CN1329103A - Method for extracting protein, short peptide, nucleic acid, isoflavone, saponin and oligosaccharide by using high and low temperature soybean cake - Google Patents
Method for extracting protein, short peptide, nucleic acid, isoflavone, saponin and oligosaccharide by using high and low temperature soybean cake Download PDFInfo
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Abstract
The present invention relates to a method for continuously-extracting protein, short peptide, nucleic acid, isoflavone, saponin and oligosaccharide from high-temp. and low-temp. soybean cake, and the said method includes the following steps: placting the high-temp. or low-temp. defatted soybean cake into an ultrasonic wall-breaking leaching tank, ultrasonic wall-breaking, dissolving, stirring, filtering, screening, separating, concentrating, hydrolyzing, electrodialyzing, desalting, sterilizing and spray-drying so as to obtain the invented various products. It not only raises the utilization rate of soybean resource, and can reduce environment-protecting cost.
Description
Technical field: the invention belongs to soybean deep processing field.
Background technology: modern science is discovered, materials such as small peptide that the soybean protein molecular degradation forms and the soybean isoflavones in the soybean, Soyasaponin, soybean oligosaccharide, soybean nucleic acid, have remarkable medical treatment and nourishing function for the mankind, so these materials are otherwise known as " soybean function material ", contain " nutritive substances " such as albumen, fat in the soybean to be different from.But because the complex manufacturing of soybean function material, the technical difficulty height, some manufacturing enterprises generally all adopt one, the simple production technology of two kinds, No. 01113946.3, Chinese patent application is " a kind of with soybean meal, maize is a method of extracting nucleic acid in the raw material production separating protein process ", 00107606.X number " extract soybean protein isolate continuously, isoflavones, saponin, the technology of oligose ", number 97105221.2 " a kind of production method of plant separation protein ", also only produce the kind below four, after aforesaid method all causes the major product functional mass to extract, at waste residue, still retain in the waste water different types of other functional mass is arranged, these functional mass are not as effectively extracting, can increase waste residue on the contrary, the content of the organic pollutant in the waste water, not only cause the wasting of resources, and causing the environmental protection cost to improve, the market competitiveness is not strong.
Summary of the invention: the present invention is not the simple combination of foregoing invention, but to remedy the deficiency that prior art can only be extracted a small amount of kind, waste resource and contaminate environment in the dregs of beans, adopted a kind of production method that can extract albumen, small peptide, nucleic acid, isoflavones, saponin, the multiple composition of oligose continuously.Its concrete production method is as follows:
1, extracts soybean protein concentrate
(a) high temperature or defatted soybean meal are thrown in the ultrasonic broken wall lixiviate jar;
(b) adopt high-power ultrasound generator that soya cells wall and nuclear membrane in the mixing dregs of beans solvent are by a certain percentage broken up, cell walls and nuclear membrane percentage of damage improve cell and endonuclear nutritive substance and functional mass solubility rate greater than 95%.
(c) according to the soybean protein stripping with etc. electric precipitating rule, the selection protein solubility is minimum, its concentration of mixed solvent of nucleic acid, isoflavones, saponin, oligose solubleness maximum is first, the ethanol of 55-80%, feed liquid proportioning in the lixiviate jar is become 1: 7-10, pH value is 7, fully stirs more than 6 hours under temperature 30-50 ℃ condition;
(d) feed liquid in the lixiviate jar is filtered by filter, obtain the bean dregs and the transparent supernatant liquor that contains nucleic acid, isoflavones, saponin, oligose composition of solid-state protein composition;
(e) contain the bean dregs of albumen composition,, keep moisture content below 7% through desolventizing machine precipitation (solvent recuperation), oven dry (temperature is controlled at 100 to 130 ℃);
(f) Hong Gan bean dregs are pulverized through pulverizer, and granularity requires the 100-120 order;
(g) remove skin of beancurd (fiber composition) through screening, sterilization can obtain the soybean protein concentrate of protein content more than 70%.
2, extract the soybean small peptide
(a) the soybean protein concentrate solid substance that extracts being added water, to become pH value 7.4-8.0 ratio of water to material be 10-15: 1, stirred at normal temperatures 15-30 minute;
(b) separate with the disk centrifuge more than 7500 rev/mins, obtain containing proteic slurries and fine-fibered;
(c) slurries are pumped into hydrolysis in intermittence that immobilized enzyme is housed or the continuous manipulation reactor, soybean protein hydrolysis liquid;
(d) hydrolyzed solution is passed through ultrafiltration membrance filter, obtain ultrafiltrated and soybean protein and soybean peptides (long-chain) mixture;
(e) with continuing hydrolysis in the mixture solid substance Returning reactor, obtain ultrafiltrated by ultra-filtration membrane once more;
(f) ultrafiltrated is passed through the ion exchange resin column desalination, through activated carbon decolorizing, deodorization;
(g) purified soybean small peptide is concentrated, sterilization, spraying drying, soybean small peptide product.
3, extract soybean nucleic acid
(a) will extract obtain in the soybean protein concentrate technology contain nucleic acid, isoflavones, saponin, the transparent supernatant liquor of oligose, regain solvent through distilling to concentrate;
(b) concentrate feed liquid and adjust solid substance 1-2%, transfer pH value 2-3.5 with HCI with deionized water;
(c) flocculating aids that adds suitable proportion filters, the transparent supernatant liquor that obtains containing the flocculating aids precipitating curdled milk of nucleic acid and contain isoflavones, saponin, oligose composition;
(d) the flocculating aids precipitating curdled milk that will contain nucleic acid precipitates flocculating aids with first, the dissolve with ethanol nucleic acid of high purity more than 95%;
(e) filtration obtains transparent liquid through filter, and vacuum concentration is regained solvent and also is concentrated into solid content 7%-9%, through sterilization, drying, gets the soybean nucleic acid of content more than 60%.
4, extract soybean isoflavones
(a) will extract obtain in the soybean nucleic acid technology contain isoflavones, saponin, the transparent liquid of oligose, by electrodialysis desalination, the feed liquid specific conductivity behind the desalination must not surpass 50us/cm
2
(b) feed liquid behind the desalination is contained soybean isoflavones, Soyasaponin by macroporous adsorbent resin in the material of resin absorption, and effusive feed liquid promptly is a soybean oligosaccharide;
(c) absorption with macroporous adsorbent resin is full close after, molten with 60-95% first, ethanol from wash-out;
(d) elutriant is regained solvent through concentrating;
(e) selection can separate dissolution with solvents, the stirring concentrated solution of isoflavones, saponin;
(f) separate through 10000 rev/mins high speed separator and draw the supernatant liquor that contains solid-state isoflavones and contain saponin;
(g) solid-state isoflavones is adjusted solid substance with deionized water, is concentrated into solid substance about 10%, can get the soybean isoflavones of content more than 80% through sterilization, spraying drying, and wherein Genistin (lignin) content is up to more than 80%.
5, extract Soyasaponin
(a) extract the isolating supernatant liquor vacuum concentration of isoflavones technology high speed separating machine;
(b) selection can be separated out the solvent of saponin, as: acetone, ether (purity is more than 95%) fully stir with 1: 5 above ratio, separate through high speed separator, get the saponin solid matter;
(c) solid matter adds a certain amount of deionized water and concentrates, and regains solvent, and solid content 9%-11% through sterilization, spraying drying, can get the Soyasaponin of content more than 60%.
6, extract soybean oligosaccharide
(a) through the effusive feed liquid that contains oligose of macroporous adsorbent resin, through reverse osmosis concentration to solid content 9%-11%;
(b) this feed liquid is further decoloured with gac, carclazyte;
(c) feed liquid after the decolouring is concentrated into solid content more than 40% through ultra-filtration membrane, through the liquid soybean oligosaccharide of direct canned one-tenth of sterilizing;
(d) Tuo Se feed liquid and dextrin are with after 1: 3 mixed, and solid substance is adjusted to the spraying drying standard, can get the soybean oligosaccharide of content 20-60% through sterilising spray.
The present invention has following characteristics: 1, the present invention is not the simple combination of prior art, but the innovation that oil prodution industry develops to high technology content and high added value direction.Past, the high temperature dregs of beans can only be used as feed, only 2000 yuan of prices per ton, and the present invention is a raw material with the high temperature dregs of beans, adopt this technology can obtain the effect same, can extract protein concentrate, small peptide, nucleic acid, isoflavones, saponin, oligose, remarkable in economical benefits continuously with low temperature soy meal, 60,000 yuan of processed outputs per ton after the processing, 3.5 ten thousand yuan of profits taxes.2, high temperature dregs of beans or low temperature soy meal mixed liquor, adopt high strength, high-power ultrasound generator, make soya cells wall and nuclear membrane percentage of damage greater than 95%, because nucleic acid, isoflavones, saponin, oligose are present in the soya cells invariably, so ultrasonic broken wall and rupture of membranes are for the stripping of nucleic acid, isoflavones, saponin, oligose, the rate that draws that improves the above-mentioned functions material has vital role.3, can only extract soybean function material below four kinds according to existing new patent searching, all the other functional mass still remain in the degree slag, waste water of processing.The present invention extracts protein concentrate, small peptide, nucleic acid, isoflavones, saponin, six kinds of products of oligose continuously on a production line; make the basic defecation of having found at present of soybean function material; production cost significantly reduces, and waste obtains comprehensive utilization, helps environment protection.4, waste each other between the product produced of prior art.For example: the production protein concentrate is a major product, and nucleic acid, isoflavones, saponin, oligose are that waste discharges; When production isoflavones, saponin, oligose, nucleic acid is as waste discharge; When producing nucleic acid, isoflavones, saponin, oligose are again as waste discharge.Such mode of production all causes the wasting of resources, and its cost height has seriously polluted environment.5, the present invention is the extraction process step that biological nature, physicochemical property, molecular weight size according to difference in functionality material in the soybean are determined, each processing sequence can not arbitrarily be changed, this method is not the simple combination of single product extractive technique, but after the extraction of difference in functionality material, help the raising of single variety functional mass purity.Give up any one process procedure or change processing sequence of the present invention, all can't on a production line, obtain above-mentioned six kinds of products.This production method has promptly solved the soybean function material of having found at present and has extracted continuously on a production line and produce, changed people again and thought that always the high temperature dregs of rice can only make the traditional concept of feed, finally raw soybeans is accomplished that " drain and eat up " basic no waste generates, reduced the content of organic pollutant, except that the utilization ratio that improves resource, also reduced the environmental protection cost.The present invention compares with the processing mode of the few kind of existing soybean function material, and its economic benefit increases substantially.
Description of drawings: Fig. 1 is a process flow sheet of the present invention.
The specific embodiment:
1, extracts FSPC
(a) high temperature or low temperature soy meal are entered in the ultrasonic broken wall pot for solvent extraction first, alcohol solvent with the conveyer elm Concentration is 55%-80%, and the feed liquid proportioning becomes 1: 7, and pH value is neutral, at temperature 30-5 Fully stir more than 6 hours under 0 ℃ of condition;
(b) adopt high-power ultrasound generator, its power 15-30KW, frequency 20-2 5KHZ, sound intensity 2-5W/cm2, act on mixed liquor, soya cells wall and nuclear membrane are hit Broken, percentage of damage is greater than 95%;
(c) well-beaten mixed liquor is filtered material conveying by 100-200 order filter The power of the pump of liquid is 10KW, and operating pressure is 0.4-0.6MPA;
(d) filter the automatic friction of the bean dregs warp desolventizing machine exsolution drying that contains Proteins that obtains, bean dregs In the solvent noresidue, moisture content is below 7%, precipitation power 100KW, 1450 rev/mins of rotating speeds;
(e) bean dregs of oven dry are pulverized through grinding roller formula pulverizer, and granularity must not be lower than 100-120 Order;
(f) remove the skin of beancurd fiber through screening machine, it is dense that sterilization can obtain the soybean of protein content more than 70% Pix protein, skin of beancurd fiber are delivered to expanded workshop and are processed into dilated food.
2, extract the soybean small peptide
(a) the soybean concentrated product is put in the pot for solvent extraction, at pH value 7.4-8.0, solid-liquid ratio is 1 10-15 fully stirred 30 minutes in 30 ℃ of situations of temperature;
The slurries that (b) will fully stir separate with 7500 rev/mins disk centrifuge, are contained Slurries and fine fibre that albumen is arranged, fine fibre are delivered to expanded workshop and are processed into dilated food, the control of seperator flow Built in 3-5 ton per hour;
The slurries that (c) will contain albumen in reactor with the soybean separation protein of powdery content more than 90% Transfer in vain concentration and be 8% protein slurry;
(d) adopt look to bury method and cross-linking method is fixed protease I, II, make diameter 1-5mm's Particle becomes immobilised enzymes, and in its pack into intermittence or continuous manipulation reactor, soy protein slurry is with 1-5 times of bed volumes/hour flow to reactor, reaction temperature 50-60 ℃, pH value is controlled at 7. 5-10.0 efflux is the hydrolyzate of soybean protein;
(e) hydrolyzate of soybean protein is filtered film by milipore filter (holding back more than the MW2000) Lower thing is MW less than 2000 soybean small peptide ultrafiltrate, and thing is soybean protein, Soybean Peptide (M on the film W is greater than 2000 mixing solid content.
(f) will mix solid content and return in the soy protein slurry and again size mixing, continue hydrolysis;
(g) soybean small peptide ultrafiltrate is passed through the desalination of macropore strong acid cation post, the feed liquid electrolyzing rate must not be greater than 20us/cm after the desalination2。
(h) feed liquid after the desalination is concentrated into solid content 9-11%, and through activated carbon decolorizing, the charcoal liquor ratio is 0. 5-1: 10, pH value 3.0-7.0, temperature 40-80 ℃;
(i) feed liquid after the decolouring draws essence through flash-sterilization (135 ℃ of 5S) spray-drying Soybean small peptide processed.
3, extract soybean nucleic acid
(a) will extract obtain in the FSPC technology contain nucleic acid, isoflavones, saponin, oligomeric The transparent supernatant of sugar, to solid content 20-40%, vapo(u)rizing temperature remains on 10 through distillation and concentration More than 0 ℃;
(b) concentrate feed liquid and adjust solid content 1-2% with deionized water, transfer pH value 2-with HCI 3.5 the mixer mixing time is 10-15 minute;
(c) the filter aid adding proportion be the 3-5% of feed liquid filter obtain contain isoflavones, saponin, The transparent liquid of compound sugar composition is delivered to desalination workshop section;
The filter aid precipitating curdled milk that (d) will contain nucleic acid uses first, the ethanol of high-purity more than 95% to dissolve Nucleic acid obtains transparent nucleic acid solution through filter, below the filter operating pressure 0.4MPA;
(e) nucleic acid solution Vacuum Concentration is regained solvent and also is concentrated into solid content 8%, through sterilization, Drying draws the soybean nucleic acid of content more than 60%, and thickening temperature is at 70-80 ℃;
4, extract isoflavones
(a) will extract obtain in the soybean nucleic acid technology contain isoflavones, saponin, the transparent liquid of compound sugar, pass through electrodialysis desalination, the electrodialysis operating pressure remains on 0.2-0.4MPA, flow-control was at 2. 5-3T/ hours, and the feed liquid electrical conductivity behind the desalination must not surpass 50us/cm2;
(b) (nonpolar macroporous adsorption resin is such as HP-by macroporous absorbent resin for the feed liquid behind the desalination 20, D330), contained isoflavones, soyasaponins, outflow in the material of resin adsorption Feed liquid namely is soyabean oligosaccharides, and the absorption flow velocity is 2.5-3T/ hour, and the resins exchange volume ratio is 5 0: 1;
(c) after macroporous absorbent resin absorption is full of, molten from wash-out with 60-95% first, ethanol gradient;
(d) eluent is regained solvent and is concentrated into solid content more than 20% through distillation and concentration, distillation Temperature is below 100 ℃, and operating pressure is at 0.1-0.4MPA;
(e) selecting can separating isoflavone, the solvent (water) of saponin fully dissolving stir ratio of water to material Be 10-50: 1;
(f) separate to draw through 10000 rev/mins high speed separator and contain solid-state isoflavones and contain The supernatant of saponin, same method separate three times repeatedly, and the supernatant of for the first time seperator withdrawal is delivered to and carried Get saponin workshop section;
(g) solid-state isoflavones is adjusted solid content with deionized water, is concentrated into solid content 10%, when concentrating Between remain on more than 1 hour, 100 ℃ of temperature are through sterilization, spray-drying can get content more than 80% Isoflavones, wherein Genistin (lignin) content is up to more than 80%.
5, extract soyasaponins
(a) extract the supernatant that isoflavones technology high speed seperator separates, Vacuum Concentration to solid content contains Amount is more than 20%;
(b) select to separate out the solvent of saponin, as: acetone, ether (purity is more than 95%) with Above ratio fully stirred in 1: 5, separated drawing saponin through high speed separator (10000 rev/mins) Solid matter, seperator charging flow velocity should be controlled at below 500kg/ hour;
(c) regain solid matter and add concentrated solvent, the concentration regained of a certain amount of deionized water (1: 5) Reach solid content 10%, through sterilization, spray-drying, can get the soyasaponins of content more than 60%.
6, extract soyabean oligosaccharides
(a) feed liquid that contains compound sugar that flows out by macroporous absorbent resin is through the reverse osmosis concentrated solid content that is reduced to Content 9%-11%, the reverse osmosis filter membrane aperture is 50nm, operating pressure be 1.5MPA with Lower;
(b) this feed liquid is decoloured with active carbon, carclazyte, and the active carbon addition is 1-2%, and carclazyte adds Amount is 1-1.5%;
(c) feed liquid and the dextrin after the decolouring puddled with 1: 3 ratio, filters, sterilizes, disputes through filter The mist drying can draw content 20-60% soyabean oligosaccharides.
Claims (1)
1, a kind of high and low temperature dregs of beans extracts the method for albumen, small peptide, nucleic acid, isoflavones, saponin, oligose, it is characterized in that: it can extract albumen, small peptide, nucleic acid, isoflavones, saponin, six kinds of compositions of oligose continuously, and its concrete production method is as described below:
(1) extracts soybean protein concentrate
(a) high temperature or defatted soybean meal are thrown in the ultrasonic broken wall lixiviate jar;
(b) adopt high-power ultrasound generator that soya cells wall and nuclear membrane in the mixing dregs of beans solvent are by a certain percentage broken up, cell walls and nuclear membrane percentage of damage improve cell and endonuclear nutritive substance and functional mass solubility rate greater than 95%.
(c) according to the soybean protein stripping with etc. electric precipitating rule, the selection protein solubility is minimum, its concentration of mixed solvent of nucleic acid, isoflavones, saponin, oligose solubleness maximum is first, the ethanol of 55-80%, feed liquid proportioning in the lixiviate jar is become 1: 7-10, pH value is 7, fully stirs more than 6 hours under temperature 30-50 ℃ condition;
(d) feed liquid in the lixiviate jar is filtered by filter, obtain the bean dregs and the transparent supernatant liquor that contains nucleic acid, isoflavones, saponin, oligose composition of solid-state protein composition;
(e) contain the bean dregs of albumen composition,, keep moisture content below 7% through desolventizing machine precipitation (solvent recuperation), oven dry (temperature is controlled at 100 to 130 ℃);
(f) Hong Gan bean dregs are pulverized through pulverizer, and granularity requires the 100-120 order;
(g) remove skin of beancurd (fiber composition) through screening, sterilization can obtain the soybean protein concentrate of protein content more than 70%.
(2) extract the soybean small peptide
(a) the soybean protein concentrate solid substance that extracts being added water, to become pH value 7.4-8.0 ratio of water to material be 10-15: 1, stirred at normal temperatures 15-30 minute;
(b) separate with the disk centrifuge more than 7500 rev/mins, obtain containing protein slurry and fine-fibered;
(c) slurries are pumped into hydrolysis in intermittence that immobilized enzyme is housed or the continuous manipulation reactor, soybean protein hydrolysis liquid;
(d) hydrolyzed solution is passed through ultrafiltration membrance filter, obtain ultrafiltrated and soybean protein and soybean peptides (long-chain) mixture;
(e) with continuing hydrolysis in the mixture solid substance Returning reactor, obtain ultrafiltrated by ultra-filtration membrane once more;
(f) ultrafiltrated is passed through the ion exchange resin column desalination, through activated carbon decolorizing, deodorization;
(g) purified soybean small peptide is concentrated, sterilization, spraying drying, soybean small peptide product.
(3) extract soybean nucleic acid
(a) will extract obtain in the soybean protein concentrate technology contain nucleic acid, isoflavones, saponin, the transparent supernatant liquor of oligose, regain solvent through distilling to concentrate;
(b) concentrate feed liquid and adjust solid substance 1-2%, transfer pH value 2-3.5 with HCL with deionized water;
(c) flocculating aids that adds suitable proportion filters, the transparent supernatant liquor that obtains containing the flocculating aids precipitating curdled milk of nucleic acid and contain isoflavones, saponin, oligose composition;
(d) the flocculating aids precipitating curdled milk that will contain nucleic acid precipitates flocculating aids with first, the dissolve with ethanol nucleic acid of high purity more than 95%;
(e) filtration obtains transparent liquid through filter, and vacuum concentration is regained solvent and also is concentrated into solid content 7%-9%, through sterilization, drying, gets the soybean nucleic acid of content more than 60%.
(4) extract soybean isoflavones
(a) will extract obtain in the soybean nucleic acid technology contain isoflavones, saponin, the transparent liquid of oligose, by electrodialysis desalination, the feed liquid specific conductivity behind the desalination must not surpass 50us/cm
2
(b) feed liquid behind the desalination is contained soybean isoflavones, Soyasaponin by macroporous adsorbent resin in the material of resin absorption, and effusive feed liquid promptly is a soybean oligosaccharide;
(c) absorption with macroporous adsorbent resin is full close after, molten with 60-95% first, ethanol from wash-out;
(d) elutriant is regained solvent through concentrating;
(e) selection can separate dissolution with solvents, the stirring concentrated solution of isoflavones, saponin;
(f) separate through 10000 rev/mins high speed separator and draw the supernatant liquor that contains solid-state isoflavones and contain saponin;
(g) solid-state isoflavones is adjusted solid substance with deionized water, is concentrated into solid substance about 10%, can get the soybean isoflavones of content more than 80% through sterilization, spraying drying, and wherein Genistin (lignin) content is up to more than 80%.
(5) extract Soyasaponin
(a) extract the isolating supernatant liquor vacuum concentration of isoflavones technology high speed separating machine;
(b) selection can be separated out the solvent of saponin, as: acetone, ether (purity is more than 95%) fully stir with 1: 5 above ratio, separate through high speed separator, get the saponin solid matter;
(c) solid matter adds a certain amount of deionized water and concentrates, and regains solvent, and solid content 9%-11% through sterilization, spraying drying, can get the Soyasaponin of content more than 60%.
(6) extract soybean oligosaccharide
(a) through the effusive feed liquid that contains oligose of macroporous adsorbent resin, through reverse osmosis concentration to solid content 9%-11%;
(b) this feed liquid is further decoloured with gac, carclazyte;
(c) feed liquid after the decolouring is concentrated into solid content more than 40% through ultra-filtration membrane, through the liquid soybean oligosaccharide of direct canned one-tenth of sterilizing;
(d) Tuo Se feed liquid and dextrin are with after 1: 3 mixed, and solid substance is adjusted to the spraying drying standard, can get the soybean oligosaccharide of content 20-60% through sterilising spray.
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CN102669523B (en) * | 2011-03-14 | 2015-09-30 | 齐齐哈尔大学 | The preparation method of functional soya oligosaccharide |
CN102617702A (en) * | 2012-03-09 | 2012-08-01 | 姜浩奎 | Production method of peptidoglycan |
CN103053786A (en) * | 2012-12-17 | 2013-04-24 | 华南理工大学 | Preparation method for low-phytic acid calcium-tolerant soybean protein |
CN104152517A (en) * | 2013-05-15 | 2014-11-19 | 上海海洋大学 | Method for extracting short peptides from sea horses |
CN104286856A (en) * | 2014-10-20 | 2015-01-21 | 长春大学 | Production method of odorless high-purity soybean oligopeptide |
CN109123036A (en) * | 2018-08-06 | 2019-01-04 | 广州灵润生物科技有限公司 | Soybean-marrow peptide composition and application |
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