CN1613879A - Clean and effective preparation of oligoxylose - Google Patents
Clean and effective preparation of oligoxylose Download PDFInfo
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- CN1613879A CN1613879A CN200410064667.4A CN200410064667A CN1613879A CN 1613879 A CN1613879 A CN 1613879A CN 200410064667 A CN200410064667 A CN 200410064667A CN 1613879 A CN1613879 A CN 1613879A
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- xylan
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- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 70
- 229920001221 xylan Polymers 0.000 claims abstract description 70
- 150000004823 xylans Chemical class 0.000 claims abstract description 70
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000006228 supernatant Substances 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 51
- HEBKCHPVOIAQTA-NGQZWQHPSA-N d-xylitol Chemical compound OC[C@H](O)C(O)[C@H](O)CO HEBKCHPVOIAQTA-NGQZWQHPSA-N 0.000 claims description 44
- 239000000203 mixture Substances 0.000 claims description 9
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- 238000000746 purification Methods 0.000 claims description 5
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- 238000001035 drying Methods 0.000 claims description 3
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- 238000004821 distillation Methods 0.000 claims description 2
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- 102000004190 Enzymes Human genes 0.000 abstract description 2
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- 238000005516 engineering process Methods 0.000 description 5
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- 238000010812 external standard method Methods 0.000 description 4
- WQYVRQLZKVEZGA-UHFFFAOYSA-N hypochlorite Chemical compound Cl[O-] WQYVRQLZKVEZGA-UHFFFAOYSA-N 0.000 description 4
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- 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 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 2
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- 206010013786 Dry skin Diseases 0.000 description 1
- 241001223091 Penicillium corylophilum Species 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 241000499912 Trichoderma reesei Species 0.000 description 1
- 241000209140 Triticum Species 0.000 description 1
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- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- FXAGBTBXSJBNMD-UHFFFAOYSA-N acetic acid;2-hydroxypropane-1,2,3-tricarboxylic acid Chemical compound CC(O)=O.OC(=O)CC(O)(C(O)=O)CC(O)=O FXAGBTBXSJBNMD-UHFFFAOYSA-N 0.000 description 1
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Abstract
A clean an effective preparation of oligoxylose is carried out by: making xylan solution bydissolving xylan in water or buffering liquid, adding xylanase into it to obtain an enzyme hydrolystic liquid, adding alcohol, centrifuging to obtain supernatant, separating to obtain oligoxylose. It costs low, has no pollution, and is effective. Its product likes natural one.
Description
Technical field
The present invention relates to a kind of preparation method of functional oligose, relate in particular to a kind of enzymatic-process preparation method of xylo-oligosaccharide, more specifically to a kind of clean and effective preparation of xylo-oligosaccharide.
Background technology
Xylo-oligosaccharide claims wood oligose again, be by 2-7 wood sugar with β-1, the functional oligose that the 4-glycosidic link is formed by connecting.Compare with other oligose, xylo-oligosaccharide has better stability, can promote bifidus bacillus propagation in specificity ground, therefore, it is the most effective bifidus factor, only needs picked-up 0.7 gram just can reach whole intestines effect (general active oligose daily dosage portion is the 2-10 gram) for each person every day.
The preparation of xylo-oligosaccharide generally includes following three main processes:
1, the extraction of xylan: xylan can be extracted from plant fiber material with methods such as alkaline solution, hot water, high pressure steam explosions; Adding ethanol can make and slightly carry xylan and be precipitated out from extract; Process ultrafiltration, ethanol sedimentation, dissolving again, redeposition, hydrogen peroxide or methods such as hypochlorite processing, column chromatography can make and slightly propose the xylan purification.
2, the degraded of xylan:, or add the reaction that is hydrolyzed of a certain amount of zytase, the different mixture of generation palliating degradation degree in the xylan lysate to the extract of plant fiber material.Used zytase is produced by superior strain or genetic engineering bacterium fermentation through seed selection usually, and common bacterial strain comprises genus bacillus, Alcaligenes, clostridium, false monospore bacillus, aspergillus niger, Trichodermareesei, Penicillium corylophilum etc.
3, the separation of xylo-oligosaccharide: the mixture solution that contains xylo-oligosaccharide is purified through methods such as centrifugation, decolorizing with activated carbon, chromatographic separation, ion-exchange, ultrafiltration, makes product through methods such as vacuum concentration, freeze concentration, spraying dryings more at last.
More than each process all have multiple diverse ways to select for use, so diversity appears in the xylo-oligosaccharide technology of preparing.Though the method that different technologies of preparing is taked is varied, the main process of overall craft flow process is as follows:
1. be to add zytase in the xylan to the enzymolysis substrate, allow the abundant hydrolysis of xylan under certain conditions;
By the absorption of activated carbon or ion exchange resin decolour, desalination;
3. collect the xylo-oligosaccharide that enzymolysis produces;
4. further xylo-oligosaccharide solution is concentrated or the dry product that obtains.
The problem that exists in such technology is that enzyme digestion reaction liquid is long-pending big, concentration is low, impurity is many, thereby efficiency of post treatment is low, the chemical industry program is many, to the equipment requirements height, so production cost remains high.
Some scholar has recognized the limitation of above-mentioned technology, brings into use the purified xylan to make the substrate of enzyme digestion reaction.At present the basic skills of the refining xylan of preparation is as follows: the concentration that adds 3 times of volumes in alkali extract is higher than 90% ethanol, and xylan etc. is precipitated out from the raw material extract, and is centrifugal or filter to isolate and slightly carry xylan; To slightly carry xylan and be dissolved in water, and add 3 times of volume of ethanol again and make the xylan precipitation and isolate xylan; Repeat the solubility small molecular weight impurity that several accompanies with macromole such as removal and xylans, oxygenants such as also adding hydrogen peroxide that has in this process or hypochlorite make the goods color thin out.As seen this is loaded down with trivial details, expensive, as to produce a sewage process.
Though used the purified xylan to make the enzyme digestion reaction substrate, the isolation technique of the xylo-oligosaccharide that is produced fails to avoid some inefficient operations such as ultrafiltration, gac or ion exchange resin absorption/wash-out or the like equally.Therefore, the novel method for preparing xylo-oligosaccharide is cleanly and efficiently demanded urgently producing.
Summary of the invention
The purpose of this invention is to provide a kind of method for preparing xylo-oligosaccharide of low-cost and pollution-less, purpose of the present invention is achieved by the following technical programs:
The clean and effective preparation of xylo-oligosaccharide of the present invention may further comprise the steps:
Steps A: xylan is dissolved in water or damping fluid is mixed with xylan solution, adds zytase in this solution, hydrolyzed xylan gets enzymolysis solution;
Step B: add ethanol in above-mentioned enzymolysis solution, the centrifuging and taking supernatant liquor obtains xylo-oligosaccharide solution;
Step C: obtain xylo-oligosaccharide from above-mentioned xylo-oligosaccharide solution separating.
Ethanol described in the inventive method recommends working concentration to be equal to or higher than 75% ethanol, and preferred concentration is higher than 90% ethanol, and preferably concentration is 95% ethanol.
The inventive method steps A is dissolved in water or damping fluid with xylan, be mixed with xylan solution, the concentration of xylan solution does not have particular requirement, as long as be convenient to operation, it is 6-30% that the present invention recommends xylan concentration, and optionally heated and stirred makes homogenization when preparation; Water described in the present invention is edible water, can be tap water, pure water or distilled water, preferred pure water and distilled water; Damping fluid of the present invention is recommended edible acetate (pH4-5.5) or citrate buffer solution (pH4-7); Zytase described in the inventive method can be made by prior art, and the present invention recommends to use utmost point thermotolerance zytase, preferred Thermotoga maritima zytase B.Hydrolysising condition of the present invention is decided according to the characteristic of selected zytase.
Consumption of ethanol among the inventive method step B is decided by concentration of ethanol and production cost, when alcohol concn is low, suitably increases the ethanol consumption, can improve sedimentation effect, and it is 1-5 times of volume of enzymolysis solution that the present invention recommends the ethanol consumption, preferred 3 times of volumes.
The thick product that obtains among the step C of the present invention is that xylo-oligosaccharide solution can further be concentrated into desired concentration, as the syrup of total sugar content 70%; Or further drying is made pulvis.
Xylan described in the inventive method can obtain by prior art for preparing.But recommend to use the xylan that makes as follows: go out alkali-soluble substance in the plant fiber material with the alkaline solution extracting in order to realize goal of the invention, the present invention better; In the alkali extracted solution, add ethanol, use acid-conditioning solution pH behind the mixing; Centrifugal or filtration collecting precipitation thing is slightly carries xylan; Slightly carry xylan at least once with washing with alcohol, the throw out that obtains is the xylan of purification.
Strength of solution described in the present invention is if no specified otherwise all refers to weight percent.
The technical process (Fig. 1, Fig. 2) that the clean and effective preparation of application xylo-oligosaccharide of the present invention prepares xylo-oligosaccharide, general characteristic is dissolution characteristics and macromole and the difference of small-molecule substance aspect solubleness that has made full use of xylan, obtains the most approaching natural product with minimum chemical reagent and minimum procedure of processing.Specifically this technical process has replaced decolouring, ultrafiltration, ion-exchange, charcoal absorption etc. with methods such as clearly demarcated, the workable dissolution/precipitation of separating effect/centrifugal and has separated step; Simultaneously, realize that in conjunction with benefit and environmental requirement low consumption is pollution-free at aspects such as reagent type, solvent strength, reaction volumes.
In the further technical scheme of the present invention, make substrate with the high density xylan and produce the high density enzymolysis solution, (seeing Fig. 3, Fig. 4, Fig. 5) improved the efficient of purifying xylo-oligosaccharide, reduces the load of aftertreatment.
Come hydrolyzed xylan with utmost point thermotolerance zytase, its beneficial effect is:
(1) utmost point thermotolerance zytase has been realized efficiently expressing of genetic engineering bacterium, produces the enzyme level height, easily purifying;
(2) reaction that is hydrolyzed under 65-90 ℃ of high temperature does not need to take anti-corrosion measure.
By the xylo-oligosaccharide in the ethanol precipitation purifying enzymolysis solution, its beneficial effect is:
(1) can use the continuously streamed whizzer, the efficient height, throughput is strong;
(2) do not need other desalination, decolouring and leaching process, the character of products obtained therefrom is near natural product.
Description of drawings
Fig. 1 is to be the process flow diagram of feedstock production xylo-oligosaccharide with the xylan.
Fig. 2 is to be the process flow diagram of feedstock production xylo-oligosaccharide with the vegetable fibre.
Fig. 3 is that the product composition of slightly carrying xylan is analyzed collection of illustrative plates; HPLC analytical column: Sugarpak1; 6.5mm the analysis of * 300mm sugar post, chromatographic condition: column temperature: 85 ℃; Moving phase: water; Flow velocity: 0.5mL/min; Differential refraction detector sensitivity: 4, external standard method is demarcated, and sample size is 10 μ L.Standard model is purchased the company in Sigma.
Fig. 4 is the hydrolysate composition analysis collection of illustrative plates of xylan in the enzymolysis solution.HPLC analytical column: Sugarpak 1; 6.5mm the analysis of * 300mm sugar post, chromatographic condition: column temperature: 85 ℃; Moving phase: water; Flow velocity: 0.5mL/min; Differential refraction detector sensitivity: 4, external standard method is demarcated, and sample size is 10 μ L.Standard model is purchased the company in Sigma, and according to standard specimen, peak 14.0 is a wood sugar, and peak 11.4 is an xylo-bioses.
Fig. 5 is composition composition analysis collection of illustrative plates and the relative content in the xylo-oligosaccharide product.HPLC analytical column and chromatographic condition are the same, and according to standard specimen, peak 14.0 is a wood sugar, and peak 11.4 is an xylo-bioses.
Embodiment
Further specify the inventive method below in conjunction with accompanying drawing:
Embodiment 1:
(1) nothing is gone mouldy straw shrug off dust and dry after wear into the long broken grass silk of 1-20mm;
(2) take by weighing grass silk 10kg, add 2.5% KOH solution 501, soak boiling later in 4 hours 15 minutes, extrusion solution; Add 2.5% KOH solution 201 in careless slag again, boiling is 15 minutes once more, extrusion solution.Merge two portions and extrude liquid, with the centrifugal acquisition supernatant liquor about 501 of continuously streamed whizzer;
(3) add 95% ethanol 150L, with phosphorus acid for adjusting pH value to 6.0, centrifugal collection is precipitated slightly carries xylan behind the mixing;
(4) ethanol 501 of adding 95% in slightly carrying xylan precipitation piece is smashed the back stirring at low speed and was made its abundant balance, centrifugal collecting precipitate in 2 hours; Add ethanol again and repeat aforementioned process 2 times, obtain the xylan of purification, (see figure 3) HPLC analytical column: Sugarpak1; 6.5mm the analysis of * 300mm sugar post, chromatographic condition: column temperature: 85 ℃; Moving phase: water; Flow velocity: 0.5mL/min; Differential refraction detector sensitivity: 4, external standard method is demarcated, and sample size is 10 μ L.Standard model is purchased the company in Sigma.Preserve sealing preservation or dry back;
(5) above-mentioned refining xylan is dissolved in pure water with the concentration of 25% (w/v), heated and stirred makes homogenization be cooled to 70 ℃ later on, add (about 20U/g) Thermotoga maritima zytase B, insulation and stirring at low speed 12 hours, resulting enzymolysis solution adopt the detection of HPLC high pressure liquid chromatography, and wherein the composition and the content of sugar are seen Fig. 4; The xylo-oligosaccharide analysis on Content is used Sugarpak1 on Waters HPLC 246-E high pressure liquid chromatograph, 6.5mm * 300mm sugar post analysis.Chromatographic condition: column temperature: 85 ℃; Moving phase: water; Flow velocity: 0.5mL/min; Differential refraction detector sensitivity: 4, external standard method is demarcated, and sample size is 10 μ L.Standard model is purchased the company in Sigma.
(6) add 95% ethanol of 3 times of volumes and mixing, centrifugal unhydrolysed xylan, the non-xylan macromole of removing in the enzymolysis solution (comprising zymoprotein) obtains xylo-oligosaccharide solution;
(7) distillation recovery ethanol from above-mentioned xylo-oligosaccharide solution, and further concentrating obtains total sugar content 70% syrup, and wherein xylo-oligosaccharide composition and relative content are seen Fig. 5.
Embodiment 2: substantially the same manner as Example 1, difference is that xylan purchases the Sigma company in the U.S., article No.: x0627.Xylan is dissolved in citrate buffer solution, is mixed with concentration and is 30% xylan solution.
Embodiment 3: substantially the same manner as Example 1, difference is that xylan is prepared by following method:
NaOH solution lixiviate from corn cob with 2% goes out xylan; Add the ethanol of the concentration about 95% of 3 times of volumes in alkali extract, xylan is precipitated out, centrifugation goes out throw out; Throw out is dissolved in water, adds 3 times of volume of ethanol again and make xylan precipitation, centrifugal collecting precipitation; Repeat the xylan that 2 acquisitions purify.Xylan is dissolved in citrate buffer solution, is mixed with concentration and is 20% xylan solution.
Embodiment 4: substantially the same manner as Example 3, difference is to make raw material with broken wheat straw.
Embodiment 5: substantially the same manner as Example 3, difference is to make raw material with bagasse.
Embodiment 6: substantially the same manner as Example 3, difference be used zytase be dredge the thermophilic hyphomycete zytase of cotton shape (Sigma, x2753), 65 ℃ of temperature of reaction, pH6.5.
Embodiment 7: substantially the same manner as Example 3, difference is that used zytase is the actinomycetes zytases, and temperature of reaction is 60 ℃, pH5.0.
Embodiment 8: substantially the same manner as Example 2, difference is that with tap water preparation xylan solution concentration be 6%, and it is low slightly to obtain product purity.
Embodiment 9: substantially the same manner as Example 1, difference is that with distilled water preparation xylan solution concentration be 15%.
Embodiment 10: substantially the same manner as Example 1, difference is with sulphur acid for adjusting pH value to 4 xylan that purifies to be dissolved in edible acetate (citric acid) damping fluid, is mixed with concentration and is 5% xylan solution.
Embodiment 11: substantially the same manner as Example 1, difference is with acetate the pH value to be transferred to 7, and the xylan that purifies is dissolved in citrate buffer solution, is mixed with concentration and is 35% xylan solution.
Embodiment 12: substantially the same manner as Example 1, difference is slightly to carry xylan with 70% ethanol 301 purifications, repeats 4 times.
Embodiment 13: substantially the same manner as Example 1, difference is that 75% ethanol 201 purifies and slightly carries xylan, repeats 6 times.
Embodiment 14: substantially the same manner as Example 1, difference is that 90% ethanol 401 purifies and slightly carries xylan 1 time.
Embodiment 15: substantially the same manner as Example 1, difference is that xylo-oligosaccharide solution produces yellow powder through vacuum-drying.
Embodiment 16: substantially the same manner as Example 1, difference is in the step (6) to add 80% ethanol separating oligomeric wood sugar of 1 times of volume in enzymolysis solution.
Embodiment 17: substantially the same manner as Example 1, difference is in the step (6) to add 80% ethanol separating oligomeric wood sugar of 5 times of volumes in enzymolysis solution.
Claims (7)
1, a kind of clean and effective preparation of xylo-oligosaccharide may further comprise the steps:
Steps A: xylan is dissolved in water or damping fluid is mixed with xylan solution, adds zytase in this solution, hydrolyzed xylan gets enzymolysis solution;
Step B: add ethanol in above-mentioned enzymolysis solution, the centrifuging and taking supernatant liquor obtains xylo-oligosaccharide solution;
Step C: the ethanol in the above-mentioned xylo-oligosaccharide solution is removed in distillation, promptly obtains xylo-oligosaccharide.
2, the clean and effective preparation of xylo-oligosaccharide according to claim 1 is characterized in that, and is described
Step B is: add 1-5 times of volume of ethanol and mix, the centrifuging and taking supernatant liquor promptly obtains xylo-oligosaccharide solution.
3, the clean and effective preparation of xylo-oligosaccharide according to claim 2 is characterized in that, adds 3 times of volume ethanol among the described step B in enzymolysis solution.
According to the clean and effective preparation of one of claim 1-3 described xylo-oligosaccharide, it is characterized in that 4, xylan solution concentration is 6-30% in the described steps A.
5, the clean and effective preparation of xylo-oligosaccharide according to claim 4 is characterized in that, also has behind the described step C: further concentrate and make the xylo-oligosaccharide syrup or drying is made the xylo-oligosaccharide pulvis.
6, the clean and effective preparation of xylo-oligosaccharide according to claim 1 is characterized in that, described ethanol is that concentration is equal to or higher than 75% ethanol.
7, the clean and effective preparation of xylo-oligosaccharide according to claim 1 is characterized in that, also has the preparation process of xylan before steps A, and is specific as follows:
Step H: raw materials pretreatment;
Step I: go out alkali-soluble substance in the raw material with the alkaline solution extracting;
Step J: in the alkali extracted solution, add ethanol, use acid-conditioning solution pH behind the mixing; Centrifugal or filtration collecting precipitation thing is slightly carries xylan;
Step K: slightly carry xylan at least once with washing with alcohol, the throw out that obtains is the xylan of purification.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200410064667.4A CN1280313C (en) | 2004-09-20 | 2004-09-20 | Clean and effective preparation of oligoxylose |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200410064667.4A CN1280313C (en) | 2004-09-20 | 2004-09-20 | Clean and effective preparation of oligoxylose |
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| CN1613879A true CN1613879A (en) | 2005-05-11 |
| CN1280313C CN1280313C (en) | 2006-10-18 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007128025A1 (en) * | 2006-05-10 | 2007-11-15 | Lenzing Aktiengesellschaft | Method for preparing xylooligosaccharides |
| CN104628890A (en) * | 2014-12-24 | 2015-05-20 | 山东龙力生物科技股份有限公司 | Energy-saving preparation method of low-ingredient xylo-oligosaccharide powder |
| CN107722136A (en) * | 2017-10-20 | 2018-02-23 | 中国林业科学研究院林产化学工业研究所 | A kind of beam system for certain degree of polymerization xylan method |
| CN109049234A (en) * | 2018-08-13 | 2018-12-21 | 安吉艾格赛思生物科技有限公司 | A kind of agriculture and forestry organic waste material recycling efficient process technical matters |
-
2004
- 2004-09-20 CN CN200410064667.4A patent/CN1280313C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007128025A1 (en) * | 2006-05-10 | 2007-11-15 | Lenzing Aktiengesellschaft | Method for preparing xylooligosaccharides |
| CN104628890A (en) * | 2014-12-24 | 2015-05-20 | 山东龙力生物科技股份有限公司 | Energy-saving preparation method of low-ingredient xylo-oligosaccharide powder |
| CN107722136A (en) * | 2017-10-20 | 2018-02-23 | 中国林业科学研究院林产化学工业研究所 | A kind of beam system for certain degree of polymerization xylan method |
| CN109049234A (en) * | 2018-08-13 | 2018-12-21 | 安吉艾格赛思生物科技有限公司 | A kind of agriculture and forestry organic waste material recycling efficient process technical matters |
| CN109049234B (en) * | 2018-08-13 | 2021-06-11 | 安吉艾格赛思生物科技有限公司 | Agricultural and forestry waste recycling efficient treatment technology |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1280313C (en) | 2006-10-18 |
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