CN104593446B - A kind of preparation method of pure xylo-oligosaccharide powder - Google Patents
A kind of preparation method of pure xylo-oligosaccharide powder Download PDFInfo
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- CN104593446B CN104593446B CN201410819669.3A CN201410819669A CN104593446B CN 104593446 B CN104593446 B CN 104593446B CN 201410819669 A CN201410819669 A CN 201410819669A CN 104593446 B CN104593446 B CN 104593446B
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- xylo
- zytase
- oligosaccharide
- xylan
- liquid
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- HEBKCHPVOIAQTA-NGQZWQHPSA-N d-xylitol Chemical compound OC[C@H](O)C(O)[C@H](O)CO HEBKCHPVOIAQTA-NGQZWQHPSA-N 0.000 title claims abstract description 68
- 239000000843 powder Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 51
- 229920001221 xylan Polymers 0.000 claims abstract description 35
- 150000004823 xylans Chemical class 0.000 claims abstract description 35
- 239000007864 aqueous solution Substances 0.000 claims abstract description 18
- 238000011084 recovery Methods 0.000 claims abstract description 10
- 239000006188 syrup Substances 0.000 claims abstract description 10
- 235000020357 syrup Nutrition 0.000 claims abstract description 10
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 238000004064 recycling Methods 0.000 claims abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000004880 explosion Methods 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 10
- 230000000694 effects Effects 0.000 claims description 9
- 238000000926 separation method Methods 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 8
- 238000001704 evaporation Methods 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- 239000002023 wood Substances 0.000 claims description 6
- 108090000790 Enzymes Proteins 0.000 claims description 5
- 102000004190 Enzymes Human genes 0.000 claims description 5
- 240000008042 Zea mays Species 0.000 claims description 5
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 239000000049 pigment Substances 0.000 claims description 5
- 239000003377 acid catalyst Substances 0.000 claims description 4
- 230000008020 evaporation Effects 0.000 claims description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid group Chemical group S(O)(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 108010089934 carbohydrase Proteins 0.000 claims description 3
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 2
- 108010001682 Dextranase Proteins 0.000 claims description 2
- 235000016383 Zea mays subsp huehuetenangensis Nutrition 0.000 claims description 2
- 235000008504 concentrate Nutrition 0.000 claims description 2
- 239000012141 concentrate Substances 0.000 claims description 2
- 235000019253 formic acid Nutrition 0.000 claims description 2
- 239000003456 ion exchange resin Substances 0.000 claims description 2
- 229920003303 ion-exchange polymer Polymers 0.000 claims description 2
- 235000009973 maize Nutrition 0.000 claims description 2
- 235000012054 meals Nutrition 0.000 claims description 2
- 238000000746 purification Methods 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- SRBFZHDQGSBBOR-IOVATXLUSA-N D-xylopyranose Chemical compound O[C@@H]1COC(O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-IOVATXLUSA-N 0.000 claims 2
- PYMYPHUHKUWMLA-UHFFFAOYSA-N arabinose Natural products OCC(O)C(O)C(O)C=O PYMYPHUHKUWMLA-UHFFFAOYSA-N 0.000 claims 1
- SRBFZHDQGSBBOR-UHFFFAOYSA-N beta-D-Pyranose-Lyxose Natural products OC1COC(O)C(O)C1O SRBFZHDQGSBBOR-UHFFFAOYSA-N 0.000 claims 1
- 238000002203 pretreatment Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 230000035943 smell Effects 0.000 description 10
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Chemical compound OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 6
- 239000000546 pharmaceutical excipient Substances 0.000 description 6
- 230000007062 hydrolysis Effects 0.000 description 5
- 238000006460 hydrolysis reaction Methods 0.000 description 5
- 238000005342 ion exchange Methods 0.000 description 4
- 229920001542 oligosaccharide Polymers 0.000 description 4
- 229920001353 Dextrin Polymers 0.000 description 3
- 239000004375 Dextrin Substances 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 239000002202 Polyethylene glycol Substances 0.000 description 3
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 3
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 3
- 235000011130 ammonium sulphate Nutrition 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000004061 bleaching Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 235000005822 corn Nutrition 0.000 description 3
- 235000019425 dextrin Nutrition 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000006047 enzymatic hydrolysis reaction Methods 0.000 description 3
- 150000002482 oligosaccharides Chemical class 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 229920001223 polyethylene glycol Polymers 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 240000007594 Oryza sativa Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 150000004676 glycans Chemical class 0.000 description 2
- 239000010903 husk Substances 0.000 description 2
- 239000002932 luster Substances 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 229960003487 xylose Drugs 0.000 description 2
- LGQKSQQRKHFMLI-SJYYZXOBSA-N (2s,3r,4s,5r)-2-[(3r,4r,5r,6r)-4,5,6-trihydroxyoxan-3-yl]oxyoxane-3,4,5-triol Chemical compound O[C@@H]1[C@@H](O)[C@H](O)CO[C@H]1O[C@H]1[C@H](O)[C@@H](O)[C@H](O)OC1 LGQKSQQRKHFMLI-SJYYZXOBSA-N 0.000 description 1
- JCSJTDYCNQHPRJ-UHFFFAOYSA-N 20-hydroxyecdysone 2,3-acetonide Natural products OC1C(O)C(O)COC1OC1C(O)C(O)C(OC2C(C(O)C(O)OC2)O)OC1 JCSJTDYCNQHPRJ-UHFFFAOYSA-N 0.000 description 1
- LGQKSQQRKHFMLI-UHFFFAOYSA-N 4-O-beta-D-xylopyranosyl-beta-D-xylopyranose Natural products OC1C(O)C(O)COC1OC1C(O)C(O)C(O)OC1 LGQKSQQRKHFMLI-UHFFFAOYSA-N 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- SQNRKWHRVIAKLP-UHFFFAOYSA-N D-xylobiose Natural products O=CC(O)C(O)C(CO)OC1OCC(O)C(O)C1O SQNRKWHRVIAKLP-UHFFFAOYSA-N 0.000 description 1
- 229920002488 Hemicellulose Polymers 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- JVZHSOSUTPAVII-UHFFFAOYSA-N Xylotetraose Natural products OCC(OC1OCC(OC2OCC(OC3OCC(O)C(O)C3O)C(O)C2O)C(O)C1O)C(O)C(O)C=O JVZHSOSUTPAVII-UHFFFAOYSA-N 0.000 description 1
- SRBFZHDQGSBBOR-LECHCGJUSA-N alpha-D-xylose Chemical compound O[C@@H]1CO[C@H](O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-LECHCGJUSA-N 0.000 description 1
- 239000001166 ammonium sulphate Substances 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- JCSJTDYCNQHPRJ-FDVJSPBESA-N beta-D-Xylp-(1->4)-beta-D-Xylp-(1->4)-D-Xylp Chemical compound O[C@@H]1[C@@H](O)[C@H](O)CO[C@H]1O[C@H]1[C@H](O)[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](O)C(O)OC2)O)OC1 JCSJTDYCNQHPRJ-FDVJSPBESA-N 0.000 description 1
- 238000009395 breeding Methods 0.000 description 1
- 230000001488 breeding effect Effects 0.000 description 1
- -1 by cooling Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010612 desalination reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 235000015816 nutrient absorption Nutrition 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 150000005846 sugar alcohols Chemical class 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- ABKNGTPZXRUSOI-UHFFFAOYSA-N xylotriose Natural products OCC(OC1OCC(OC2OCC(O)C(O)C2O)C(O)C1O)C(O)C(O)C=O ABKNGTPZXRUSOI-UHFFFAOYSA-N 0.000 description 1
Abstract
The invention discloses a kind of preparation method of pure xylo-oligosaccharide powder, the pH value of the adjustment xylan aqueous solution is 3.0 6.0, adds zytase enzymolysis, obtains the xylan enzymolysis liquid containing zytase；Xylan enzymolysis liquid is subjected to ultrafiltration membrance filter, the molecular cut off of milipore filter is 1000~1500Da, 0.5~0.7MPa is pressed before milipore filter, 0.3~0.5MPa is pressed after film, respectively obtains xylo-oligosaccharide raw sugar liquid 1, and zytase 2, the macromolecular oligo sugar mixed liquor of recovery, zytase 2 and mixed liquor are squeezed into saccharifying tank, while add new zytase, the zytase recycling of recovery, macromolecular oligo sugar repeats saccharification, enzymolysis, prepares xylo-oligosaccharide raw sugar liquid 2 and the zytase 3 of recovery；Merge obtained xylo-oligosaccharide raw sugar liquid, refine, obtain xylo-oligosaccharide syrup；Through vacuum belt concentration or scraper evaporator concentration, pure xylo-oligosaccharide powder is obtained.Present invention reduces production cost, improve raw material utilization efficiency, improve product quality, there are good market prospects.
Description
Technical field
The present invention relates to a kind of preparation method of pure xylo-oligosaccharide powder, belong to technical field of functional sugar alcohol production.
Background technology
Xylo-oligosaccharide is one kind of oligosaccharide, is using xylan as substrate, hydrolysis β-Isosorbide-5-Nitrae by β-Isosorbide-5-Nitrae-endo-xylanase
The degree of polymerization that glycosidic bond is formed is 2-7 oligosaccharide.Xylo-oligosaccharide, which can improve organism (humans and animals) archenteric flora, puts down
Weighing apparatus, promote the growth of alimentary canal beneficial bacteria, suppress harmful microbe breeding, promote nutrient absorption, improve immunity of organisms.
One kind is described in the preparation method (patent No. ZL 200410023875.X) for the patent xylo-oligosaccharide announced
Hemicellulose in corncob is converted into xylan and the therefrom method of purifying oligo-xylose, but this method shortcoming exists
In：Zytase is not merely with just by enzyme-deactivating, being recycled, the utilization rate of enzyme is very low, zytase valency after once
Lattice are expensive, cause product cost higher；In xylo-oligosaccharide concentration process, concentrated, high temperature concentration time length, made using conventional vacuum
It is deep into product color, in powder preparing processes (such as content 20%~70%) must add a certain amount of excipient such as dextrin,
Starch etc., is then spray-dried, and due to excipient be present, is caused the reduction of xylo-oligosaccharide powder solubility property, is mingled with other
The problems such as smell and influence its using effect and scope.
One kind is described in patent " a kind of method of producing low polyxylose with dual-aqueous phase hydrolyzation system " (CN101294175B)
Zytase repeats the method that recycling prepares xylo-oligosaccharide, is integrated in this method by two-phase separation system and prepares oligomeric wood
Sugar, enzymolysis liquid are stood in distributing trough, and zytase is distributed in phase polyethylene glycol system, and phase system realizes that wood is poly- in recovery
The recycling of carbohydrase, xylo-oligosaccharide are distributed in lower phase ammonium sulphate system, are reclaimed the oligosaccharide of residual by milipore filter and are gathered
Ethylene glycol reuses, and the method has the following disadvantages：1) fusing point of polyethylene glycol is 64 DEG C~66 DEG C, and existing zytase is most
Suitable hydrolysis temperature is 50 DEG C~60 DEG C, and therefore, at a temperature of peak enzymolysis-ability, polyethylene glycol may be so that solid state is present and influences
Use；2) there is harmfulness in the ammonium sulfate added in diphasic system, be not suitable for making as food additives to health
In xylooligosaccharides production, meanwhile, ammonium sulfate adds the pressure that subsequent ion exchanges process desalination.
In patent " a kind of preparation method of rice husk xylo-oligosaccharides " (CN101381753B), xylo-oligosaccharide prepared by rice husk is sugared
Liquid directly prepares xylo-oligosaccharide finished product using conventional vacuum drying mode, and it is free of excipient, but in this method, liquid glucose 40~
At 60 DEG C, the vacuum concentration time is 15~20h, and xylo-oligosaccharide liquid glucose can cause color and luster to deepen under long-time high temperature, and should
Method can not obtain high-purity xylo-oligosaccharide powder.
The content of the invention
For above-mentioned prior art, it is an object of the invention to provide a kind of preparation method of pure xylo-oligosaccharide powder, using steaming
Zytase is continuously reclaimed in the broken pretreatment of steam explosion, milipore filter and macromolecular oligo sugar repetition enzymolysis, the refined of enzymolysis liquid, liquid glucose are fast
Fast efficient concentration, cooling, crush etc. technique prepare without excipient high-purity xylo-oligosaccharide powder, solve xylo-oligosaccharide powder by
Solubility property caused by addition in excipient reduces, adulterates product color caused by other smells and the concentration of long-time high temperature
The problems such as pool is deepened.
To achieve the above object, the present invention uses following technical proposals：
A kind of preparation method of pure xylo-oligosaccharide powder, comprises the following steps：
(1) pH value for adjusting the xylan aqueous solution is 3.0-6.0, adds zytase and is digested, and is obtained poly- containing wood
The xylan enzymolysis liquid of carbohydrase；
(2) the xylan enzymolysis liquid of step (1) is subjected to ultrafiltration membrance filter, the molecular cut off of milipore filter for 1000~
1500Da, 0.5~0.7MPa is pressed before milipore filter, 0.3~0.5MPa is pressed after film, respectively obtains xylo-oligosaccharide raw sugar liquid 1, and return
The mixed liquor of zytase 2 and the macromolecular oligo sugar of receipts, the mixed liquor of zytase 2 and macromolecular oligo sugar is squeezed into saccharification
Tank, while new zytase is added, the zytase recycling of recovery, macromolecular oligo sugar repeats saccharification, enzymolysis, prepared low
Xylan raw sugar liquid 2 and the zytase 3 of recovery, such zytase are reused；
(3) the xylo-oligosaccharide raw sugar liquid obtained in combining step (2), and refined, obtain xylo-oligosaccharide syrup；
(4) the xylo-oligosaccharide syrup of step (3) is concentrated through vacuum belt or scraper evaporator concentrates, by cooling, powder
It is broken to obtain high-purity xylo-oligosaccharide powder.
In step (1), the preparation method of the xylan aqueous solution is：Locate in advance by solvent using maize cob meal as raw material
Reason, separation of solid and liquid remove the pretreated water solution containing pigment, and filter residue and the process water of acquisition are made into solid-to-liquid ratio as 1:2-6(g/
ML liquid to be blasted), in pressure 1.5-2.5MPa, processing time 120s-240s, diluted acid catalyst explosion liquid gross mass is accounted for
Under the conditions of 0.1%-1.5%, continuous steam explosion treatment is carried out, separation of solid and liquid, collects the aqueous solution rich in xylan.
The mass concentration of the xylan aqueous solution of preparation is 1%-8%.
The diluted acid catalyst is sulfuric acid, acetic acid, formic acid, citric acid.
The addition of zytase is：The zytase of 30-50UI units activities in every gram of xylan；Preferably 40UI.
New zytase addition is in step (2)：The zytase of 5-20UI units activities in every gram of xylan；It is preferred that
For 10UI.
In step (3), the process for purification of xylo-oligosaccharide raw sugar liquid includes activated carbon decolorizing and ion exchange resin cleans.
In step (4), vacuum belt concentration parameter is that vacuum is -80~-120KPa, one section of heating-up temperature 95~130
DEG C, two sections of 95~130 DEG C of heating-up temperatures, three sections of heating-up temperatures are 60~90 DEG C, and chilling temperature is 20~40 DEG C；Scraper plate evaporation is dense
Contracting parameter be temperature control at 115 DEG C~130 DEG C, evaporating pressure be -0.08~-0.098MPa, and drop temperature control is at 105 DEG C
~120 DEG C, for the control of scraper plate rotating speed in 3~5m/s, chilling temperature is 20~40 DEG C.
Beneficial effects of the present invention：
(1) zytase of the invention can be realized by milipore filter and recycled and reused, and reduce the life of xylo-oligosaccharide
Cost is produced, the macromolecular glycan after enzymolysis in enzymolysis liquid can repeat enzymolysis and prepare xylo-oligosaccharide after ultrafiltration membrance filter, improve
The utilization ratio of raw material.
(2) syrup of the invention prepares xylo-oligosaccharide powder by rapidly and efficiently concentration, dry, cooling, crushing, due to keeping away
Exempt from that high temperature concentration time is long, the addition of excipient (dextrin etc.), obtained the water solubility of product, smell, color and luster etc. obvious
Improve.
(3) present invention reduces production cost, improve raw material utilization efficiency, improve product quality, have good
Market prospects.
Brief description of the drawings
Fig. 1 is process chart prepared by pure xylo-oligosaccharide powder.
Embodiment
Below by instantiation, the present invention will be further elaborated, it should explanation, the description below be only for
The present invention is explained, its content is not defined.
Embodiment 1：
1) corn core raw material removes the pretreated water solution containing pigment, obtained by crushing, hot-water pretreatment, separation of solid and liquid
The filter residue obtained is made into solid-to-liquid ratio as 1 with process water:2 liquid to be blasted, urged in pressure 1.5MPa, processing time 220s, diluted acid
Agent is accounted under the conditions of explosion liquid gross mass 0.8%, is carried out continuous steam explosion treatment, separation of solid and liquid, is collected rich in xylan
The aqueous solution；
2) pH value for adjusting the xylan aqueous solution is 6.0, and 40UI is added according to every gram of xylan in the aqueous solution of xylan
The ratio of units activity adds zytase, and enzyme hydrolysis temperature is 50 DEG C, and the enzymatic hydrolysis reaction time is 7.0h, obtains xylo-oligosaccharide
Enzymolysis liquid；
3) enzymolysis liquid carries out ultrafiltration membrance filter, and the molecular cut off of milipore filter is 1200Da, and 0.5MPa, film are pressed before milipore filter
After press 0.3MPa, reclaim zytase and macromolecular oligo sugar, squeeze into saccharifying tank, zytase recycling, macromolecular oligo
The repeated saccharification enzymolysis of sugar；
4) filtered solution is 80 DEG C through activated carbon decolorizing, activated carbon decolorizing temperature, and activated carbon addition accounts for the hundred of liquid glucose weight
It is 0.4%, bleaching time 30min to divide ratio, is cleaned by ion exchange, flow velocity 9m3/h；
5) xylo-oligosaccharide syrup is dried is concentrated by evaporation by scraper evaporator, and scraper plate evaporation drying parameter is that temperature control exists
115 DEG C, evaporating pressure is -0.085MPa, and drop temperature is controlled at 105 DEG C, and scraper plate rotating speed controls is in 3.5m/s chilling temperatures
25 DEG C, crushing prepares pure xylo-oligosaccharide powder.
Embodiment 2：
1) corn core raw material removes the pretreated water solution containing pigment, obtained by crushing, hot-water pretreatment, separation of solid and liquid
The filter residue obtained is made into solid-to-liquid ratio as 1 with process water:4 liquid to be blasted, urged in pressure 1.8MPa, processing time 200s, diluted acid
Agent is accounted under the conditions of explosion liquid gross mass 0.6%, is carried out continuous steam explosion treatment, separation of solid and liquid, is collected rich in xylan
The aqueous solution；
2) pH value for adjusting the xylan aqueous solution is 4.0, and ultrafiltration in embodiment 1 is added in the aqueous solution of xylan and is reclaimed
Zytase recycling, while by the new zytase of ratio addition of every gram of xylan 10UI units activity, enzyme hydrolysis temperature
Spend for 45 DEG C, the enzymatic hydrolysis reaction time is 8.0h, obtains xylo-oligosaccharide enzymolysis liquid；
3) enzymolysis liquid carries out ultrafiltration membrance filter, and the molecular cut off of milipore filter is 1200Da, and 0.65MPa is pressed before milipore filter,
0.45MPa is pressed after film, zytase and macromolecular oligo sugar is reclaimed, squeezes into saccharifying tank, zytase reuses, and macromolecular is low
The repeated saccharification enzymolysis of glycan；
4) filtered solution is 70 DEG C through activated carbon decolorizing, activated carbon decolorizing temperature, and activated carbon addition accounts for the hundred of liquid glucose weight
It is 0.6%, bleaching time 50min to divide ratio, is cleaned by ion exchange, flow velocity 12m3/h；
5) xylo-oligosaccharide syrup is dried by vacuum belt concentration, and vacuum is -90KPa, one section of 115 DEG C of heating-up temperature,
Two sections of 105 DEG C of heating-up temperatures, three sections of heating-up temperatures are 85 DEG C, and chilling temperature is 30 DEG C, crushes to obtain pure xylo-oligosaccharide powder；
Embodiment 3：
1) corn core raw material removes the pretreated water solution containing pigment, obtained by crushing, hot-water pretreatment, separation of solid and liquid
The filter residue obtained is made into solid-to-liquid ratio as 1 with process water:6 liquid to be blasted, urged in pressure 2.0MPa, processing time 150s, diluted acid
Agent is accounted under the conditions of explosion liquid gross mass 0.2%, is carried out continuous steam explosion treatment, separation of solid and liquid, is collected rich in xylan
The aqueous solution；
2) pH value for adjusting the xylan aqueous solution is 5.0, and ultrafiltration recovery wood in embodiment 2 is added in the aqueous solution of xylan
Dextranase reuses, while adds new zytase in the ratio of every gram of xylan 8UI units activity, and enzyme hydrolysis temperature is 55
DEG C, the enzymatic hydrolysis reaction time is 5.5h, obtains xylo-oligosaccharide enzymolysis liquid；
3) enzymolysis liquid carries out ultrafiltration membrance filter, and the molecular cut off of milipore filter is 1200Da, and 0.7MPa, film are pressed before milipore filter
After press 0.5MPa, reclaim zytase and macromolecular oligo sugar, squeeze into saccharifying tank, zytase recycling, macromolecular oligo
The repeated saccharification enzymolysis of sugar；
4) filtered solution is 90 DEG C through activated carbon decolorizing, activated carbon decolorizing temperature, and activated carbon addition accounts for the hundred of liquid glucose weight
It is 0.2%, bleaching time 20min to divide ratio, is cleaned by ion exchange, flow velocity 7m3/h；
5) xylo-oligosaccharide syrup, which is dried, passes through vacuum belt type drying, and vacuum is -110KPa, one section of 105 DEG C of heating-up temperature,
Two sections of 95 DEG C of heating-up temperatures, three sections of heating-up temperatures are 75 DEG C, and chilling temperature is 25 DEG C, crushes to obtain pure xylo-oligosaccharide powder.
Pure xylo-oligosaccharide powder prepared by embodiment 1~3 carries out compound mensuration, as described in Table 1：
Table 1:The xylo-oligosaccharide product component situation (weight/mass percentage composition) of embodiment 1~3
| Project | Xylobiose | Xylotriose | Xylotetrose | The wooden sugar of pentasaccharides~wood seven | Xylo-oligosaccharide content amounts to |
| Embodiment 1 | 31.32% | 20.12% | 11.06% | 14.05% | 76.55% |
| Embodiment 2 | 31.45% | 19.98% | 11.34% | 13.87% | 76.64% |
| Embodiment 3 | 31.21% | 20.04% | 11.28% | 13.99% | 76.52% |
As shown in Table 1：Zytase is reclaimed by milipore filter to reuse, and does not interfere with xylo-oligosaccharide product component.
Table 2:Embodiment 1~3 is compared with terms of traditional handicraft xylo-oligosaccharide powder solubility property, mobility, smell
| Project | Solubility property | Mobility | Smell |
| The xylo-oligosaccharide powder of embodiment 1 | 5.2s | 3.9s | Without other smells |
| The xylo-oligosaccharide powder of embodiment 2 | 5.5s | 3.7s | Without other smells |
| The xylo-oligosaccharide powder of embodiment 3 | 5.6s | 3.8s | Without other smells |
| Traditional handicraft xylo-oligosaccharide powder | 9.6s | 5s | It is mingled with dextrin smell |
Found out by table 2：Syrup through convection drying, cooling, crush xylo-oligosaccharide powder compared with Icing Sugar is made in traditional handicraft,
Solubility property, mobility, smell etc. be improved significantly, there is good beneficial effect.
The embodiment 1-3 of table 3 with traditional handicraft often prepare 1 ton of xylo-oligosaccharide powder used in zytase cost compared with
As shown in Table 3：The average unit cost of zytase used in embodiment 1-3 xylo-oligosaccharide powders per ton in 300 or so members, and
Traditional handicraft zytase cost is at 900 yuan or so, and by being recycled to zytase, can reach reduces xylo-oligosaccharide production
The effect of product cost.
Claims (6)
1. a kind of preparation method of pure xylo-oligosaccharide powder, it is characterised in that comprise the following steps：
(1) the pH values for adjusting the xylan aqueous solution are 3.0-6.0, add zytase and are digested, are obtained containing xylan
The xylan enzymolysis liquid of enzyme；
(2) the xylan enzymolysis liquid of step (1) is subjected to ultrafiltration membrance filter, the molecular cut off of milipore filter for 1000~
1500Da, 0.5~0.7MPa is pressed before milipore filter, 0.3~0.5MPa is pressed after film, respectively obtains xylo-oligosaccharide raw sugar liquid 1, with
And the mixed liquor of zytase 2 and the macromolecular oligo sugar of recovery, the mixed liquor of zytase 2 and macromolecular oligo sugar is beaten
Entering saccharifying tank, while add new zytase, the zytase recycling of recovery, macromolecular oligo sugar repeats saccharification, enzymolysis,
Prepare xylo-oligosaccharide raw sugar liquid 2 and the zytase 3 of recovery, such zytase are reused；
(3) the xylo-oligosaccharide raw sugar liquid obtained in combining step (2), and refined, obtain xylo-oligosaccharide syrup；
(4) the xylo-oligosaccharide syrup of step (3) is concentrated through vacuum belt or scraper evaporator concentrates, by cooling, crushed
Obtain pure xylo-oligosaccharide powder；
In step (1), the preparation method of the xylan aqueous solution is：Pass through solvent pre-treatment by raw material of maize cob meal, Gu
Liquid, which separates, removes the pretreated water solution containing pigment, and filter residue and the process water of acquisition are made into solid-to-liquid ratio as 1:2-6's is to be blasted
Liquid, under the conditions of pressure 1.5-2.5MPa, processing time 120s-240s, diluted acid catalyst 0.1% -1.5%, carry out continuous
Steam explosion treatment, separation of solid and liquid, collect the aqueous solution rich in xylan；
In step (4), vacuum belt concentration parameter is that vacuum is -80~-120KPa, one section of heating-up temperature 95~130
DEG C, two sections of 95~130 DEG C of heating-up temperatures, three sections of heating-up temperatures are 60~90 DEG C, and chilling temperature is 20~40 DEG C；
In step (4), scraper plate be concentrated by evaporation parameter be temperature control at 115 DEG C~130 DEG C, evaporating pressure is -0.08~-
0.098MPa, drop temperature control at 105 DEG C~120 DEG C, the control of scraper plate rotating speed in 3~5m/s, chilling temperature is 20~
40℃。
2. the preparation method of pure xylo-oligosaccharide powder according to claim 1, it is characterised in that in step (1), preparation
The mass concentration of the xylan aqueous solution is 1% -8%.
3. the preparation method of pure xylo-oligosaccharide powder according to claim 1, it is characterised in that described dilute in step (1)
Acid catalyst is sulfuric acid, acetic acid, formic acid, citric acid.
4. the preparation method of the pure xylo-oligosaccharide powder according to claim 1, it is characterised in that in step (1), wood is poly-
The addition of carbohydrase is：The zytase of 30-50UI units activities in every gram of xylan.
5. the preparation method of the pure xylo-oligosaccharide powder according to claim 1, it is characterised in that in step (2), new wood
Dextranase addition is：The zytase of 5-20UI units activities in every gram of xylan.
6. the preparation method of the pure xylo-oligosaccharide powder according to claim 1, it is characterised in that oligomeric in step (3)
The process for purification of xylose raw sugar liquid includes activated carbon decolorizing and ion exchange resin cleans.
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| CN112458133B (en) * | 2020-10-30 | 2023-01-10 | 济南茂腾生物科技有限公司 | Method for preparing xylo-oligosaccharide from corn bran |
| CN112458125B (en) * | 2020-10-30 | 2022-08-26 | 济南茂腾生物科技有限公司 | Method for preparing xylo-oligosaccharide from corncob powder |
| CN112481331B (en) * | 2020-10-30 | 2022-07-08 | 济南茂腾生物科技有限公司 | Method for preparing xylooligosaccharide from hemicellulose |
| CN113261678A (en) * | 2021-04-15 | 2021-08-17 | 山东卫康生物医药科技有限公司 | Preparation process of natto xylooligosaccharide powder suitable for people with low immunity |
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| CN114457059B (en) * | 2022-01-21 | 2024-03-19 | 青岛尚德生物技术有限公司 | Xylanase-containing enzyme preparation and application thereof in production of xylooligosaccharide |
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