CN101880298A - Method for preparing food-grade xylooligosaccharide - Google Patents

Method for preparing food-grade xylooligosaccharide Download PDF

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Publication number
CN101880298A
CN101880298A CN 201010228806 CN201010228806A CN101880298A CN 101880298 A CN101880298 A CN 101880298A CN 201010228806 CN201010228806 CN 201010228806 CN 201010228806 A CN201010228806 A CN 201010228806A CN 101880298 A CN101880298 A CN 101880298A
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China
Prior art keywords
food
acid
xylooligosaccharide
preparation
grade
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Pending
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CN 201010228806
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Chinese (zh)
Inventor
张泽生
王可凤
吕晓玲
孙平
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Tianjin University of Science and Technology
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Tianjin University of Science and Technology
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Priority to CN 201010228806 priority Critical patent/CN101880298A/en
Publication of CN101880298A publication Critical patent/CN101880298A/en
Pending legal-status Critical Current

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Abstract

The invention relates to a method for preparing food-grade xylooligosaccharide, which comprises the following steps of: putting xylose, edible acid and polyol into a reaction kettle in a weight ratio, mixing the mixture uniformly to perform polymerization, controlling the temperature to be between 140 and 260 DEG C, reacting the mixture for 0.25 to 4 hours under the vacuum degree of 0 to 1 to form a polymer, and cooling and crushing the polymer to obtain the food-grade xylooligosaccharide. The polymer content of the xylooligosaccharide obtained by the method is up to over 93 percent, the reducing sugar content is less than 1 percent, and the average molecular weight is between 500 and 900; and the xylooligosaccharide is of milk white, has good mouthfeel and can fully meet the application in food processing.

Description

A kind of preparation method of food-grade xylooligosaccharide
Technical field
The invention belongs to field of food, relate in particular to a kind of preparation method of food-grade xylooligosaccharide.
Background technology
Xylo-oligosaccharide is the oligosaccharide mixture that 2~7 wood sugars are formed by connecting with β-1,4 glycosidic link, wherein based on xylo-bioses and xylotriose.Xylo-oligosaccharide has efficiently (bifidus bacillus efficiently rises in value), stable, safe, nontoxic, good characteristic such as Application Areas is wide, and can effectively keep HUMAN HEALTH: the organic acid that its produces can reduce enteron aisle pH value, suppresses the infection of pathogeny bacterium, reduces corrupt substance, promotes intestines peristalsis, prevent constipation; It can also synthesize vitamin B group, promote protein digestion to absorb, improve body immunity.At present, the exploitation of xylo-oligosaccharide be applied in the functional foodstuff in occupation of significant status.
It normally is raw material with the natural phant that traditional technology is produced xylo-oligosaccharide, adopt methods such as acidolysis, enzymolysis, high temperature degradation or microwave degradation, with the xylan degrading in the plant is the xylo-oligosaccharide of different polymerization degree, and then obtains through operations such as a series of separation, purifying.These three kinds of methods of acidolysis, high temperature degradation and microwave degradation have had a strong impact on the prospects for commercial application of xylo-oligosaccharide owing to exist that technical difficulty is big, the bad control of speed of response and by product are more and are not easy to shortcoming such as separation and purification.Newer technology is biological enzyme, and it is to be substrate with the xylan, utilizes the microbial enzyme hydrolysis and gets, its by product is less and be easy to make with extra care, but zytase costs an arm and a leg, and is stronger to Substratspezifitaet, bacterium producing multi enzyme preparation culture condition demand complexity, growth cycle is short, and needs in time to change bacterial strain.
By retrieval, find following several pieces of patent publication us: 1, a kind of preparation method of functional low polyxylose alcohol (CN101440109) is to be raw material with common xylo-oligosaccharide, under the effect of catalyzer, makes functional low polyxylose alcohol by hydrogenation reaction.2, a kind of method for preparing lower polyxylose (CN1403591) comprises the raw material corn cob is carried out pre-treatment in alkali metal hydroxide aqueous solution; Under effects such as weak-type catalyzer such as acetate, formic acid, citric acid, carry out the directly-heated cracking then; After the directly-heated cracking with zytase liquid reaction, by activated carbon decolorizing and ion exchange resin removal of impurities, vacuum concentration again, can maltodextrin etc. be vehicle, spray-dried must the xylo-oligosaccharide pulvis.3, a kind of production method of high-purity oligoxylose (CN1556110), be to be raw material with the corn cob, after dilute acid pretreatment and boiling, with zytase in pH3~10, carry out enzymolysis under 30~70 ℃, enzymolysis solution again with macromolecular substance and small molecules monose in ultrafiltration and the nanofiltration removal enzymolysis solution, obtains xylo-oligosaccharide content at last and reaches above xylo-oligosaccharide syrup of 90% (to solid substance) or powder-product after refining.
Above-mentioned three pieces of patent documentations also exist the general shortcoming of prior art.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art part, a kind of preparation method of food-grade xylooligosaccharide of new high efficiency is provided.
The present invention is achieved through the following technical solutions:
A kind of preparation method of food-grade xylooligosaccharide, by weight proportion wood sugar, edible acid and polyvalent alcohol are dropped in the reactor, mix polymerization, temperature is controlled at 140 ℃~260 ℃, reaction times 0.25h~4h, vacuum tightness 0~1 forms polymkeric substance, with pulverizing after this polymkeric substance cooling, promptly get food-grade xylooligosaccharide.
And the weight percentage ranges of described wood sugar, edible acid and polyvalent alcohol is respectively:
Wood sugar 73%~96.9%
Edible acid 0.1%~7%
Polyvalent alcohol 3%~20%.
And described edible acid is citric acid, oxysuccinic acid, fumaric acid, tartrate, succsinic acid or hexanodioic acid.
And described polyvalent alcohol is Xylitol, sorbyl alcohol, N.F,USP MANNITOL, melampyrum or erythritol.
And described reactor is a high temperature interlayer stainless steel cauldron, and uses the thermal oil heat supply.
Advantage of the present invention and positively effect are:
1, the present invention controls product degree of polymerization and reaction kinetics by the part by weight, reaction times, temperature and the vacuum tightness that change reactant, conversion unit adopts high temperature interlayer stainless steel cauldron, and use the thermal oil heat supply, simple and safe operation, whole process of production is expensive cheap, technical difficulty is less, and the suitability for industrialized production ability is strong, high efficiency.
2, the raw materials used economy of the present invention is easy to get, and product is creamy white after pulverizing, and by product is less, has exempted complicated loaded down with trivial details purification procedures of later stage, and product can directly be used in the food as additive.
3, in the xylo-oligosaccharide that the present invention obtains, polymer content is up to 93%, and reducing sugar content is less than 1%, and molecular-weight average is between 500~900, and product is creamy white, and mouthfeel is better, can fully satisfy xylo-oligosaccharide in Application in Food Processing.
Embodiment
Below in conjunction with embodiment, the present invention is further described; Following embodiment is illustrative, is not determinate, can not limit protection scope of the present invention with following embodiment.
Embodiment 1:
A kind of preparation method of food-grade xylooligosaccharide, step is:
With wood sugar 96.9 grams, tartrate 0.1 gram and sorbyl alcohol 3 grams, drop in the reactor, mix polymerization, used reactor is a high temperature interlayer stainless steel cauldron, and uses thermal oil heat supply, temperature to be controlled at about 140 ℃, reaction 4h, vacuum tightness 0 forms polymkeric substance; With pulverizing after this polymkeric substance cooling, promptly get food-grade xylooligosaccharide.
Embodiment 2:
With wood sugar 79 grams, oxysuccinic acid 5 grams and N.F,USP MANNITOL 16 grams, drop in the reactor, mix polymerization, used reactor is a high temperature interlayer stainless steel cauldron, and uses thermal oil heat supply, temperature to be controlled at about 260 ℃, reaction 0.25h, vacuum tightness 1 forms polymkeric substance; With pulverizing after this polymkeric substance cooling, promptly get food-grade xylooligosaccharide.
Embodiment 3:
With wood sugar 90 grams, citric acid 1.2 grams and Xylitol 8.8 grams, drop in the reactor, mix polymerization, used reactor is a high temperature interlayer stainless steel cauldron, and uses thermal oil heat supply, temperature to be controlled at about 180 ℃, reaction 1h, vacuum tightness 1 forms polymkeric substance; With pulverizing after this polymkeric substance cooling, promptly get food-grade xylooligosaccharide.
Be tested and appraised, up to 93%, reducing sugar content is that molecular-weight average is between 500~900 below 1% by the prepared target product content of the inventive method.

Claims (5)

1. the preparation method of a food-grade xylooligosaccharide, it is characterized in that: by weight proportion wood sugar, edible acid and polyvalent alcohol are dropped in the reactor, mix polymerization, temperature is controlled at 140 ℃~260 ℃, reaction times 0.25h~4h, vacuum tightness 0~1 forms polymkeric substance, with pulverizing after this polymkeric substance cooling, promptly get food-grade xylooligosaccharide.
2. the preparation method of food-grade xylooligosaccharide according to claim 1, it is characterized in that: the weight percentage ranges of described wood sugar, edible acid and polyvalent alcohol is respectively:
Wood sugar 73%~96.9%
Edible acid 0.1%~7%
Polyvalent alcohol 3%~20%.
3. the preparation method of food-grade xylooligosaccharide according to claim 1 and 2, it is characterized in that: described edible acid is citric acid, oxysuccinic acid, fumaric acid, tartrate, succsinic acid or hexanodioic acid.
4. the preparation method of food-grade xylooligosaccharide according to claim 1 and 2, it is characterized in that: described polyvalent alcohol is Xylitol, sorbyl alcohol, N.F,USP MANNITOL, melampyrum or erythritol.
5. the preparation method of food-grade xylooligosaccharide according to claim 1, it is characterized in that: described reactor is a high temperature interlayer stainless steel cauldron, and uses the thermal oil heat supply.
CN 201010228806 2010-07-16 2010-07-16 Method for preparing food-grade xylooligosaccharide Pending CN101880298A (en)

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CN 201010228806 CN101880298A (en) 2010-07-16 2010-07-16 Method for preparing food-grade xylooligosaccharide

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102329341A (en) * 2011-06-23 2012-01-25 天津实发中科百奥工业生物技术有限公司 Preparation method of oligose
CN110256510A (en) * 2019-06-06 2019-09-20 南京林业大学 A method of producing multicomponent xylo-oligosaccharide
CN113004348A (en) * 2021-03-26 2021-06-22 南京工业大学 Method for preparing oligosaccharide by mechanical self-assembly

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3876794A (en) * 1972-12-20 1975-04-08 Pfizer Dietetic foods
CN1251109A (en) * 1997-03-19 2000-04-19 考尔特食品科学公司 Polymerization of mono- and disaccharides using low levels of polycarboxylic acids
CN1403591A (en) * 2001-09-05 2003-03-19 中国农业大学 Prepn of oligoxylose
CN1556110A (en) * 2004-01-05 2004-12-22 江南大学 Production method of high purity oligoxylose

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3876794A (en) * 1972-12-20 1975-04-08 Pfizer Dietetic foods
CN1251109A (en) * 1997-03-19 2000-04-19 考尔特食品科学公司 Polymerization of mono- and disaccharides using low levels of polycarboxylic acids
CN1403591A (en) * 2001-09-05 2003-03-19 中国农业大学 Prepn of oligoxylose
CN1556110A (en) * 2004-01-05 2004-12-22 江南大学 Production method of high purity oligoxylose

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102329341A (en) * 2011-06-23 2012-01-25 天津实发中科百奥工业生物技术有限公司 Preparation method of oligose
CN110256510A (en) * 2019-06-06 2019-09-20 南京林业大学 A method of producing multicomponent xylo-oligosaccharide
CN113004348A (en) * 2021-03-26 2021-06-22 南京工业大学 Method for preparing oligosaccharide by mechanical self-assembly
CN113402569A (en) * 2021-03-26 2021-09-17 南京工业大学 Method for preparing oligosaccharide by mechanical self-assembly
CN113402569B (en) * 2021-03-26 2022-04-12 南京工业大学 Method for preparing oligosaccharide by mechanical self-assembly
CN113004348B (en) * 2021-03-26 2023-01-24 南京工业大学 Method for preparing oligosaccharide by mechanical self-assembly

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Application publication date: 20101110