CN104530143B - Method for preparing soybean whey oligosaccharide through coupling of heating, flocculating, air floating and ultra-filtering - Google Patents
Method for preparing soybean whey oligosaccharide through coupling of heating, flocculating, air floating and ultra-filtering Download PDFInfo
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Abstract
The invention relates to a method for extracting a soybean whey oligosaccharide from soybean whey. The method concretely includes the steps that heating, flocculating, air floating and intermittent flow-crossing ultra-filtering are coupled; a segmented treatment mode is adopted in a ground-breaking mode at a pretreatment stage, and ingeniously combined with air floating separation; composite flocculants with specific components and a specific proportion are selected. The high-quality soybean oligosaccharide product low in maillard browning reaction occurrence rate is provided, the extraction ratio of the soybean whey oligosaccharide can reach 85% and is much higher than that at a common level in the field, the effect that all steps and parameters supplement each other and act in a coordinated mode is achieved, the cost is lowered, and the method is high in operability.
Description
Technical field
The invention belongs to food processing technology field, the present invention relates to a kind of extraction soybean oligo saccharide from soybean whey liquid
Method, a kind of method that heating, flocculation, air supporting and Ultrafiltration Coupling prepare soy-bean whey oligosaccharide.
Background technology
China is the native place of Semen sojae atricolor, and the developing history of bean product is long.In recent years, China puts into substantial amounts of manpower and materials
Having built up hundreds of soybean protein manufacturing enterprises, there is tens of family in the most fairly large producer.But with China's current technology water
Flat, often produce 1t soybean protein isolate and take around discharge 10t soya whey wastewater.Soybean Milk clear water is to produce soybean separation protein
In vain, the high concentrated organic wastewater that produces in the food products such as protein concentrate (acid system) and bean curd, its Main Ingredients and Appearance is: albumen
Matter, saccharide, salt.Traditional way is regarded to be had no the refuse of value and directly discharges, or through biochemical simple process
Discharge, not only pollutes environment, and wastes the material particularly useful to Human Physiology, i.e. soybean oligo saccharide and lactalbumin
Deng.Therefore, while soybean protein produces and develops rapidly, the recycling to the high added value resource in waste water, the most still
Extension to the product of Soybean production, also reduces the environmental pollution that soya whey wastewater is brought simultaneously.Therefore milk surum is given up
The developmental research of the soybean oligo saccharide in water has the highest market value and social value.Soybean oligo saccharide year demand in the world
Amount reaches 1.93 ten thousand t.Wherein the old people of China the most about about 600,000,000, child, anemia of pregnant woman the intestines and stomach is bad and the crowd such as diabetes, depend on
According to this target market, domestic soybean oligo saccharide market annual requirement just has ton up to ten thousand.Additionally, because of exclusive pure of soybean oligo saccharide
Natural characteristic, the aspect such as food, medicine and feed additive has a great application potential, and other oligosaccharide alternative or sugarcane
Sugar, is applied in other food, has immeasurable demand equally.
At present, from soybean whey liquid, the technological means of extraction purification soybean oligo saccharide is a lot, such as, membrance separation, heating,
Flocculant, ultrafiltration, centrifugal, ion exchange resin etc., also have between each means with the use of situation, but due to whey
In containing the small molecular protein of better heat stability, even if in above-mentioned heating or add flocculant etc. or the process cooperated
After, still there is most small molecular protein to be difficult to coagulative precipitation, it is also difficult to thoroughly to be divided by protein contained in soybean whey liquid
Separate out, cause there is also many practical problems such as extraction ratio is low, purification degrees is low, fouling membrane is serious, Membrane cleaning aborning.Ask
Topic is in particular in: although soybean whey liquid processes through early stage heating or flocculant etc., but poor effect, the solution before ultrafiltration
In still contain excess lactalbumin, owing to lactalbumin has certain viscosity, be easily attached on film, formed gel, make
Become Pore Blocking, thus cause membrane flux to be decayed rapidly, make ultrafiltration not to be normally carried out.Therefore, although remove lactalbumin
Means are a lot, but between each means, the effect of mutual coordinated is bad, does not has more preferable optimum organization, the most not to concrete skill
Art means carry out pioneering improvement, the most effectively solve the membrane pollution problem that lactalbumin brings.Further, since generally use sheet frame
Protein in filter separation soybean whey liquid, is necessary for adding substantial amounts of kieselguhr as filter aid, was therefore running
Journey will produce the mixed waste of substantial amounts of kieselguhr and albumen, and cause the pollution of environment.Therefore, how technique is obtained
Simply, easily operated, do not produce pollutant, film contamination resistance is strong, product yield high, quality is high soybean oligo saccharide preparation side
Method is this area urgent problem.
Summary of the invention
The purpose of the present invention: a kind of method extracting soybean oligo saccharide from soybean whey liquid, is specially one heating, wadding
The method that solidifying, air supporting prepares whey-soybean oligosaccharide with Ultrafiltration Coupling.A kind of high-quality soybean oligo saccharide is provided simultaneously, increases and produce
Product scientific and technological content, adds the economic benefit of enterprise.
Present invention solves the technical problem that: the present invention solves present in prior art, although remove lactalbumin
Means are a lot, but the poor effect of mutual coordinated between each means, the most concrete technological means do not carried out pioneering changing
The problem entered；Substantially increase quality and the yield of product；Effectively solve the membrane pollution problem that lactalbumin brings；Do not produce ring
The pollution in border.Provide that a kind of technique is simple, easily operated, do not produce pollutant, film contamination resistance is strong, product yield is high,
The soybean oligo saccharide preparation method that quality is high.
Technical scheme: the extraction purification preparation method of a kind of soybean oligo saccharide, it is characterised in that according to following
Prepared by step:
(1) stage pretreatment: first stage: first by soybean whey liquid under the conditions of pH value=4.5-5.5, be heated to 50
DEG C-55 DEG C, keep 1-2h；Second stage: then under the conditions of pH value=6.0-8.5, is heated to 90 DEG C-92 DEG C, keeps 10-15
Minute, complete pretreatment；Phase III: natural cooling, stand to soy-bean whey liquid temp simultaneously and be 50-60 DEG C；It is centrifuged afterwards
Obtain centrifugal liquid A standby；
(2) flocculant flocculation: mix with centrifugal liquid A with flocculant solution, make centrifugal liquid A flocculate, slightly extracted
Liquid, flocculant and centrifugal liquid are based on mass volume ratio: overall flocculant usage is 0.7-0.9g/L centrifugal liquid A, and flocculating conditions is
PH4.5-6.0, temperature 50-60 DEG C, quiet heavy time 40-90min；Centrifugal liquid B is obtained standby after Li Xin；Wherein, flocculant is that shell gathers
Sugar, or chitosan, aluminum chloride and sodium alginate three's mixture, and chitosan, aluminum chloride and sodium alginate usage ratio
It is 4:3:2 by quality ratio；Further preferably flocculant is the mixture of chitosan and hydroxypropyl starch, and specific usage ratio
It is 4:1 by quality ratio, but this flocculant usage amount is replaced with 0.07-0.09g/L centrifugal liquid A；
(3) dissolved air flotation: centrifugal liquid B that step (2) obtains be input in air-floating apparatus, obtains air supporting and divides after dissolved air flotation
From whey；
(4) Ultrafiltration Purifying: the dissolved air flotation whey after the air-float purification that will obtain in step (3) pours ultrafiltration apparatus into
In, use batch (-type) cross-flow ultrafiltration to carry out Ultrafiltration Purifying, the liquid collected is raw sugar liquid；Wherein, batch (-type) cross-flow ultrafiltration work
Skill parameter: transmembrane pressure 60-65 KPa or 65-70KPa, pH value 7.0-7.5, extension rate 1 times；
(5) desalination bleaching: the raw sugar liquid obtained in step (4) is passed through exchange resin elution, uses 001 × the last 7
Acid cation exchange resin post is sequentially connected with the moon after first sun with D301-T macroporous weakly basic anion exchange resin, wherein,
Desalination bleaching condition is: 001 × 7 strong acid cation exchange resin column and D301-T macroreticular weakly base anion exchange tree
Fat column volume ratio 1: 1, flow velocity 2.0-2.5 BV/h；
(6) lyophilizing: the soy oligosaccharides sugar juice after the desalination bleaching that will obtain in step (5) is placed in freezer dryer cold
Lyophilizing is dry, and obtaining white powder is soybean oligo saccharide；Wherein, preferably freeze drying machine parameter: suction 1Pa, cold well temperature-
50 DEG C, oligosaccharide solution is placed in freezer dryer and continues 16-24h lyophilization.
Preferred stage pretreatment: first stage: first by soybean whey liquid under the conditions of pH value=5-5.2, be heated to
When 52 DEG C-53 DEG C, keep 1.5h；Second stage: then under the conditions of pH value=7, is heated to 90 DEG C, keeps 15 minutes；3rd
Stage: natural cooling, stand simultaneously to soy-bean whey liquid temp be 55 DEG C.
Preferred steps (4) Ultrafiltration Purifying uses the ultrafilter membrane of MWCO3000 or interception to be the regenerated cellulose of 5000kDa
Ultrafilter membrane or the ultrafilter membrane of MWCO 8000.
The dissolved air flotation of preferred steps (4) step (3), the air pressure in air-floating apparatus is 0.7Mpa-0.9Mpa, charging
Liquid temp 50 DEG C-55 DEG C.
Soybean oligo saccharide prepared by this invention has in prepared by acidic beverages well applies effect, this soybean oligo saccharide
The generation of Maillard reaction can be significantly reduced；The pH value of acidic beverages is 4～7 or lower.
Beneficial effects of the present invention:
(1) present invention uses the processing mode of stagewise pioneeringly at soybean whey liquid pretreatment stage, overcomes list
The prejudice of one condition heat treated, inventor, on the basis of previous work, is found surprisingly that in research, uses following pre-place
Reason, i.e. first by soybean whey liquid under the conditions of pH value=4.5-5.5, be heated to 50 DEG C-55 DEG C, keeps 1-2h；Then at pH value
Under the conditions of=6.0-7.5, it is heated to 90 DEG C-92 DEG C, keeps 10-15 minute, last natural cooling, stand to temperature simultaneously and be
50-60℃；Achieving unthinkable technique effect, the content of soybean oligo saccharide finished product, purity and quality are greatly improved, and film is dirty
Dye problem is the most effectively solved.First by soybean whey liquid under the conditions of pH value=4.5-5.5, when being heated to 50 DEG C-55 DEG C, protect
Hold 1-2h, in the process, creatively sterilizing, lactalbumin degeneration precipitation or protein molecular are fully extended, promote milk surum
Albumen be embedded in intramolecular a large amount of hydrophobic group gradually expose, the Maillard reaction reducing soybean oligo saccharide etc. beneficial effect
Effectively combine.In the process, creatively first process with temperate condition, lactalbumin in weakly acidic condition not
The opaque Weak Gels of disconnected formation, and compared to elastic clear gel, this Weak Gels has certain viscosity, bigger surface area,
Weak Gels can again act as adsorbent, a certain amount of albumen in absorption system, and this efficiently utilizes the formation Weak Gels stage；
The mode using high temperature, short time afterwards makes lactalbumin rapid condensation precipitate, and decreases the high temperature shadow to soybean oligo saccharide quality
Ring, kill may prolific in following process, can the microorganism of decomposing soybean oligosaccharide, substantially increase again simultaneously
Settling velocity and precipitation capacity, make a large amount of lactalbumin form transparent resilient gel and be easily isolated；Last natural cooling, quiet
Put to the process reality that temperature is 50-60 DEG C be also complicated precipitation and the process fully interacted.Above-mentioned place stage by stage
Reason, the extremely effective extracted amount that improve soybean oligo saccharide and purity；Inventor is also found surprisingly that, this pre-assistant subtracts significantly
Lack the usage amount of flocculant, the conventional steps necessary such as the freezing process also need not beneficially flocculated before flocculation, the most more
Adding follow-up air-flotation process effect, the membrane pollution problem of long-standing problem this area is the most effectively solved.It addition, second-order
The pH value of section is close with the pH value of flocculant flocculated stage, decreases operation, has saved time and cost, it is to avoid system pH
Change and the vibrations of unnecessary pH value repeatedly.
(2) present invention is innovatively by pretreatment mode unique for soybean whey liquid and the ingenious combination of dissolved air flotation.Although making
After flocculant, whey solution still contains the albumen of undenatured precipitation, peptide etc., needs before ultrafiltration the most effectively to locate
Reason；Owing to have employed the processing mode of stagewise at soybean whey liquid pretreatment stage, the unmodified whey protein molecules of part
In structure, also acquisition is fully extended, lactalbumin is embedded in intramolecular a large amount of hydrophobic group and the most gradually comes out, and polypeptide is also
Coming to life, hydrophobic group interacts, and adds ability of aggregation, the easier floating such as the albumen that flocculates not removed, peptide,
And present certain frothing capacity at air supporting liquid level and mutually bond, thus improve protein and be oriented in the energy of oil-water interfaces
Power, advantageously in the removal of albumen etc., it is also possible to omits common high speed centrifugation separating step before dissolved air flotation.
(3) flocculant that the present invention selects is unique, develops two kinds of built-up flocculants being suitable for soy-bean whey.Send out
A person of good sense, during seeking optimum flocculent, is found surprisingly that, when the mixture that flocculant is chitosan and hydroxypropyl starch,
And specific usage ratio is 4:1 by quality ratio, flocculation there occurs that the change of matter, more protein are flocculated further
Getting off, this flocculant usage amount is also successively decreased with the multiple of the order of magnitude, and the addition of flocculant is centrifuged by original 0.7-0.9g/L
Liquid A, is reduced to 0.07-0.09g/L centrifugal liquid A, and two kinds of components produce effective synergism, and use other modified starch and
Other ions are worked in coordination with chitosan, and it is good with hydroxypropyl starch synergy that effect is all not so good as.And hydroxypropyl starch is cheap,
Product cost can be reduced into, and have wider temperature and pH value range, use flexibly, do not limited by high/low temperature and acid-base value
System, preferably high substitution value hydroxypropyl starch.This is likely due to, propoxyl side chain number on glucose unit in hydroxypropyl starch
Mesh increases, and length increases, and the free terminal number of molecule increases, and molecule is transitioned into branching molecule, molecule free end by spiral line type molecule
Number is the most, and affine, absorption more strengthens, and more readily diffuses in other molecule, when the temperature increases, and hydroxypropyl starch molecule
Warm-up movement accelerate, collision frequency increases, and intermolecular absorption is wound network structure, is formed more with positively charged chitosan
Powerful network body, plays bridging and the trapping cleaning effect of uniqueness, because itself belongs to during chitosan with protein coacervation
In non-ionic starch derivant, it will not produce impact to the amount of charge of system again.Chitosan, water insoluble, can be dissolved in
Diluted acid, the product after deacetylation, can be absorbed by the body, chitosan is gradually degraded in an acidic solution, as the pH of solution
During less than dissociation constant (PKa) of chitosan, amino will completely or partially be protonated, and now chitosan is positively charged.If this
Time solution pH more than the average isoelectric point, IP of protein, then protein molecule will due to-COO-group band net negative charge, band is just
The chitosan of electric charge is i.e. combined by electrostatic attraction with electronegative protein colloid, the electric charge fall of protein adhesive surface
Low, make colloidal solid de-steady and produce flocculating sedimentation, form linear polymer；But be used alone flocculate with chitosan and there is cost
Height, flocculation depends on the quantity of sour environment and positive and negative charge, and chitosan dosage is too high also easily produces embedding effect to albumen,
It is unfavorable for charging neutrality.The use of hydroxypropyl starch is it can be avoided that chitosan produces embedding effect to albumen.This flocculant is into
This relatively low " green " flocculant.The problem effectively solving fouling membrane.The deacetylating degree of chitosan of the application is preferably greater than 90%.
Flocculant of the present invention can also be the mixture of chitosan, polymerization aluminum chloride and sodium alginate three, and specific
Usage ratio is 4:3:2 by quality ratio, achieves unexpected flocculating effect.This composite flocculation agent can be dedicated to
The flocculation of soybean whey protein.Not having the particular combination of this kind of composite flocculation agent in prior art, staff is also not easy
Three assembles and produces the effect of excellence.The problem that this flocculant effectively solves fouling membrane.
(4) present invention also provides for the soy oligosaccharides sugar product that a kind of Maillaid braun reaction incidence rate is low.Inventor is unexpected
Discovery, the soybean oligo saccharide prepared with conventional method of soybean oligo saccharide obtained according to the inventive method or commercial products ratio
Relatively, Maillaid braun reaction incidence rate has a significantly reduction, and especially acid or tend in neutral beverage, this is very beneficial for
Soybean oligo saccharide application in acidic beverages is processed, because beverage processing would generally avoid Maillaid braun reaction as far as possible
Occur.
(5) target product that the present invention is obtained is each operation and parameter complements each other, common synergistic result, subtracts
Few operation, reduces cost, creates unforeseeable technique effect.The extraction ratio of product of the present invention improves than conventional method
15-20%, makes the extraction rate reached of whey-soybean oligosaccharide to 79-85%.
Drawing through test, cross-flow interval ultrafiltration mode is suitable to separate soy-bean whey oligosaccharide, and Responds Surface Methodology (RSM) is excellent
Change obtain optimum reaction condition be pressure 60KPa, pH value 7.3, extension rate 1 times, under the conditions of this, retention rate of proteins, total sugar pass through
Rate is respectively 99.10% and 86.16%, and analyzes through HPLC, and ultrafiltration gained cottonseed sugar, content of stachyose are respectively 0.90-1.20
mg/ml、4.89-5.83mg/ml.Gained raw sugar liquid light transmittance is brought up to 93.6% by 68.1%, and clear, in faint yellow.
The white powder of soybean oligo saccharide prepared by the present invention, with the presence of a little crystalline lens, indices index all meets
Physical and chemical standards in GB/T 22491-2008.
Flocculant contrast test: to gained treatment fluid analyzing proteins content, retention rate of proteins, total sugar transmitance, fouling membrane
The indexs such as degree；Other process conditions all use the present invention's and identical；Chitosan, aluminum chloride and sodium alginate three's mixture
Proportioning is 4:3:2 by quality ratio, and addition is 0.7-0.9g/L centrifugal liquid A；Chitosan and the mixture of hydroxypropyl starch, and
Specific usage ratio is 4:1 by quality ratio, and addition is 0.07-0.09g/L centrifugal liquid A；Chitosan dosage is 0.7-0.9g/
L centrifugal liquid A；Albumen removal efficiency, retention rate of proteins, total sugar calculate the most according to a conventional method through each indexs such as filter, fouling membrane；Result
It is shown in Table 1.
Table 1
Note: before and after a, b, c represent process, the difference in change opposite sex is notable (P<0.05), parallel frequency n>=3.
The purpose that soya whey wastewater carries out pretreatment is to remove macromole quality protein in soya whey wastewater
Matter, clarified wastewater, and it is more preferable to make the waste water after this process carry out effect when oligosaccharide is prepared in ultrafiltration, reduces ultrafilter membrane simultaneously
Pollute.Result shows: the retention rate of proteins diversity of three kinds of methods is not notable, total sugar transmitance and the equal significant difference of fouling degree of membrane
(P ＜ 0.05).Chitosan, aluminum chloride are with sodium alginate compared with single chitosan flocculating method, and protein removal rate is bright
Showing and increase, treatment fluid fouling membrane after ultrafiltration is the least.Chitosan is higher with hydroxypropyl starch flocculence albumen removal efficiency, reaches 50%
Above, and total sugar transmitance is the highest, and fouling degree of membrane is minimum, and relatively stock solution reduces more than 40%.It is essential that chitosan and hydroxypropyl
Starch consumption is little, it is possible to be substantially reduced cost.
The Mei Lade brown stain test of soybean oligo saccharide
Accurately weigh soybean oligo saccharide sample, be configured to the solution of 10%, take 2mL and add the glycine 2mL of 0.5%, so
Rear addition HCI or the aqueous solution 4mL of NaOH regulating allocation pH value 4-10, and in boiling water bath, heat 90min, it is cooled to room temperature
After, colorimetric determination under 420nm, deionized water makees reference, and it is commercial that matched group is commercial soybean oligo saccharide or conventional method obtains
Soybean oligo saccharide.Result such as table 2 below:
Table 2
| Sample | pH4 | pH5 | pH6 | pH7 | pH8 | pH9 | pH10 |
| Soybean oligo saccharide of the present invention | 0.03 | 0.05 | 0.11 | 0.12 | 0.32 | 0.56 | 0.67 |
| Commercially available soybean oligo saccharide 1 | 0.09 | 0.22 | 0.30 | 0.46 | 0.62 | 0.68 | 0.8 |
| Commercially available soybean oligo saccharide 2 | 0.1 | 0.20 | 0.29 | 0.39 | 0.58 | 0.75 | 0.8 |
Table 2 is shown that the soybean oligo saccharide of separate sources to be changed in the browning degree of pH value 4～10.It can be seen that this
The soybean oligo saccharide of invention is when pH value 4～7, and soybean oligo saccharide brown stain degree is relatively low, and change is little, the soybean oligo saccharide of the present invention
Brown stain degree changes notable under acidity and neutrallty condition, and under the conditions of alkalescence, brown stain degree is higher；And commercially available two soy oligosaccharides
Sugar-like product are changed significantly under acidity and neutrallty condition, and under the conditions of alkalescence, brown stain degree is the highest.Commercially available soybean oligo saccharide 1 and 2 exists
It is easier under sour environment browning reaction.The soybean oligo saccharide carbonyl amine condensation product of this possible present invention is easy to hydrolysis leads
Cause, be unfavorable for the carrying out of Maillard reaction.
Embodiment 1
The extraction purification preparation method of a kind of soybean oligo saccharide, it is characterised in that prepare according to following steps:
(1) stage pretreatment: first stage: first by soybean whey liquid under the conditions of pH value=4.5, is heated to 50 DEG C
DEG C, keep 1 hour；Second stage: then under the conditions of pH value=6.0, is heated to 90 DEG C DEG C, keeps 10 minutes；Phase III:
Natural cooling, stand simultaneously to soy-bean whey liquid temp be 50 DEG C；Centrifugal that centrifugal liquid A is standby afterwards；
(2) flocculant flocculation: mix with centrifugal liquid A with flocculant, make centrifugal liquid A flocculate, obtain crude extract, wadding
Solidifying agent with centrifugal liquid based on mass volume ratio: overall flocculant usage is 0.7g/L centrifugal liquid A, and flocculating conditions is pH4.5, temperature 50
DEG C, quiet heavy time 40min；Centrifugal liquid B is obtained standby after Li Xin；Wherein, flocculant is chitosan, aluminum chloride and sodium alginate three
Person's mixture, and chitosan, aluminum chloride and sodium alginate usage ratio be 4:3:2 by quality ratio；
(3) dissolved air flotation: centrifugal liquid B that step (2) obtains be input in air-floating apparatus, obtains air supporting and divides after dissolved air flotation
From whey；Air pressure in air-floating apparatus is 0.7Mpa, feeding liquid temperature 50 C；
(4) Ultrafiltration Purifying: the dissolved air flotation whey after the air-float purification that will obtain in step (3) pours ultrafiltration apparatus into
In, use batch (-type) cross-flow ultrafiltration to carry out Ultrafiltration Purifying, the liquid collected is raw sugar liquid；Wherein, batch (-type) cross-flow ultrafiltration work
Skill parameter: transmembrane pressure 60-65 KPa or 65-70KPa, pH value 7.0-7.5, extension rate 1 times；Preferably employ MWCO3000's
Ultrafilter membrane；
(5) desalination bleaching: the raw sugar liquid obtained in step (4) is passed through exchange resin elution, uses 001 × the last 7
Acid cation exchange resin post is sequentially connected with the moon after first sun with D301-T macroporous weakly basic anion exchange resin, wherein,
Desalination bleaching condition is: 001 × 7 strong acid cation exchange resin column and D301-T macroreticular weakly base anion exchange tree
Fat column volume ratio 1: 1, flow velocity 2.0-2.5 BV/h；
(6) lyophilizing: the soy oligosaccharides sugar juice after the desalination bleaching that will obtain in step (5) is placed in freezer dryer cold
Lyophilizing is dry, and obtaining white powder is soybean oligo saccharide；Wherein, preferably freeze drying machine parameter: suction 1Pa, cold well temperature-
50 DEG C, oligosaccharide solution is placed in freezer dryer and continues 16-24h lyophilization.
Whey-soybean oligosaccharide extraction ratio is about 81%
Embodiment 2
The extraction purification preparation method of a kind of soybean oligo saccharide, it is characterised in that prepare according to following steps:
(1) stage pretreatment: first stage: first by soybean whey liquid under the conditions of pH value=5.0, is heated to 55 DEG C,
Keep 2h；Second stage: then under the conditions of pH value=8.5, is heated to 92 DEG C, keeps 15 minutes；Phase III: the coldest
But, stand simultaneously to soy-bean whey liquid temp be 60 DEG C；Centrifugal that centrifugal liquid A is standby afterwards；
(2) flocculant flocculation: mix with centrifugal liquid A with flocculant, make centrifugal liquid A flocculate, obtain crude extract, wadding
Solidifying agent with centrifugal liquid based on mass volume ratio: overall flocculant usage is 0.7-0.9g/L centrifugal liquid A, and flocculating conditions is pH4.5-
6.0, temperature 50-60 DEG C, quiet heavy time 40-90min；Centrifugal liquid B is obtained standby after Li Xin；Wherein, flocculant is chitosan；
(3) dissolved air flotation: centrifugal liquid B that step (2) obtains be input in air-floating apparatus, obtains air supporting and divides after dissolved air flotation
From whey；Air pressure in air-floating apparatus is 0.9Mpa, feeding liquid temperature 55 DEG C；
(4) Ultrafiltration Purifying: the dissolved air flotation whey after the air-float purification that will obtain in step (3) pours ultrafiltration apparatus into
In, use batch (-type) cross-flow ultrafiltration to carry out Ultrafiltration Purifying, the liquid collected is raw sugar liquid；Wherein, batch (-type) cross-flow ultrafiltration work
Skill parameter: transmembrane pressure 60-65 KPa or 65-70KPa, pH value 7.0-7.5, extension rate 1 times；Employing interception is
The regenerated cellulose ultrafilter membrane of 5000kDa；
(5) desalination bleaching: the raw sugar liquid obtained in step (4) is passed through exchange resin elution, uses 001 × the last 7
Acid cation exchange resin post is sequentially connected with the moon after first sun with D301-T macroporous weakly basic anion exchange resin, wherein,
Desalination bleaching condition is: 001 × 7 strong acid cation exchange resin column and D301-T macroreticular weakly base anion exchange tree
Fat column volume ratio 1: 1, flow velocity 2.0-2.5 BV/h；
(6) lyophilizing: the soy oligosaccharides sugar juice after the desalination bleaching that will obtain in step (5) is placed in freezer dryer cold
Lyophilizing is dry, and obtaining white powder is soybean oligo saccharide；Wherein, preferably freeze drying machine parameter: suction 1Pa, cold well temperature-
50 DEG C, oligosaccharide solution is placed in freezer dryer and continues 16-24h lyophilization.Whey-soybean oligosaccharide extraction ratio is about 79%.
Embodiment 3
The extraction purification preparation method of a kind of soybean oligo saccharide, it is characterised in that prepare according to following steps:
(1) stage pretreatment: first stage: first by soybean whey liquid under the conditions of pH value=5.0, is heated to 55 DEG C,
Keep 2h；Second stage: then under the conditions of pH value=8.5, is heated to 92 DEG C, keeps 15 minutes；Phase III: the coldest
But, stand simultaneously to soy-bean whey liquid temp be 60 DEG C；Centrifugal that centrifugal liquid A is standby afterwards；
(2) flocculant flocculation: mix with centrifugal liquid A with flocculant, make centrifugal liquid A flocculate, obtain crude extract, wadding
Solidifying agent with centrifugal liquid based on mass volume ratio: overall flocculant usage is 0.07-0.09g/L centrifugal liquid A, and flocculating conditions is pH4.5-
6.0, temperature 50-60 DEG C, quiet heavy time 40-90min；Centrifugal liquid B is obtained standby after Li Xin；Wherein, flocculant is chitosan and hydroxyl
The mixture of propyl group starch, and specific usage ratio is 4:1 by quality ratio；
(3) dissolved air flotation: centrifugal liquid B that step (2) obtains be input in air-floating apparatus, obtains air supporting and divides after dissolved air flotation
From whey；Air pressure in air-floating apparatus is 0.9Mpa, feeding liquid temperature 55 DEG C；
(4) Ultrafiltration Purifying: the dissolved air flotation whey after the air-float purification that will obtain in step (3) pours ultrafiltration apparatus into
In, use batch (-type) cross-flow ultrafiltration to carry out Ultrafiltration Purifying, the liquid collected is raw sugar liquid；Wherein, batch (-type) cross-flow ultrafiltration work
Skill parameter: transmembrane pressure 60-65 KPa or 65-70KPa, pH value 7.0-7.5, extension rate 1 times；Employing interception is
The regenerated cellulose ultrafilter membrane of 5000kDa；
(5) desalination bleaching: the raw sugar liquid obtained in step (4) is passed through exchange resin elution, uses 001 × the last 7
Acid cation exchange resin post is sequentially connected with the moon after first sun with D301-T macroporous weakly basic anion exchange resin, wherein,
Desalination bleaching condition is: 001 × 7 strong acid cation exchange resin column and D301-T macroreticular weakly base anion exchange tree
Fat column volume ratio 1: 1, flow velocity 2.0-2.5 BV/h；
(6) lyophilizing: the soy oligosaccharides sugar juice after the desalination bleaching that will obtain in step (5) is placed in freezer dryer cold
Lyophilizing is dry, and obtaining white powder is soybean oligo saccharide；Wherein, preferably freeze drying machine parameter: suction 1Pa, cold well temperature-
50 DEG C, oligosaccharide solution is placed in freezer dryer and continues 16-24h lyophilization.Whey-soybean oligosaccharide extraction ratio is about 85%.
Claims (2)
1. the extraction purification preparation method of a soybean oligo saccharide, it is characterised in that prepare according to following steps:
(1) stage pretreatment: first stage: first by soybean whey liquid under the conditions of pH value=4.5-5.5, be heated to 50 DEG C-
55 DEG C, keep 1-2h；Second stage: then under the conditions of pH value=6.0-8.5, is heated to 90 DEG C-92 DEG C, keeps 10-15 to divide
Clock；Phase III: natural cooling, stand to soy-bean whey liquid temp simultaneously and be 50-60 DEG C；Centrifugal that centrifugal liquid A is standby afterwards；
(2) flocculant flocculation: mix with centrifugal liquid A with flocculant, make centrifugal liquid A flocculate, obtain crude extract, flocculant
With centrifugal liquid A based on mass volume ratio: overall flocculant usage is 0.7-0.9g/L centrifugal liquid A, flocculating conditions is pH4.5-6.0,
Temperature 50-60 DEG C, quiet heavy time 40-90min；Centrifugal liquid B is obtained standby after Li Xin；Wherein, flocculant is chitosan, or shell gathers
Sugar, aluminum chloride and sodium alginate three's mixture, and chitosan, aluminum chloride are with sodium alginate usage ratio by quality ratio
For 4:3:2；Or the mixture that flocculant is chitosan and hydroxypropyl starch, and specific usage ratio is 4:1 by quality ratio,
But this flocculant usage amount is replaced with 0.07-0.09g/L centrifugal liquid A；Wherein deacetylating degree of chitosan is more than 90%；
(3) dissolved air flotation: centrifugal liquid B that step (2) obtains be input in air-floating apparatus, after obtaining dissolved air flotation after dissolved air flotation
Whey；Air pressure in air-floating apparatus is 0.7Mpa-0.9Mpa, feeding liquid temperature 50 C-55 DEG C；
(4) Ultrafiltration Purifying: the dissolved air flotation whey after the air-float purification that will obtain in step (3) is poured in ultrafiltration apparatus, adopts
Carrying out Ultrafiltration Purifying with batch (-type) cross-flow ultrafiltration, the liquid collected is raw sugar liquid；Wherein, batch (-type) cross-flow ultrafiltration technology ginseng
Number: transmembrane pressure 60-65 KPa or 65-70KPa, pH value 7.0-7.5, extension rate 1 times；Ultrafiltration Purifying uses MWCO3000's
Ultrafilter membrane or regenerated cellulose ultrafilter membrane that interception is 5000kDa or the ultrafilter membrane of MWCO 8000；
(5) desalination bleaching: the raw sugar liquid obtained in step (4) is passed through exchange resin elution, uses 001 × 7 highly acid
Cation exchange resin column is sequentially connected with the moon after first sun with D301-T macroporous weakly basic anion exchange resin, obtains Semen sojae atricolor
Oligosaccharide solution；Wherein, desalination bleaching condition is: 001 × 7 strong acid cation exchange resin column is weak with D301-T macropore
Basic anion exchange resin column volume ratio 1: 1, flow velocity 2.0-3.0 BV/h；
(6) lyophilizing: the soy oligosaccharides sugar juice after the desalination bleaching that will obtain in step (5) is placed in freezer dryer freezing dry
Dry, obtaining white powder is soybean oligo saccharide；This soybean oligo saccharide can significantly reduce the generation of Maillard reaction；Wherein, cold
Lyophilizer parameter: suction 10Pa, cold well temperature-50 DEG C, it is cold that oligosaccharide solution is placed in freezer dryer lasting 16-24h
Lyophilizing is dry.
The extraction purification preparation method of a kind of soybean oligo saccharide the most according to claim 1, it is characterised in that stage pre-
Process: the first stage: first by soybean whey liquid under the conditions of pH value=5-5.2, be heated to 52 DEG C-53 DEG C, keep 1.5h；Second
In the stage: then under the conditions of pH value=7, it is heated to 90 DEG C, keeps 15 minutes；Phase III: natural cooling, stand to greatly simultaneously
Soyabean milk clear liquid temperature is 55 DEG C.
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| CN105439397B (en) * | 2016-01-20 | 2017-12-08 | 山东禹王生态食业有限公司 | A kind of soybean protein whey wastewater handling process |
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| CN1128151C (en) * | 2001-01-19 | 2003-11-19 | 北京中联捷思科技发展有限公司 | Method for extracting soy bean oligosaccharide from soy bean whey water |
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