CN1186461C - Prepn of oligoxylose - Google Patents
Prepn of oligoxylose Download PDFInfo
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- CN1186461C CN1186461C CNB011311711A CN01131171A CN1186461C CN 1186461 C CN1186461 C CN 1186461C CN B011311711 A CNB011311711 A CN B011311711A CN 01131171 A CN01131171 A CN 01131171A CN 1186461 C CN1186461 C CN 1186461C
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Abstract
The present invention discloses a method for preparing oligo xylose, which belongs to the field of food processing. The present invention has the purpose that the present invention provides a method for achieving the industrial production that hemicellulose in a corn cob is converted into oligo xylose with high quality, and the present invention comprises the detailed proposal that a raw corn cob is pre-processed in a water solution of an alkali metal hydroxide, and the direct thermal cracking is carried out under the functions of weak acid type catalysts such as acetic acid, formic acid, citric acid, etc.; the corn cob can react with a xylanase solution after carrying out the direct thermal cracking, the trash extraction is carried out through active carbon decolorization and ion exchange resin, and then vacuum concentration is carried out; thereby, malto dextrin, etc. can be used as excipient. An oligo xylose powder agent is obtained through spray drying.
Description
The present invention relates to the hemicellulose in the corn cob is converted into the method for xylo-oligosaccharide, belong to food processing field.
Xylo-oligosaccharide also claims wood oligose (xylooligosaccharides), and with β-1,4-xyloside bond is closed and formed by 2～7 D-wood sugars, is an important member in the functional oligose family.Its sweetness ratio sucrose and glucose are all low, and is similar with maltose, is about 40% of sucrose.Xylo-oligosaccharide is better to the stability of pH value and heat, even also do not decompose substantially in acidic conditions (pH=2.5～7) heating, is suitable in the acidic drinks such as sour milk, lactobacillus drink and soda pop.Figure below is the main component and the chemical structure of xylo-oligosaccharide.
Xylo-bioses (is called for short X
2)
Xylotriose (is called for short X
3)
Survival rate height in the xylo-oligosaccharide absorption extremely difficult to digest, enteron aisle has fabulous bifidus bacillus proliferative, and it selects usability to be higher than other functional oligose.The physiological function of having studied at present the xylo-oligosaccharide of affirmation already mainly comprises: (1) provides lower energy, satisfies the requirement that happiness food sweets is worried the person of getting fat again, also can supply diabetics, adiposis patient and hypertensive patient edible; (2) bifidus bacillus and promote its propagation in the activation enteron aisle suppresses pathogenic bacteria, prevents diarrhoea; (3) prevent constipation; (4) reduce cholesterol in serum content, bring high blood pressure down, generate nutritive substance, enhancing body immunizing power and opposing tumour; (5) can not cause carious tooth, help oral Health; (6) remove enterogenous endotoxin.
Xylo-oligosaccharide generally is to be rich in the plant resources of xylan, is raw material as wood chip, corn cob, cotton seed hulls, rice husk and vegetable seed shell etc., after the internal cutting type xylanase hydrolysis, separates again, makes with extra care and make.China's corn cob aboundresources, but be not reported about the method for from corn cob, extracting xylo-oligosaccharide.
The objective of the invention is to provide a kind of method for preparing lower polyxylose of making raw material of corn cob.
In order to reach decolouring, removal of impurities that technical scheme that purpose of the present invention takes comprises the stripping, xylanase hydrolysis reaction and the xylo-oligosaccharide solution that adopt xylan in alkali hydroxide soln pre-treatment corn cob meal, washing, the corn cob meal, to concentrate and dry technology, wherein:
(1) alkali hydroxide soln that adopts of corn cob meal pre-treatment is solution such as potassium hydroxide, sodium hydroxide, during pre-treatment, the concentration of alkali hydroxide soln is 0.5%～1.5%, 30 ℃～60 ℃ of treatment temps, time 30min～120min, corn cob meal and alkali hydroxide soln weight ratio are 1: 8～1: 12;
(2) directly-heated boiling fragmentation pattern is adopted in the stripping of xylan in the corn cob meal, boiling temperature is 155 ℃～180 ℃, cooking time 30min～120min, the weight ratio of corn cob meal and water is 1: 6～1: 10, use weak-type catalyzer such as acetate, formic acid, citric acid etc. in the digestion process, addition is 0.2%～1.5% of a corn cob meal weight;
What (3) enzymatic hydrolysis reaction used is sp.E-86 type zytase liquid, 45 ℃～60 ℃ of enzymatic hydrolysis reaction temperature, enzymatic hydrolysis reaction time 4h～10h, zytase liquid is 1ml/1.2g～1ml/1.6g with the ratio of corn cob meal, zytase liquid enzymic activity is 50UI/ml～70UI/ml;
(4) activity charcoal powder is adopted in the decolouring of xylo-oligosaccharide solution, and actual conditions is 80 ℃ of bleaching temperatures, and the volume ratio of gac and liquid glucose is 0.5%～1.5%, bleaching time 25min～40min;
(5) xylo-oligosaccharide solution employing strong acid type cationic resin such as E306FG and macropore weak base type anionite-exchange resin such as D001 carry out removal of impurities.
In the above-mentioned method for preparing lower polyxylose, the used best alkali metal hydroxide of corn cob meal pre-treatment is a sodium hydroxide, and optimal concentration is 0.7%, and Optimal Temperature is 55 ℃, and the optimum treatment time is 60min, and best feed liquid weight ratio is 1: 10.
In the above-mentioned method for preparing lower polyxylose, when corn cob meal carried out directly-heated boiling cracking, best boiling temperature was 165 ℃, and cooking time 120min, optimum catalyst are acetate, and addition is 0.5% of a corn cob meal weight.
In the above-mentioned method for preparing lower polyxylose, xylanase hydrolysis reaction optimum temps is 55 ℃, reaction times 8h, and zytase liquid is 1ml/1.45g with the ratio of corn cob meal, zytase liquid enzymic activity is 60UI/ml.
In above-mentioned xylo-oligosaccharide preparation method's the decolorization, the optimum volume ratio of gac and liquid glucose is 1%, bleaching time 30min.
In the above-mentioned method for preparing lower polyxylose, adopt the economic benefits and social benefits vacuum concentration, under 75 ℃ of the simmer down tos, xylo-oligosaccharide enzyme liquid is concentrated to the syrup of total sugar content 15%～20% for the first time; For the second time under 75 ℃ of the simmer down tos, the xylo-oligosaccharide liquid glucose is concentrated to the syrup of total sugar content 55%～75%.
In the above-mentioned method for preparing lower polyxylose, can adopt the agent of spray drying method for preparation xylo-oligosaccharide Icing Sugar, the inlet temperature of hot blast is 130 ℃～160 ℃ during spraying drying, and temperature out is 65 ℃～85 ℃, and mass flow is 0.8～1.2m
310 seconds～20 seconds residence time in the/h, tower, vehicle is maltodextrin, beta-cyclodextrin or W-Gum.
In the above-mentioned method for preparing lower polyxylose, the suitableeest vehicle of preparation xylo-oligosaccharide Icing Sugar agent is a maltodextrin.
Among the above-mentioned preparation method, the selection of zytase and preparation technology and the explosion of directly-heated vapour separate that the selection of catalyzer and reaction conditions is crucial in the process.
Tall building invention has following advantage:
(1) adopt alkali metal hydroxide such as solution such as potassium hydroxide, sodium hydroxide under certain temperature and time conditions, corn cob to be carried out pre-treatment, removed the most of xylogen in the corn cob, and make its weave construction become loose relatively, help the stripping of xylan in the corn cob;
(2) adopting high temperature steaming and quick-fried the combining of directly-heated vapour is that directly-heated boiling cracked mode is handled corn cob, xylan in the corn cob is dissolved out to greatest extent, promptly improve working efficiency, reduced the cost of equipment again, made the xylo-oligosaccharide suitability for industrialized production become relatively easy and easy;
(3) select the zytase liquid hydrolysis of producing to obtain xylo-oligosaccharide product based on xylo-bioses by the xylan liquid of directly-heated boiling cracking corn cob gained by the spE-86 bacterial strain.
Detailed process block diagram of the present invention is as follows:
Corn cob
↓
Removal of impurities
↓
Pulverize
↓
Pre-treatment
↓
Washing
↓
Size mixing
↓
The high temperature steaming cracking
↓
Vapor-liquid separation
↓
Xylanase hydrolysis
↓
Filter
↓
Once decolouring
↓
A vacuum concentration
↓
Secondary decolourization
↓
Ion-exchange
↓
Secondary vacuum concentrates
Xylo-oligosaccharide syrup vehicle
↓
Spraying drying
↓
Xylo-oligosaccharide powdery product
The invention provides a kind of means that combine with enzyme process and physical chemistry makes hemicellulose in the corn cob meal change into the method for xylo-oligosaccharide.This method comprises the raw material corn cob in the aqueous solution such as alkali metal hydroxide such as potassium hydroxide, sodium hydroxide, carries out pre-treatment under 30 ℃～60 ℃ of certain temperatures and the time 30min～120min; To under effects such as weak-type catalyzer such as acetate, formic acid, citric acid, adopt directly-heated steam through pretreated corn cob in 155 ℃～180 ℃ Pintsch process 30min～120min; With the corn cob meal mixture of directly-heated cracking gained in 45 ℃～60 ℃ temperature under the effect of zytase liquid, reaction 4h～10h is warming up to 90 ℃～105 ℃ then, insulation 10min～30min; With gained xylo-oligosaccharide liquid glucose by activated carbon decolorizing and Zeo-karb such as E306FG and anionite-exchange resin such as D001 removal of impurities, vacuum concentration is 55%～75% liquid glucose again, with maltodextrin, beta-cyclodextrin or W-Gum is vehicle, and spray-dried total sugar content is 20%～50% xylo-oligosaccharide pulvis.
The sp.E-86 type zytase liquid that the present invention adopts is to be made through liquid fermenting by streptomycete sp.E-86 bacterial strain.
For better removing the color of gained xylo-oligosaccharide enzyme liquid, activated carbon decolorizing of the present invention can be twice.
Ion exchange resin removal of impurities process of the present invention is positive negative and positive, and xylo-oligosaccharide liquid glucose temperature is less than 45 ℃, and per hour xylo-oligosaccharide liquid glucose flow velocity is 1～2 times of resin volume, and the specific conductivity of gained liquid glucose is less than 50VS/cm, and pH is 4.5～6.0.
The present invention illustrates with following example:
Embodiment 1
Take by weighing 40 orders～60 purpose corn cob meal 500kg adding 4000L and contain in the solution of 0.7% sodium hydroxide, stir 55 ℃ of stir process 60min under the 75rpm condition.Centrifuging, the washing filter cake to pH be 7.0.Water is with filter cake furnishing slurry, and solid-to-liquid ratio is 1: 8, adds 2.5kg acetate, behind 160 ℃ of following boiling cracking 2h, enters enzymatic vessel through vapour liquid separator, is cooled to 55 ℃.Use the pH to 5.5 of the sodium hydroxide solution conditioned reaction liquid of 1mol/ml hydrochloric acid soln and 1mol/ml respectively, the amount of pressing 1ml enzyme liquid/1.45g corn cob meal adds sp.E-86 type zytase liquid, its enzymic activity is 60UI/ml, behind the enzyme digestion reaction 8h, at 90 ℃ of insulation deactivation 15min, be cooled to 60 ℃ and carry out Plate Filtration.The activity charcoal powder that in liquid glucose, adds cumulative volume 1%, 80 ℃ are stirred decolouring 30min, filter, with liquid glucose simmer down to total sugar content 15% xylo-oligosaccharide syrup at 75 ℃.15% syrup is carried out secondary decolourization, and decolorization condition is with for the first time identical.To carry out removal of impurities through ion exchange resin column on the syrup of twice decolouring then, the liquid glucose specific conductivity is less than 50VS/cm, pH5.0.At last under 75 ℃, it is 7% light yellow thick xylo-oligosaccharide syrup that liquid glucose is concentrated into total sugar content, yield 8.8%.
Embodiment 2
Take by weighing 40 orders～60 purpose corn cob meal 500kg, add 4000L and contain in the solution of 0.5% sodium hydroxide, stir 55 ℃ of stir process 60min under the 75rpm condition.Centrifuging, the washing filter cake to pH be 7.0.Water is with filter cake furnishing slurry, and solid-to-liquid ratio is 1: 8, adds the 2.0kg citric acid, behind 160 ℃ of following boiling cracking 2h, enters enzymatic vessel through vapour liquid separator, is cooled to 55 ℃.Use the pH to 5.5 of the sodium hydroxide solution conditioned reaction liquid of 1mol/ml hydrochloric acid soln and 1mol/ml respectively, press the amount sp.E-86 type zytase liquid of 1ml enzyme liquid/1.3g corn cob meal, its enzymic activity is 70UI/ml, behind the enzyme digestion reaction 6h, at 90 ℃ of insulation deactivation 15min, be cooled to 60 ℃ and carry out Plate Filtration.The activity charcoal powder that in liquid glucose, adds cumulative volume 1%, 80 ℃ are stirred decolouring 30min, filter, with liquid glucose simmer down to total sugar content 20% xylo-oligosaccharide syrup at 75 ℃.20% syrup is carried out secondary decolourization, and decolorization condition is with for the first time identical.To carry out removal of impurities through ion exchange resin column on the syrup of twice decolouring then, the liquid glucose specific conductivity is less than 50VS/cm, pH5.0.At last under 75 ℃, it is 70% light yellow thick xylo-oligosaccharide syrup that liquid glucose is concentrated into total sugar content, yield 8.5%.
Embodiment 3
Take by weighing 40 orders～60 purpose corn cob meal 500kg and add 4000L and contain in the solution of 0.7% sodium hydroxide, stir 55 ℃ of stir process 60min under the 75rpm condition.Centrifuging, the washing filter cake to pH be 7.0.Water is with filter cake furnishing slurry, and solid-to-liquid ratio is 1: 8, behind 165 ℃ of following boiling cracking 2h, enters enzymatic vessel through vapour liquid separator, is cooled to 55 ℃.Use the pH to 5.5 of the sodium hydroxide solution conditioned reaction liquid of 1mol/ml hydrochloric acid soln and 1mol/ml respectively, the amount of pressing 1ml enzyme liquid/1.45g corn cob meal adds sp.E-86 type zytase liquid, its enzymic activity is 60UI/ml, behind the enzyme digestion reaction 8h, at 90 ℃ of insulation deactivation 15min, be cooled to 60 ℃ and carry out Plate Filtration.The activity charcoal powder that in liquid glucose, adds cumulative volume 1%, 80 ℃ are stirred decolouring 30min, filter, with liquid glucose simmer down to total sugar content 15% xylo-oligosaccharide syrup at 75 ℃.15% syrup is carried out secondary decolourization, and decolorization condition is with for the first time identical.To carry out removal of impurities through ion exchange resin column on the syrup of twice decolouring then, the liquid glucose specific conductivity is less than 50VS/cm, pH5.0.At last under 75 ℃, it is 70% light yellow thick xylo-oligosaccharide syrup that liquid glucose is concentrated into total sugar content, yield 7.6%.
Embodiment 4
Xylo-oligosaccharide syrup at the 100kg 40% that makes by condition among the embodiment 1 and step, adding content is 98% maltodextrin 120kg, 145 ℃ of inlet temperatures, 85 ℃ of temperature outs, mass flow is to carry out spraying drying under the 1.0m3/h condition, obtains the xylo-oligosaccharide powdery product of content 25%.
Claims (8)
1, a kind of method for preparing lower polyxylose comprises decolouring, removal of impurities, the concentrated and dry technology of the stripping, xylanase hydrolysis reaction and the xylo-oligosaccharide solution that adopt xylan in alkali hydroxide soln pre-treatment corn cob meal, washing, the corn cob meal, wherein:
(1) alkali hydroxide soln that adopted of corn cob meal pre-treatment is potassium hydroxide, sodium hydroxide solution, during pre-treatment, the concentration of alkali hydroxide soln is 0.5%～1.5%, 30 ℃～60 ℃ of treatment temps, time 30min～120min, corn cob meal and alkali hydroxide soln weight ratio are 1: 8～1: 12;
(2) directly-heated boiling fragmentation pattern is adopted in the stripping of xylan in the corn cob meal, boiling temperature is 155 ℃～180 ℃, cooking time 30min～120min, the weight ratio of corn cob meal and water is 1: 6～1: 10, use acetate, formic acid, citric acid weak-type catalyzer in the digestion process, addition is 0.2%～1.5% of a corn cob meal weight;
What (3) enzymatic hydrolysis reaction used is sp.E-86 type zytase liquid, 45 ℃～60 ℃ of enzymatic hydrolysis reaction temperature, enzymatic hydrolysis reaction time 4h～10h, zytase liquid is 1ml/1.2g～1ml/1.6g with the ratio of corn cob meal, zytase liquid enzymic activity is 50UI/ml～70UI/ml;
(4) activity charcoal powder is adopted in the decolouring of xylo-oligosaccharide solution, and actual conditions is 80 ℃ of bleaching temperatures, and the volume ratio of gac and liquid glucose is 0.5%～1.5%, bleaching time 25min～40min;
(5) xylo-oligosaccharide solution adopts strong acid type cationic resin and macropore weak base type anionite-exchange resin to carry out removal of impurities.
2, method for preparing lower polyxylose according to claim 1, the used alkali metal hydroxide of its corn cob meal pre-treatment is a sodium hydroxide, and concentration is 0.7%, and temperature is 55 ℃, and the treatment time is 60min, the feed liquid weight ratio is 1: 10.
When 3, method for preparing lower polyxylose according to claim 1, its corn cob meal were carried out directly-heated boiling cracking, boiling temperature was 165 ℃, and cooking time 120min, catalyzer are acetate, and addition is 0.5% of a corn cob meal weight.
4, method for preparing lower polyxylose according to claim 1, its xylanase hydrolysis temperature of reaction is 55 ℃, reaction times 8h, zytase liquid is 1ml/1.45g with the ratio of corn cob meal, zytase liquid enzymic activity is 60UI/ml.
5, method for preparing lower polyxylose according to claim 1, the volume ratio of gac and liquid glucose is 1% in decolorization, bleaching time 30min.
6, method for preparing lower polyxylose according to claim 1, the present invention adopts the economic benefits and social benefits vacuum concentration, for the first time under 75 ℃ of the simmer down tos, the xylo-oligosaccharide liquid glucose is concentrated to the syrup of total sugar content 15%～20%; For the second time under 75 ℃ of the simmer down tos, the xylo-oligosaccharide liquid glucose is concentrated to the syrup of total sugar content 55%～75%.
7, method for preparing lower polyxylose according to claim 1, the present invention adopts the agent of spray drying method for preparation xylo-oligosaccharide Icing Sugar, and the inlet temperature of hot blast is 130 ℃～160 ℃ during spraying drying, and temperature out is 65 ℃～85 ℃, and mass flow is 0.8～1.2m
310 seconds～20 seconds residence time in the/h, tower, vehicle is maltodextrin, beta-cyclodextrin or W-Gum.
8, method for preparing lower polyxylose according to claim 7, preparation xylo-oligosaccharide Icing Sugar agent vehicle is a maltodextrin.
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|---|---|---|---|
| CNB011311711A CN1186461C (en) | 2001-09-05 | 2001-09-05 | Prepn of oligoxylose |
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|---|---|---|---|
| CNB011311711A CN1186461C (en) | 2001-09-05 | 2001-09-05 | Prepn of oligoxylose |
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| CN1186461C true CN1186461C (en) | 2005-01-26 |
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Families Citing this family (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1332040C (en) * | 2003-03-27 | 2007-08-15 | 南京大学 | Decolouring method of hydrolytic neutralization liquid in xylose production process |
| CN1916171B (en) * | 2006-09-11 | 2010-05-12 | 中国农业大学 | Method for producing xylobiose, and dedicated immobilized enzyme |
| CN101565468B (en) * | 2009-05-08 | 2011-12-28 | 河南工业大学 | Method for producing xylo-oligosaccharide by utilizing cotton seed hulls |
| CN101880298A (en) * | 2010-07-16 | 2010-11-10 | 天津科技大学 | Method for preparing food-grade xylooligosaccharide |
| CN104109722B (en) * | 2014-07-01 | 2016-03-30 | 丽水学院 | A kind of method preparing xylo-oligosaccharide |
| CN104164520B (en) * | 2014-07-15 | 2016-06-22 | 南京林业大学 | A kind of method that acetic acid controlled catalytic xylan directionally hydrolyzing produces multicomponent oligomeric xylose |
| CN105077132A (en) * | 2015-08-07 | 2015-11-25 | 浙江海洋学院 | Method for making seafood seasoning through low-value fishes |
| CN105483184A (en) * | 2016-01-07 | 2016-04-13 | 中国科学院过程工程研究所 | Production method of high-yield xylooligosaccharide |
| CN105463040A (en) * | 2016-01-13 | 2016-04-06 | 中国科学院过程工程研究所 | Method for raising yield of xylooligosaccharide |
| CN105753645A (en) * | 2016-03-31 | 2016-07-13 | 常州大学 | Method for preparing powder xylitol with purity being 55% |
| CN107212403A (en) * | 2017-04-21 | 2017-09-29 | 浙江禾蓓生物科技有限公司 | Caulis et Folium Tritici aestivi barley green composition and its preparation process |
| CN107868806A (en) * | 2017-11-27 | 2018-04-03 | 许昌学院 | A kind of method that xylo-oligosaccharide is prepared by lignocellulosic |
| CN108251472B (en) * | 2018-01-09 | 2021-10-15 | 北京林业大学 | Preparation method of xylo-oligosaccharide |
| CN112359080A (en) * | 2020-11-03 | 2021-02-12 | 江苏康维生物有限公司 | Preparation method of xylo-oligosaccharide with high xylobiose and xylotriose content |
| 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 |
| CN115369190A (en) * | 2022-02-21 | 2022-11-22 | 淮阴师范学院 | Method for preparing xylo-oligosaccharide mixed solution by controlled catalytic biomass oriented hydrolysis of bamboo vinegar |
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2001
- 2001-09-05 CN CNB011311711A patent/CN1186461C/en not_active Expired - Lifetime
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Address after: 136 mailbox, No. 17 Tsinghua East Road, Haidian District, Beijing, 100083 Co-patentee after: Shandong LongLive Bio-technology Co., Ltd. Patentee after: China Agricultural University Address before: 136 mailbox, No. 17 Tsinghua East Road, Haidian District, Beijing, 100083 Co-patentee before: Longli Biological Science and Technology Co., Ltd., Shandong Patentee before: China Agricultural University |
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