin obtaining according to aforesaid method product, meets Chinese Pharmacopoeia standard, USP standard and European Pharmacopoeia standard.
It should be noted that, rutin raw material sources of the present invention can be from Remote Lemongrass Herb, buckwheat (comprising cauline leaf, flower), and Herba Hyperici, cursor hooks youngster rattan, Cortex malloti japonici leaf, Chinese ilex, the capsule of weeping forsythia, the sophora bud, outstanding graceful eucalyptus leaves, waits plant, but is not limited to these plants.The said content of the present invention utilizes determined by ultraviolet spectrophotometry, with reference to the National Standard Method of Determination of rutin.
It should be noted that, the macroporous resin of using in the embodiment of the present invention, or non-polar macroporous resin, or low-pole macroporous resin, or the source of resin anion(R.A) can be existing product on market, also can, according to the needs of research, carry out technology customization, obtain suitable specific surface area and aperture, obtain the desirable resin that we need.Therefore the resin of mentioning in embodiment can be the resin of name model, the resin that also can not named.Because resin model Dou Shi producer names voluntarily, need the resin of what type, resin producer can research and develop voluntarily.
The method of extraction purification high-purity rutoside of the present invention is described below by specific embodiment.Description is below only for the present invention is described, is not also not should be appreciated that and become limitation of the present invention.
Embodiment 1
A. take 10 kilograms of the sophora bud, be crushed to 60-100 order, add distilled water first to use 100 liters of stirrings; Get 50 grams of zymins (cellulase: proteolytic enzyme: amylase=1:1:1) and add in stirring liquid, regulate pH to 6.0, under 45 DEG C of conditions, enzymolysis 1 hour, centrifugal, or Plate Filtration.By filter residue, first with 50 DEG C of extraction 1h of 60% ethanol of 150 liters, suction filtration, again by 50 DEG C of points of second extraction of 60% ethanol of 150 liters, merges extracted twice liquid by filter residue, must be containing the extracting solution of rutin.
B. the above-mentioned extracting solution containing rutin is crossed to specific surface area 550-600m
2/ g, aperture is the nonpolar macroporous adsorption resin adsorption column (15 liters of resin volumes) of 100-110 dust, uses afterwards the 50% alcohol flushing post of 90 liters, concentrate eluant, filters, dry, obtain 2.12 kilograms of rutin fine work, content 99%, other indexs all meet pharmacopoeia of each country standard.
Embodiment 2
A. take 100 kilograms of the sophora bud, pulverize, 60-100 order, adds distilled water first to use 2000 liters of stirrings; Get 100 grams of zymins (cellulase: proteolytic enzyme: amylase=5:2:3) and add in stirring liquid, regulate pH to 4.9, under 40 DEG C of conditions, enzymolysis 3 hours, centrifugal, or Plate Filtration.By filter residue, first with 70 DEG C of extraction 1h of 70% ethanol of 1500 liters, suction filtration, again by 70 DEG C of points of second extraction of 70% ethanol of 1500 liters, merges extracted twice liquid by filter residue, must be containing the extracting solution of rutin.
B. the above-mentioned extracting solution containing rutin is crossed to HPD100A resin column, its specific surface area 550-600m
2/ g, aperture is 100-110 dust (130 liters of resin volume), uses afterwards the 70% alcohol flushing post of 1040 liters, concentrate eluant filters, dry, obtains 20.1 kilograms of rutin fine work, content 98.6%, other indexs all meet pharmacopoeia of each country standard.
Embodiment 3
A. take 500 kilograms of the sophora bud, pulverize, 80-100 order, adds distilled water first to use 4000 liters of stirrings; Get 4000 grams of zymins (cellulase: proteolytic enzyme: amylase=3:1:3) and add in stirring liquid, regulate pH to 6, under 50 DEG C of conditions, enzymolysis 3 hours, centrifugal, or Plate Filtration.By filter residue, first with 80 DEG C of extraction 1h of 60% ethanol of 4000 liters, suction filtration, again by 80 DEG C of points of second extraction of 60% ethanol of 4000 liters, merges extracted twice liquid by filter residue, must be containing the extracting solution of rutin.
B. the above-mentioned extracting solution containing rutin is crossed to non-polar resin post, its specific surface area 650-700m
2/ g, aperture is 110-120 dust (500 liters of resin volume), uses afterwards the 60% alcohol flushing post of 1000 liters, concentrate eluant filters, dry, obtains 102.5 kilograms of rutin fine work, content 98.5%, other indexs all meet pharmacopoeia of each country standard.
Embodiment 4
A. take 100 kilograms of bitter buckwheats, pulverize, 80-100 order, adds distilled water first to use 2000 liters of stirrings; Get 4000 grams of zymins (cellulase: proteolytic enzyme: amylase=3:1:3) and add in stirring liquid, regulate pH to 6, under 50 DEG C of conditions, enzymolysis 3 hours, centrifugal, or Plate Filtration.Filter residue, again by 80 DEG C of points of second extraction of 55% ethanol of 700 liters, is merged to extracted twice liquid, must be containing the extracting solution of rutin.
B. the above-mentioned extracting solution containing rutin is crossed to HPD-400 resin column, its specific surface area 500-550m
2/ g, aperture is 75-80 dust (200 liters of resin volume), uses afterwards the 55% alcohol flushing post of 600 liters, concentrate eluant filters, dry, obtains 19.9 kilograms of rutin fine work, content 98.4%, other indexs all meet pharmacopoeia of each country standard.
Embodiment 5
A. take 1000 kilograms of the sophora bud, pulverize, 80-100 order, adds distilled water first to use 20000 liters of stirrings; Get 500 grams of zymins (cellulase: proteolytic enzyme: amylase=3:1:3) and add in stirring liquid, regulate pH to 6, under 45 DEG C of conditions, enzymolysis 2 hours, centrifugal, or Plate Filtration.Filter residue, again by 65 DEG C of points of second extraction of 65% ethanol of 8000 liters, is merged to extracted twice liquid, must be containing the extracting solution of rutin.
B. the above-mentioned extracting solution containing rutin is crossed to nonpolar adsorption resin post, its specific surface area 700-800m
2/ g, aperture is 80-90 dust (1500 liters of resin volume), uses afterwards the 65% alcohol flushing post of 4500 liters, concentrate eluant filters, dry, obtains 209 kilograms of rutin fine work, content 99.5%, other indexs all meet pharmacopoeia of each country standard.
Embodiment 6 (comparative example)
A. take 100 kilograms of the sophora bud, pulverize, 80-100 order, adds distilled water first to use 500 liters of stirrings; Get 60 grams of zymins (cellulase: proteolytic enzyme: amylase=3:1:1) and add in stirring liquid, regulate pH to 6, under 45 DEG C of conditions, enzymolysis 3 hours, centrifugal, or Plate Filtration.Filter residue, again by 80 DEG C of points of second extraction of 75% ethanol of 2000 liters, is merged to extracted twice liquid, must be containing the extracting solution of rutin.
B. the above-mentioned extracting solution containing rutin is crossed to CD-3 adsorption resin column, its specific surface area 1600m
2/ g, aperture is 310 dusts (100 liters of resin volumes), uses afterwards the 75% alcohol flushing post of 200 liters, and concentrate eluant filters, dry, obtains 30.35 kilograms of rutin fine work, and content 68.5%, need to further refine, and just can reach standards of pharmacopoeia.
Embodiment 7
A. take 250 kilograms of the sophora bud, pulverize, 60-100 order, adds distilled water first to use 1500 liters of stirrings; Get 250 grams of zymins (cellulase: proteolytic enzyme: amylase=5:1:1) and add in stirring liquid, regulate pH to 6, under 40 DEG C of conditions, enzymolysis 3 hours, centrifugal, or Plate Filtration.Filter residue, again by 70 DEG C of points of second extraction of 70% ethanol of 3250 liters, is merged to extracted twice liquid, must be containing the extracting solution of rutin.
B. the above-mentioned extracting solution containing rutin is crossed to non-polar resin post, its specific surface area 800m
2/ g, aperture is 290-300 dust (500 liters of resin volume), uses afterwards the 60% alcohol flushing post of 1000 liters, concentrate eluant filters, dry, obtains 52.5 kilograms of rutin fine work, content 99.4%, other indexs all meet pharmacopoeia of each country standard.
Embodiment 8
A. take 200 kilograms of the sophora bud, pulverize, 80-100 order, adds distilled water first to use 1600 liters of stirrings; Get 200 grams of zymins (cellulase: proteolytic enzyme: amylase=5:1:1) and add in stirring liquid, regulate pH to 6, under 50 DEG C of conditions, enzymolysis 3 hours, centrifugal, or Plate Filtration.Filter residue, again by 75 DEG C of points of second extraction of % ethanol of 1000 liters, is merged to extracted twice liquid, must be containing the extracting solution of rutin.
B. the above-mentioned extracting solution containing rutin is crossed to non-polar resin post, its specific surface area 550-600m
2/ g, aperture is 150 dusts (200 liters of resin volumes), uses afterwards the 80% alcohol flushing post of 1200 liters, concentrate eluant filters, dry, obtains 42.4 kilograms of rutin fine work, content 98.6%, other indexs all meet pharmacopoeia of each country standard.
Embodiment 9 (comparative example)
A. take 100 kilograms of the sophora bud, pulverize, 80-100 order, adds distilled water first to use 700 liters of stirrings; Get 50 grams of zymins (cellulase: proteolytic enzyme: amylase=3:1:3) and add in stirring liquid, regulate pH to 6, under 50 DEG C of conditions, enzymolysis 3 hours, centrifugal, or Plate Filtration.Filter residue, again by 80 DEG C of points of second extraction of 90% amylalcohol of 1800 liters, is merged to extracted twice liquid, must be containing the extracting solution of rutin.
B. the above-mentioned extracting solution containing rutin is crossed to XAD-7 adsorption resin column, its specific surface area 560-710m
2/ g, aperture is 450 dusts (150 liters of resin volumes), uses afterwards the 75% alcohol flushing post of 400 liters, and concentrate eluant filters, dry, obtains 28.87 kilograms of rutins, and content 72%, need to further refine, and just can reach standards of pharmacopoeia.
Embodiment 10
A. take 65 kilograms of the sophora bud, pulverize, 80-100 order, adds distilled water first to use 585 liters of stirrings; Get 65 grams of zymins (cellulase: proteolytic enzyme: amylase=3:1:3) and add in stirring liquid, regulate pH to 6, under 45 DEG C of conditions, enzymolysis 2 hours, centrifugal, or Plate Filtration.Filter residue, again by 80 DEG C of points of second extraction of 75% ethanol of 585 liters, is merged to extracted twice liquid, must be containing the extracting solution of rutin.
B. the above-mentioned extracting solution containing rutin is crossed to nonpolar adsorption resin post, its specific surface area 800-900m
2/ g, aperture is 120-130 dust (250 liters of resin volume), uses afterwards the 60% alcohol flushing post of 2000 liters, concentrate eluant filters, dry, obtains 13.52 kilograms of rutin fine work, content 98.5%, other indexs all meet pharmacopoeia of each country standard.
Embodiment 11
A. take 85 kilograms of the sophora bud, pulverize, 80-100 order, adds distilled water first to use 935 liters of stirrings; Get 42.5 grams of zymins (cellulase: proteolytic enzyme: amylase=3:1:3) and add in stirring liquid, regulate pH to 6, under 50 DEG C of conditions, enzymolysis 3 hours, centrifugal, or Plate Filtration.Filter residue, again by 80 DEG C of points of second extraction of 75% ethanol of 935 liters, is merged to extracted twice liquid, must be containing the extracting solution of rutin.
B. the above-mentioned extracting solution containing rutin is crossed to nonpolar adsorption resin post, its specific surface area 900-1000m
2/ g, aperture is 130-140 dust (85 liters of resin volume), uses afterwards the 75% alcohol flushing post of 595 liters, concentrate eluant filters, dry, obtains 18.15 kilograms of rutin fine work, content 99.5%, other indexs all meet pharmacopoeia of each country standard.
Embodiment 12
A. take 90 kilograms of the sophora bud, pulverize, 80-100 order, adds distilled water first to use 900 liters of stirrings; Get 90 grams of zymins (cellulase: proteolytic enzyme: amylase=1:1:1.5) and add in stirring liquid, regulate pH to 6, under 50 DEG C of conditions, enzymolysis 3 hours, centrifugal, or Plate Filtration.Filter residue, again by 80 DEG C of points of second extraction of 60% ethanol of 1080 liters, is merged to extracted twice liquid, must be containing the extracting solution of rutin.
B. the above-mentioned extracting solution containing rutin is crossed to D101 adsorption resin column, its specific surface area 550-600m
2/ g, aperture is 90-100 dust (150 liters of resin volume), uses afterwards the 60% alcohol flushing post of 450 liters, concentrate eluant filters, dry, obtains 19.08 kilograms of rutin fine work, content 99.6%, other indexs all meet pharmacopoeia of each country standard.
Embodiment 13
A. take 152 kilograms of the sophora bud, pulverize, 80-100 order, adds distilled water first to use 1216 liters of stirrings; Get 76 grams of zymins (cellulase: proteolytic enzyme: amylase=4.5:1.1:3.1) and add in stirring liquid, regulate pH to 6, under 45 DEG C of conditions, enzymolysis 3 hours, centrifugal, or Plate Filtration.Filter residue, again by 80 DEG C of points of second extraction of 70% ethanol of 1976 liters, is merged to extracted twice liquid, must be containing the extracting solution of rutin.
B. the above-mentioned extracting solution containing rutin is crossed to HPD-300 adsorption resin column, its specific surface area 800-870m
2/ g, aperture is 50-55 dust (230 liters of resin volume), uses afterwards the 70% alcohol flushing post of 460 liters, concentrate eluant filters, dry, obtains 31.92 kilograms of rutin fine work, content 98.6%, other indexs all meet pharmacopoeia of each country standard.
Embodiment 14
A. take 180 kilograms of the sophora bud, pulverize, 80-100 order, adds distilled water first to use 1620 liters of stirrings; Get 18 grams of zymins (cellulase: proteolytic enzyme: amylase=5:1:1) and add in stirring liquid, regulate pH to 6, under 45 DEG C of conditions, enzymolysis 2 hours, centrifugal, or Plate Filtration.Filter residue, again by 80 DEG C of points of second extraction of 80% ethanol of 1976 liters, is merged to extracted twice liquid, must be containing the extracting solution of rutin.
B. the above-mentioned extracting solution containing rutin is crossed to low-pole macroporous resin adsorption post as D101C, its specific surface area 600m
2/ g, aperture is 300 dusts (260 liters of resin volumes), uses afterwards the 85% alcohol flushing post of 460 liters, concentrate eluant filters, dry, obtains 31.92 kilograms of rutin fine work, content 98.5%, other indexs all meet pharmacopoeia of each country standard.
Embodiment 15
A. take 100 kilograms of the sophora bud, pulverize, 80-100 order, adds distilled water first to use 1000 liters of stirrings; Get 400 grams of zymins (cellulase: proteolytic enzyme: amylase=5:1:1) and add in stirring liquid, regulate pH to 6, under 40 DEG C of conditions, enzymolysis 2 hours, centrifugal, or Plate Filtration.Filter residue, again by 80 DEG C of points of second extraction of 75% ethanol of 1700 liters, is merged to extracted twice liquid, must be containing the extracting solution of rutin.
B. the above-mentioned extracting solution containing rutin is crossed to LX-60 adsorption resin column, its specific surface area 600m
2/ g, aperture is 310 dusts (180 liters of resin volumes), uses afterwards the 75% alcohol flushing post of 500 liters, concentrate eluant filters, dry, obtains 21.9 kilograms of rutin fine work, content 99%, other indexs all meet pharmacopoeia of each country standard.
Embodiment 16
A. take sophora bud 120 kg, pulverize, 80-100 order, adds distilled water first to use 1000 liters of stirrings; Get 576 grams of zymins (cellulase: proteolytic enzyme: amylase=4:2:1) and add in stirring liquid, regulate pH to 6, under 40 DEG C of conditions, enzymolysis 2 hours, centrifugal, or Plate Filtration.Filter residue, again by 80 DEG C of points of second extraction of 75% ethanol of 2040 liters, is merged to extracted twice liquid, must be containing the extracting solution of rutin.
B. the above-mentioned extracting solution containing rutin is crossed to DA101 adsorption resin column, its specific surface area 650m
2/ g, aperture is 80-90 dust (150 liters of resin volume), uses afterwards the 65% alcohol flushing post of 450 liters, concentrate eluant filters, dry, obtains 24.96 kilograms of rutin fine work, content 99.5%, other indexs all meet pharmacopoeia of each country standard.
Embodiment 17 (comparative example)
A. take 100 kilograms of the sophora bud, pulverize, 80-100 order, adds distilled water first to use 1200 liters of stirrings; Get 1000 grams of zymins (cellulase: proteolytic enzyme: amylase=3:1:3) and add in stirring liquid, regulate pH to 6, under 50 DEG C of conditions, enzymolysis 3 hours, centrifugal, or Plate Filtration.Filter residue, again by 80 DEG C of points of second extraction of 65% ethanol of 2500 liters, is merged to extracted twice liquid, must be containing the extracting solution of rutin.
B. the above-mentioned extracting solution containing rutin is crossed to XAD-5 adsorption resin column, its specific surface area 415m
2/ g, aperture is 68 dusts (150 liters of resin volumes), uses afterwards the 65% alcohol flushing post of 450 liters, and concentrate eluant filters, dry, obtains 28 kilograms of rutins, and content 68.5%, need to further refine, and just can reach standards of pharmacopoeia.
Embodiment 18
A. take sophora bud 120 kg, pulverize, 80-100 order, adds distilled water first to use 1200 liters of stirrings; Get 288 grams of zymins (cellulase: proteolytic enzyme: amylase=3.5:1.5:1.2) and add in stirring liquid, regulate pH to 5.5, under 60 DEG C of conditions, enzymolysis 2 hours, centrifugal, or Plate Filtration.Filter residue, again by 80 DEG C of points of second extraction of 60% ethanol of 1440 liters, is merged to extracted twice liquid, must be containing the extracting solution of rutin.
B. the above-mentioned extracting solution containing rutin is crossed to ADS-4 adsorption resin column, its specific surface area 1200m
2/ g, aperture is 90 dusts (180 liters of resin volumes), uses afterwards the 60% alcohol flushing post of 360 liters, concentrate eluant filters, dry, obtains 24.2 kilograms of rutin fine work, content 98.5%, other indexs all meet pharmacopoeia of each country standard.
Embodiment 19
A. take sophora bud 120 kg, pulverize, 60-100 order, adds distilled water first to use 1440 liters of stirrings; Get 120 grams of zymins (cellulase: proteolytic enzyme: amylase=5:1:1) and add in stirring liquid, regulate pH to 6, under 45 DEG C of conditions, enzymolysis 6 hours, centrifugal, or Plate Filtration.Filter residue, again by 80 DEG C of points of second extraction of 60% ethanol of 1440 liters, is merged to extracted twice liquid, must be containing the extracting solution of rutin.
B. the above-mentioned extracting solution containing rutin is crossed to SIP-1200 macroporous resin adsorption post, its specific surface area 500-600m
2/ g, aperture is 120 dusts (180 liters of resin volumes), uses afterwards the 60% alcohol flushing post of 360 liters, concentrate eluant filters, dry, obtains 25 kilograms of rutin fine work, content 98.5%, other indexs all meet pharmacopoeia of each country standard.
Embodiment 20 (comparative example)
(1) do not add the experiment of combining enzyme
A. take sophora bud 120 kg, pulverize, 80-100 order, adds distilled water first to use 1200 liters of stirrings; Centrifugal, or Plate Filtration.Filter residue, again by 80 DEG C of points of second extraction of 70% ethanol of 1440 liters, is merged to extracted twice liquid, must be containing the extracting solution of rutin.
B. the above-mentioned extracting solution containing rutin is crossed to ADS-4 adsorption resin column, its specific surface area 1200m
2/ g, aperture is 90 dusts (180 liters of resin volumes), uses afterwards the 60% alcohol flushing post of 360 liters, concentrate eluant filters, dry, obtains 14.92 kilograms of rutin fine work, content 98.5%, other indexs all meet pharmacopoeia of each country standard.
(2) directly extract experiment
A. take sophora bud 120 kg, pulverize, 60-100 order, by 80 DEG C of points of second extraction of 60% ethanol of 1440 liters, merges extracted twice liquid, must be containing the extracting solution of rutin.
B. concentrate eluant, filters, dry, obtains 30 kilograms of rutins, and content 67%, need to further refine, and just can reach standards of pharmacopoeia.
Embodiment 21
A. take sophora bud 120 kg, pulverize, 80-100 order, adds distilled water first to use 1200 liters of stirrings; Get 120 grams of zymins (cellulase: proteolytic enzyme: amylase=5:1:1) and add in stirring liquid, regulate pH to 5.6, under 40 DEG C of conditions, enzymolysis 5 hours, centrifugal, or Plate Filtration.Filter residue, again by 80 DEG C of points of second extraction of 60% ethanol of 1440 liters, is merged to extracted twice liquid, must be containing the extracting solution of rutin.
B. the above-mentioned extracting solution containing rutin is crossed to D301R resin anion(R.A) post, its specific surface area 1000m
2/ g, aperture is 100 dusts (120 liters of resin volumes), uses afterwards the 60% alcohol flushing post of 360 liters, concentrate eluant filters, dry, obtains 20 kilograms of rutin fine work, content 95.6%, other indexs all meet pharmacopoeia of each country standard.
Although illustrated and described embodiments of the invention, for the ordinary skill in the art, be appreciated that without departing from the principles and spirit of the present invention and can carry out multiple variation, amendment, replacement and modification to these embodiment, scope of the present invention is limited by claims and equivalent thereof.
Claims (18)
1. extract a processing method for rutin, it is characterized in that processing step is:
A. obtain Extraction of rutin liquid.
B. use separating medium to carry out fractionation by adsorption to described containing Extraction of rutin liquid, with the alcohol wash-out separating medium of 1-8 times of volume, collect and merge stream part of containing rutin, obtain elutriant.
C. concentrate eluant, filters, dry, obtains rutin sterling.
2. the processing method of extraction rutin according to claim 1, is characterized in that: described Extraction of rutin liquid obtains in the following manner: by containing the raw material pulverizing of rutin, sieve, raw material powder adds distilled water, regulate pH to 4.0-6.0, add a certain amount of compound enzymic preparation, at 40-60 DEG C of enzymolysis 1-6 hour, filter, then filter residue is according to raw material: the weight/volume of alcohol=1:5～20, at a certain temperature, stirs and extracts, filter, obtain Extraction of rutin liquid.
3. the processing method of extraction rutin according to claim 2, is characterized in that: described compound enzymic preparation comprises the component of following weight part: 1-5 part cellulase, 1-5 part proteolytic enzyme and the diastatic mixture of 1-5 part.
4. the processing method of extraction rutin according to claim 3, is characterized in that: described compound enzymic preparation addition is the 0.01-1% of rutin raw material powder addition.
5. the method for extraction rutin according to claim 2, is characterized in that, described Extraction of rutin liquid is by using the first alcohol solution that the filter residue of enzyme extraction is extracted and obtained.
6. the processing method of extraction rutin according to claim 5, is characterized in that: described the first alcohol solution is the group that is selected from 1～20 fat of carbon atom alcohol composition.
7. the processing method of extraction according to claim 6 rutin, is characterized in that: described alcohol is selected from methyl alcohol, ethanol, butanols, a kind of in amylalcohol or wherein two kinds, three kinds.
8. according to claim 6, the processing method of the extraction rutin described in 7, is characterized in that: described determining alcohol is 20-90 volume %.
9. the processing method of extraction rutin according to claim 8, is characterized in that: described determining alcohol is 50-80 volume %.
10. the method for extraction rutin according to claim 1, is characterized in that, the alcohol of described wash-out separating medium is the second alcohol solution.
The method of 11. extraction rutins according to claim 10, it is characterized in that, described the second alcohol solution concentration is 30 volume %～100 volume %, wherein, and the group that in described the second alcohol solution, contained alcohol selects the fatty alcohol that freely contains 1～3 carbon atom to form.
The processing method of 12. extraction rutins according to claim 1, is characterized in that: described separating medium is ion exchange resin or macroporous adsorbent resin; A, B step alcohol kind used and determining alcohol, can be identical, also can be different.
The processing method of 13. extraction rutins according to claim 12, is characterized in that: described separating medium is specific surface area 500m
2more than/g, aperture is more than 50 dusts.
The processing method of 14. extraction rutins according to claim 13, is characterized in that: described separating medium specific surface area 500-1500m
2/ g, aperture is 50-300 dust.
The processing method of 15. extraction rutins according to claim 14, is characterized in that: described separating medium specific surface area 500-1500m
2/ g, aperture is 50-150 dust.
16. according to claim 1, and 12,13, the separating medium described in 14,15 is macroporous adsorbent resin.
17. according to claim 1, and 12,13,14,15, the separating medium described in 16 is macroporous adsorbent resin, described macroporous adsorbent resin is nonpolar or low-pole or Semi-polarity.
18. according to claim 1, and 12,13, the separating medium described in 14,15 is ion exchange resin, described ion exchange resin is anionite-exchange resin.
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