CN103333932A - A method for preparing xylooligosaccharide - Google Patents
A method for preparing xylooligosaccharide Download PDFInfo
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- CN103333932A CN103333932A CN2012105900924A CN201210590092A CN103333932A CN 103333932 A CN103333932 A CN 103333932A CN 2012105900924 A CN2012105900924 A CN 2012105900924A CN 201210590092 A CN201210590092 A CN 201210590092A CN 103333932 A CN103333932 A CN 103333932A
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- xylo
- oligosaccharide
- corn cob
- corncobs
- zytase
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Abstract
The invention relates to a method for preparing xylooligosaccharide. According to the method provided by the invention, corncobs are immersed in a dilute alkali solution, then the immersed corncobs are washed with water and degraded with xylanase, and then the xylooligosaccharide is prepared by existing preparation steps of the xylooligosaccharide. According to the method, the corncobs are immersed in the dilute alkali solution, and therefore the method has an advantage of reduced alkali usage over traditional technologies. In addition, after the corncobs are immersed, redundant alkali solution can be squeezed out and directly recycled and reutilized. Traditional alkali treatment technologies usually extract xylan from corncob powder by using a concentrated alkali solution, while the method provided by the invention uses the dilute alkali solution to immerse the corncobs and the xylan is still remained in the solid. The immersed corncobs before enzymatic degradation are washed with water, thereby reducing cost of follow-up decolorization and impurity removal, and preventing xylan loss.
Description
Technical field
The present invention relates to biological chemical field, is specifically related to a kind of method for preparing xylo-oligosaccharide from lignocellulose.
Background technology
Xylo-oligosaccharide also claims wood oligose, be a kind of important function food, it promotes the breeding of probiotics in the enteron aisle in addition except having low-heat, good physicochemical property such as stable, safe, nontoxic, suppress unique physiological function of harmful bacteria growing, now caused global extensive concern.The method that prepare at present xylo-oligosaccharide is a lot, and its raw material mainly is to be the feedstock production xylo-oligosaccharide with the corn cob, and dense corn cob core is big, and output is many, easily collection.Other raw materials also comprise Pericarppium arachidis hypogaeae, bagasse, and cotton seed hulls, rice husk etc. are rich in the lignocellulose of xylan.Before with zytase these raw materials being hydrolyzed, in order to improve its productive rate, often to carry out certain pre-treatment to raw material, stripping xylan or make the hemicellulose short texture is conducive to the contact of enzyme.Its pretreatment process can be divided into two big classes, and the first kind is to go out xylan with the high alkali liquid extracting, filter then and in and alkali lye, enzymic hydrolysis obtains the xylo-oligosaccharide liquid glucose.Another kind method be with dilution high temperature stripping xylan then enzymic hydrolysis obtain xylo-oligosaccharide.Patent disclosure is arranged the weak acid pyroprocessing prepare the method for xylo-oligosaccharide, only make raw material with corn cob meal, adopt the weak acid catalyzer to carry out cracking, the stripping xylo-oligosaccharide, control pH value, carry out enzymolysis with zytase, the high temperature enzyme that goes out, filter residue, by gac and ion-exchanger decolouring removal of impurities, hold back the macromole xylan with the macromole mwco membrane, sodium filter membrane concentrating and desalinating and vacuum concentration, spraying drying obtains xylo-oligosaccharide, this method adopts corn cob meal as raw material, solid-to-liquid ratio is at 1:6-10, temperature is about the 155-180 degree, pretreatment time is about 30-120min, this method liquid-solid ratio is big as can be seen, the temperature height, the equipment requirements height, investment is big, and the energy consumption of its treating processes is therefore very big; Also have in much the alkaline process of the xylo-oligosaccharide of bibliographical informations prepares, usually use the alkaline solution of 10-15% concentration, solid-to-liquid ratio is at 1:10-20, xylan in the lignocellulose is carried out the stripping extracting, neutralize alkali then, again the xylan that extracts is carried out enzymic hydrolysis and obtain xylo-oligosaccharide, the consumption of alkali is also more than the quality of raw material self, has consumed a large amount of chemical; Have report to adopt microwave method that the particulate state corn cob is carried out micro-wave digestion, follow-uply carry out enzymolysis to clearing up residue again, the enzyme that goes out, separation, collection obtain xylo-oligosaccharide, yet microwave also has a segment distance in industrial application.Aforesaid method exists more or less that to consume chemical many, the energy consumption height, and problem such as sewage is many is unfavorable for the Sustainable development of environment.
Summary of the invention
The present invention provides a kind of method for preparing xylo-oligosaccharide from corn cob for overcoming the deficiencies in the prior art, and cost is low, and energy consumption is low, and facility investment is low, can be suitable for the large-scale production of corn cob xylo-oligosaccharide.
The applicant finds that in long term studies with traditional comparing with high alkali liquid extracting xylan, with sig water soaking corn core, the corn cob after will soaking then enzymolysis again prepares xylo-oligosaccharide, can significantly reduce the amount of cost and waste liquid, thereby facilitate the present invention.
Preparation method of the present invention is with sig water soaking corn core, and after the corn cob washing after will soaking again, with the zytase degraded, the preparation process by existing xylo-oligosaccharide obtains xylo-oligosaccharide again.
The preparation process of described existing xylo-oligosaccharide refers to filtration, decolouring, desalination step behind the enzymolysis.
The preparation process of above-mentioned existing xylo-oligosaccharide also includes concentrated step after the desalination step.
The inventive method, its a kind of concrete steps are as follows:
(1) the corn cob sig water immersion treatment after will pulverizing;
(2) extrude alkali lye, the corn cob after washing is soaked;
(3) with the corn cob wet-milling or be ground into pasty state;
(4) the pH value of adjusting mashed prod adds zytase, carries out enzymolysis;
(5) the gained mixture namely obtains thick xylo-oligosaccharide liquid after filtration behind the enzymolysis.
(6) xylo-oligosaccharide liquid is through decolouring, and desalination concentrates and obtains the xylo-oligosaccharide finished product.
Wherein the middle sig water of step (1) is 3～10:1 with the volume mass of corn cob than (ml/g), is preferably 3～6:1.
The mass volume ratio of used alkali lye in the step 1) (g/ml) concentration is 1～1.5%, preferred 1.2%.
The temperature of dipping by lye corn cob is 0～100 ℃ in the above-mentioned steps (1), preferred 0-40 ℃.
The treatment time of dipping by lye corn cob is 30min～48h in the above-mentioned steps (1), preferred 30min-24h.
The addition of zytase is 300-1500U/ gram corn cob raw material dry weight in the above-mentioned steps (4).
The enzymatic hydrolysis condition of zytase is 45-55 ℃ in the above-mentioned steps (4), and enzymolysis time is 6-72h.
The present invention adopts sig water soaking corn core, compares with traditional technology, and alkali charge reduces greatly; In addition, after the immersion, can also extrude unnecessary alkali lye, directly recycle.The tradition alkali pretreatment normally goes out xylan with high alkali liquid extracting from corn cob meal, and the present invention is to use sig water soaking corn core, xylan still is retained in the solid, corn cob after washing is soaked earlier before enzymolysis, can reduce the cost of follow-up decolouring removal of impurities, and can not cause the loss of xylan.After corn-cob structure is soft by the sig water immersion, carry out wet-grinding technology and relative device again, can further discongest hemicellulose, increase the contact probability of hemicellulose and enzyme, accelerate hydrolysis rate, thereby improve the yield of xylo-oligosaccharide.The present invention is simple for process, and treatment temp is low, and alkali charge is few, and equipment requirements is low, and xylo-oligosaccharide yield height is convenient to large-scale production.
Figure of description:
Fig. 1: the present invention prepares the process route chart of xylo-oligosaccharide.
Embodiment
Employed raw material and equipment can be selected arbitrary product on the market for use among the present invention.For example zytase is optional available from Qingdao Weilan Biology Group Co., Ltd., enzyme 200000 U/g alive.
The present invention is with sig water soaking corn core, after the corn cob washing after will soaking again, obtain thick xylo-oligosaccharide liquid with the zytase degraded, for the follow-up step of thick xylo-oligosaccharide liquid, can carry out with reference to existing method for preparing lower polyxylose, and be not limited to the record of the specific embodiment of the invention.Those of ordinary skill in the art can select the preparation process behind the enzymolysis under technical thought of the present invention.
Embodiment 1
The corn plug is ground into diameter less than the particle of 0.5cm; Take by weighing the corn cob granule of five parts of each heavy 10g, add mass volume ratio respectively and be 0.5%, 1%, 1.5%, 2% and 5% sodium hydroxide solution 60ml, 20 ℃ were soaked 24 hours; Extrude alkali lye (can reuse), the mixture that washing obtains; The mixture wet-milling is become pasty state; Regulate pH to 4.5-6.0, add the 15mg zytase, 50 ℃ of enzymolysis 24 hours, 100 ℃ of deactivation 10min, filter, get thick xylo-oligosaccharide liquid, with the content of high-performance liquid chromatogram determination xylo-oligosaccharide, as calculated, the yield of xylo-oligosaccharide is respectively 7%, 45%, 48%, 44% and 40%.Xylo-oligosaccharide liquid is through decolouring, and desalination concentrates, and namely obtains the xylo-oligosaccharide finished product.
Above-mentioned experimental result shows, behind the sodium hydroxide solution soaking corn core of 1-1.5%, the yield of xylo-oligosaccharide far above 0.5% soaking with sodium hydroxide after the yield of xylo-oligosaccharide, and the yield than xylo-oligosaccharide after the soaking with sodium hydroxide of 2-5% is higher, so the present invention adopts the sig water soaking corn core of 1-1.5% to prepare xylo-oligosaccharide and obtained unexpected effect, can effectively reduce the consumption of alkali lye, reduce the corrosion to equipment, reduce production costs, reduce environmental pollution.
Embodiment 2
The corn plug is ground into diameter less than the corn cob granule of 0.5cm; Take by weighing the 10g corn cob granule, the adding mass volume ratio is 1.5% sodium hydroxide solution 60ml, and 20 ℃ were soaked 24 hours; Extrude alkali lye (can reuse), the mixture that washing obtains; The mixture wet-milling is become pasty state; Regulate pH to 4.5-6.0, add the 15mg zytase, 50 ℃ of enzymolysis 24 hours boil inactivator, filter, and get thick xylo-oligosaccharide liquid, and with the content of high-performance liquid chromatogram determination xylo-oligosaccharide, as calculated, the yield of xylo-oligosaccharide is 48%.Xylo-oligosaccharide liquid is through decolouring, and desalination concentrates, and namely obtains the xylo-oligosaccharide finished product.
Control experiment: operation steps is the same, and unique difference is that the mixture after the washing directly carries out follow-up enzymolysis without wet-milling, and the yield of final xylo-oligosaccharide only is 37%.
Above-mentioned experimental result shows, after the corn cob process wet-milling operation after diluted alkaline soaks, can further discongest hemicellulose, increases the contact probability of hemicellulose and enzyme, accelerates hydrolysis rate, thereby can significantly improve the yield of xylo-oligosaccharide.
Embodiment 3
The corn plug is ground into diameter less than the corn cob granule of 0.5cm; Take by weighing the 10g corn cob granule, the adding mass volume ratio is 1.5% sodium hydroxide solution 30ml, and 20 ℃ were soaked 24 hours; Extrude alkali lye (can reuse), the mixture that washing obtains; The mixture wet-milling is become pasty state; Regulate pH to 4.5-6.0, add the 15mg zytase, 50 ℃ of enzymolysis 24 hours boil inactivator, filter, and get thick xylo-oligosaccharide liquid, and with the content of high-performance liquid chromatogram determination xylo-oligosaccharide, as calculated, the yield of xylo-oligosaccharide is 45%.Xylo-oligosaccharide liquid is through decolouring, and desalination concentrates, and namely obtains the xylo-oligosaccharide finished product.
Embodiment 4
The corn plug is ground into diameter less than the corn cob granule of 0.5cm; Take by weighing the 10g corn cob granule, the adding mass volume ratio is 1.5% sodium hydroxide solution 60ml, and 20 ℃ were soaked 24 hours; Extrude alkali lye (can reuse), the mixture that washing obtains; The mixture wet-milling is become pasty state; Regulate pH to 4.5-6.0, add the 75mg zytase, 55 ℃ of enzymolysis 72 hours boil inactivator, filter, and get thick xylo-oligosaccharide liquid, and with the content of high-performance liquid chromatogram determination xylo-oligosaccharide, as calculated, the yield of xylo-oligosaccharide is 76%.Xylo-oligosaccharide liquid is through decolouring, and desalination concentrates, and namely obtains the xylo-oligosaccharide finished product.
Embodiment 5
The corn plug is ground into diameter less than the corn cob granule of 0.5cm; Take by weighing the 10g corn cob granule, the adding mass volume ratio is 1.5% sodium hydroxide solution 100ml, and 0 ℃ was soaked 48 hours; Extrude alkali lye (can reuse), the mixture that washing obtains; The mixture wet-milling is become pasty state; Regulate pH to 4.5-6.0, add the 15mg zytase, 50 ℃ of enzymolysis 24 hours boil inactivator, filter, and get thick xylo-oligosaccharide liquid, and with the content of high-performance liquid chromatogram determination xylo-oligosaccharide, as calculated, the yield of xylo-oligosaccharide is 59%.Xylo-oligosaccharide liquid is through decolouring, and desalination concentrates, and namely obtains the xylo-oligosaccharide finished product.
Embodiment 6
The corn plug is ground into diameter less than the corn cob granule of 0.5cm; Take by weighing the 10g corn cob granule, the adding mass volume ratio is 1.5% sodium hydroxide solution 60ml, and 25 ℃ were soaked 24 hours; Extrude alkali lye (can reuse), the mixture that washing obtains is regulated pH to 4.5-6.0, add the 60mg zytase, 45 ℃ of enzymolysis 72 hours boil inactivator, filter, get thick xylo-oligosaccharide liquid, with the content of high-performance liquid chromatogram determination xylo-oligosaccharide, as calculated, the yield of xylo-oligosaccharide is 68%.Xylo-oligosaccharide liquid is through decolouring, and desalination concentrates, and namely obtains the xylo-oligosaccharide finished product.
Embodiment 7
The corn plug is ground into diameter less than the corn cob granule of 0.5cm; Take by weighing the 10g corn cob granule, the adding mass volume ratio is 1.5% sodium hydroxide solution 60ml, 100 ℃ of boiling 30min; Extrude alkali lye (can reuse), the mixture that washing obtains; The mixture wet-milling is become pasty state; Regulate pH to 4.5-6.0, add the 75mg zytase, 50 ℃ of enzymolysis 6 hours boil inactivator, filter, and get thick xylo-oligosaccharide liquid, and with the content of high-performance liquid chromatogram determination xylo-oligosaccharide, as calculated, the yield of xylo-oligosaccharide is 37%.Xylo-oligosaccharide liquid is through decolouring, and desalination concentrates, and namely obtains the xylo-oligosaccharide finished product.
Method of the present invention has significantly reduced cost and the generation of waste of preparation under the situation of the yield that does not reduce xylo-oligosaccharide, have good application and popularization value.
Claims (10)
1. a method for preparing xylo-oligosaccharide is characterized in that, described method is with sig water soaking corn core, and after the corn cob washing after soaking, with the zytase degraded, the preparation process by existing xylo-oligosaccharide obtains xylo-oligosaccharide again.
2. the method for claim 1 is characterized in that, the preparation process of described existing xylo-oligosaccharide refers to filtration, decolouring, desalination, enrichment step behind the enzymolysis.
3. claim 1 or 2 described methods, its concrete steps are as follows:
(1) the corn cob sig water immersion treatment after will pulverizing;
(2) extrude alkali lye, the corn cob after washing is soaked;
(3) with the corn cob wet-milling or be ground into pasty state;
(4) the pH value of adjusting mashed prod adds zytase, carries out enzymolysis;
(5) the gained mixture namely obtains thick xylo-oligosaccharide liquid after filtration behind the enzymolysis.
(6) xylo-oligosaccharide liquid is through decolouring, and desalination concentrates and obtains the xylo-oligosaccharide finished product.
4. as claim 1 or 3 described methods, it is characterized in that described sig water and the volume mass ratio of corn cob are 3～10:1.
5. method as claimed in claim 3 is characterized in that described sig water and the volume mass ratio of corn cob are 3～6:1.
6. as claim 1 or 3 described methods, the mass volume ratio concentration that it is characterized in that described sig water is 1～1.5%.
7. method as claimed in claim 3 is characterized in that the temperature of dipping by lye corn cob in the described step (1) is 0-100 ℃.
8. method as claimed in claim 3 is characterized in that the treatment time of dipping by lye corn cob in the described step (1) is 30min-48h.
9. method as claimed in claim 3, the addition that it is characterized in that zytase in the described step (4) are 300-1500U/ gram corn cob raw material dry weight.
10. method as claimed in claim 3 is characterized in that the hydrolysis temperature of zytase in the described step (4) is 45-55 ℃, and enzymolysis time is 6-72h.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104087634A (en) * | 2014-07-11 | 2014-10-08 | 清华大学 | Method for preparing xylooligosaccharide by using sorgo fermentation residue |
| CN105440165A (en) * | 2015-10-20 | 2016-03-30 | 石河子大学 | Method for extracting xylan from cottonseed hulls by microwave-assisted alkali liquor |
| CN106636254A (en) * | 2016-12-28 | 2017-05-10 | 山东龙力生物科技股份有限公司 | Process for preparing high-purity xylooligosaccharide |
| CN106636256A (en) * | 2016-12-28 | 2017-05-10 | 山东龙力生物科技股份有限公司 | Xylooligosaccharide with low DP (degree of polymerization) as well as preparation method and application of xylooligosaccharide |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101696427A (en) * | 2009-11-03 | 2010-04-21 | 天津科技大学 | Method for producing fuel ethanol and 2,3-butanediol by using fibrous matter |
| CN101914589A (en) * | 2010-08-06 | 2010-12-15 | 河南省科学院生物研究所有限责任公司 | New method for producing low polyxylose by utilizing microorganism |
-
2012
- 2012-12-29 CN CN2012105900924A patent/CN103333932A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101696427A (en) * | 2009-11-03 | 2010-04-21 | 天津科技大学 | Method for producing fuel ethanol and 2,3-butanediol by using fibrous matter |
| CN101914589A (en) * | 2010-08-06 | 2010-12-15 | 河南省科学院生物研究所有限责任公司 | New method for producing low polyxylose by utilizing microorganism |
Non-Patent Citations (1)
| Title |
|---|
| 王海等: "用玉米芯酶法制备低聚木糖", 《食品科学》, vol. 23, no. 5, 31 December 2002 (2002-12-31), pages 81 - 83 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104087634A (en) * | 2014-07-11 | 2014-10-08 | 清华大学 | Method for preparing xylooligosaccharide by using sorgo fermentation residue |
| CN104087634B (en) * | 2014-07-11 | 2018-02-27 | 清华大学 | A kind of method that xylo-oligosaccharide is prepared with sugar grass fermentation residue |
| CN105440165A (en) * | 2015-10-20 | 2016-03-30 | 石河子大学 | Method for extracting xylan from cottonseed hulls by microwave-assisted alkali liquor |
| CN106636254A (en) * | 2016-12-28 | 2017-05-10 | 山东龙力生物科技股份有限公司 | Process for preparing high-purity xylooligosaccharide |
| CN106636256A (en) * | 2016-12-28 | 2017-05-10 | 山东龙力生物科技股份有限公司 | Xylooligosaccharide with low DP (degree of polymerization) as well as preparation method and application of xylooligosaccharide |
| CN106636256B (en) * | 2016-12-28 | 2024-03-08 | 山东龙力生物科技股份有限公司 | Xylo-oligosaccharide with low polymerization degree and preparation method and application thereof |
| CN106636254B (en) * | 2016-12-28 | 2024-03-08 | 山东龙力生物科技股份有限公司 | Preparation process of high-purity xylo-oligosaccharide |
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Application publication date: 20131002 |