CN101440109A - Method for preparation of functional low polyxylose alcohol - Google Patents
Method for preparation of functional low polyxylose alcohol Download PDFInfo
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- CN101440109A CN101440109A CNA2008102497475A CN200810249747A CN101440109A CN 101440109 A CN101440109 A CN 101440109A CN A2008102497475 A CNA2008102497475 A CN A2008102497475A CN 200810249747 A CN200810249747 A CN 200810249747A CN 101440109 A CN101440109 A CN 101440109A
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- xylo
- oligosaccharide
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- oligomerization
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- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims description 39
- 238000000034 method Methods 0.000 title abstract description 17
- 238000005984 hydrogenation reaction Methods 0.000 claims abstract description 19
- 239000012263 liquid product Substances 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 8
- HEBKCHPVOIAQTA-NGQZWQHPSA-N d-xylitol Chemical compound OC[C@H](O)C(O)[C@H](O)CO HEBKCHPVOIAQTA-NGQZWQHPSA-N 0.000 claims description 35
- 238000006243 chemical reaction Methods 0.000 claims description 34
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Abstract
The invention discloses a method for preparing functional oligomerization xylitol, which belongs to the technical field. The preparation method comprises that common oligomerization xylose is taken as a raw material; and under the action of a catalyst, by a hydrogenation reaction, the functional oligomerization xylitol is prepared. The method has the advantages of improving product physical-chemical property and guarantee period of the oligomerization xylose, modifying strengthened physiological function of a product structure functional group, and effectively improving poor conditions of the prior material oligomerization xylose, wherein the process equipment and technical line are relatively mature, and easy to operate; moreover, on the basis of keeping basic physiological properties of the prior oligomerization xylose, the prepared functional oligomerization xylitol has higher sugariness and more pure sweetness, and tastes soft, and the liquid product is transparent.
Description
Technical field
The present invention relates to a kind of preparation method of functional low polyxylose alcohol, belong to technological field of biochemistry.
Background technology
Oligose (Oligosaccharide) or title oligosaccharides, it is a kind of efficient bifidus factor, it also is a kind of food fibre, it is the oligose that is connected to form straight or branched by 2-10 monose by glycosidic link, functional oligose has characteristic, physiologically active and the nourishing function of many excellences, is widely used as fields such as healthcare products, medicine, food, agricultural.Abroad, people are in great demand to the functional oligose series products that integrates " nutrition, health care ".The widespread use exploitation of oligose is to raising people's immunizing power, and prevention and inhibition hyperlipidemia, diabetes, obesity and relative disease particularly to the propagation bifidus bacillus, are optimized the interior microecological balance of body and played an important role.Use more oligose at present and mainly contain oligofructose, oligomeric isomaltose, xylo-oligosaccharide etc.
Xylo-oligosaccharide (xylo-oligosaccharide) is with β-1 by 2-7 D-xylose residues, 4 glycosidic links in conjunction with and the oligose that constitutes, be to be rich in the plant resources of xylan, adopt the degraded of dilute acid hydrolysis or microbial transformation extraction or high pressure, biological enzyme (zytase) catalyzed conversion to decompose a kind of oligose that hemicellulose is produced from corn cob, cotton seed hull, bagasse etc.It has the high efficiently multiplying bifidus bacillus, effective intake few (only needing 0.7g～1.4g that unusual effect is just arranged for each person every day), and good acid heat stability (pH2.5-8.0 heating 1h does not down have considerable change) is not absorbed by human consumption, and good compatibleness is arranged.Therefore, more and more be subjected to the favor of vast food, healthcare products, functional feed healthcare products, medical research unit and production firm.
At present, the xylo-oligosaccharide product that the whole bag of tricks is produced, particularly liquid product is because also there is the decolouring technology problem in the problem of technology, it is yellow or light yellow transparent liquid that target level of product quality is set outward appearance, but color and luster is subjected to shelf-time and Temperature Influence and progressively deepens, cause liquid product need improve storage environment requirement (0-4 ℃ of following low temperature seal preserved 18 months), if normal temperature is deposited the goods he phase and can relatively be lacked (6 months); Also remain with the corn peculiar taste in the product, indivedual crowds have unconformable phenomenon; On using, there is sugariness problem on the low side, is about 40% of sucrose.In the product that has sugariness to require, also need to add in addition sweeting agent and replenish sugariness.And powder product has extremely strong water absorbability, need in selection, environment for use and the operating process of wrapping material, note the control of ambient moisture, improper as moisture preventive measure, the phenomenon that moisture absorption is united and lumpd appears in exposing process to the open air easily, this causes unfavorable factor also for the Application and Development of xylo-oligosaccharide terminal consumption product, particularly in the solid preparation production technique in the process for processing as capsule, tablet or powder product.
Summary of the invention
The objective of the invention is to overcome the prior art deficiency, utilize the distinctive chemical structure of xylo-oligosaccharide reaches provides a kind of functional low polyxylose alcohol with the biological nature of structurally associated preparation method simultaneously.The low polyxylose alcohol that utilizes this method production is on the basis of having preserved original xylo-oligosaccharide basic physiological characteristic, and sugariness obviously improves, and sweet taste is pure, and soft mouth feel, liquid product are the water white transparency shape, and the quality guaranteed period can be increased to more than 24 months.
The present invention's technical scheme of being taked of dealing with problems is: a kind of preparation method of functional low polyxylose alcohol, it is characterized in that, it is a raw material with common xylo-oligosaccharide, may further comprise the steps: 1) utilizing solid content is 5%～60% xylo-oligosaccharide solution, add the catalyzer that accounts for xylo-oligosaccharide solid quality 1%～15%, the conditioned reaction system pH is squeezed into the hydrogenation still in the 4.0-9.0 scope jointly with it; 2) logical High Purity Hydrogen in the hydrogenation still, reaction system is warming up to 60 ℃, hydrogenation begins, and stops heating when temperature rises to 90 ℃～125 ℃, reaction pressure remains in the 7Mpa-12Mpa scope, reaction time 20min～120min; 3) the reducing sugar quality accounts for 0.2% of total reducing sugar and finishes reaction when following in the reaction system, with nitrogen that the hydrogen exchange of remnants is clean, blowing, sedimentation then, again to feed liquid decolour, ion-exchange, concentrate the low polyxylose alcohol liquid product, or carry out drying treatment and get solid phase prod.
The further technical scheme of the present invention is: a kind of preparation method of functional low polyxylose alcohol, it is characterized in that, it is raw material with the xylo-oligosaccharide, may further comprise the steps: 1) utilizing solid content is 30%～50% xylo-oligosaccharide solution, add the catalyzer that accounts for xylo-oligosaccharide solid quality 7%～9%, the conditioned reaction system pH is squeezed into the hydrogenation still in the 6.5-8.5 scope jointly with it; 2) logical High Purity Hydrogen in the hydrogenation still, reaction system is warming up to 60 ℃, hydrogenation begins, and stops heating when temperature rises to 90 ℃～110 ℃, reaction pressure remains in the 9Mpa-11Mpa scope, reaction time 30min～50min; 3) the reducing sugar quality accounts for 0.2% of total reducing sugar and finishes reaction when following in the reaction system, with nitrogen that the hydrogen exchange of remnants is clean, blowing, sedimentation then, again to feed liquid decolour, ion-exchange, concentrate the low polyxylose alcohol liquid product, or carry out drying treatment and get solid phase prod.
The invention has the beneficial effects as follows:
Method of the present invention can effectively promote product physico-chemical property, quality guaranteed period and the modified product structure function group of raw material xylo-oligosaccharide and strengthen physiological function, and processing unit and technological line all are comparative maturities, operation easily, especially to having the manufacturer of hydrogenation apparatus, do not need additionally to add equipment, only need the change processing parameter just can produce, help the production and the popularization of product of the present invention.
The functional low polyxylose alcohol that the method for the invention makes has following physico-chemical property: sweet taste character is similar with sucrose to honey, sugariness is according to the variation of sugar concentration, the 80%-120% that is about sucrose, local flavor is pure, soft mouth feel, liquid product is the water white transparency shape, and the quality guaranteed period can be increased to more than 24 months; Has the acidproof heat-proof performance, even do not have considerable change at the following 80 ℃ of heating 1h of acidic conditions (pH3.0-8.0); Have indigestibility, very stable in Digestive systems such as saliva, gastric juice, pancreatic juice, intestinal juice; Chemical property is stable, is difficult to react with other material.And the hygroscopic property of powder product is also effectively reduced.
The functional low polyxylose alcohol that the method for the invention makes has following physiological function, comprising: 1. suppress pathogeny bacterium diarrhoea.But low polyxylose alcohol high efficiently multiplying bifidus bacillus, other harmful bacterium is played restraining effect, in addition, low polyxylose alcohol has stronger adsorptive power to pathogenic bacteria, as intestinal bacteria, enteritis door Salmonella etc., because low polyxylose alcohol is not degraded by the digestive ferment in the enteron aisle, the pathogenic bacteria that portability adheres to excretes by enteron aisle, thereby ward off disease cluster in enteron aisle, reach and prevent the purpose of suffering from diarrhoea; 2. prevent constipation.Bifidus bacillus utilizes low polyxylose alcohol, produces a large amount of short chain fatty acids; Can stimulate intestines peristalsis, increase the ight soil wettability, and keep certain osmotic pressure, thereby prevent that constipation from taking place; 3. protect liver function.Low polyxylose alcohol can promote liver glycogen synthetic, and blood sugar can not rise, and the liver problem sufferer is had the liver function of improvement and lipotropic effect, treats B-mode chronic persistent hepatitis, and chronic hepatitis B and liver cirrhosis have obvious curative effects, are hepatitis concurrent disease patient's desirable auxiliarys.4. take in low polyxylose alcohol, can reduce the toxic metabolite product and form, significantly reduced the burden that liver divides toxolysin; 5. bring high blood pressure down.Studies show that the ratio that bifidus bacillus in height that a people's diastole presses and its ight soil accounts for total count is tangible negative correlativing relation, and low polyxylose alcohol can be good at breeding the quantity of bifidus bacillus in the enteron aisle, and Hypertensive Population is had good adjuvant treatment effect; 6. can enhancing body immunizing power, anticancer.Show that through a large amount of test-results bifidus bacillus a large amount of breedings in enteron aisle can be played antitumous effect.This antitumous effect is given the credit to cell, cell wall constituent and the exocytosis thing of bifidus bacillus, and immunity of organisms is improved; 7. prevention of dental caries.Low polyxylose alcohol is unique polyol, and it can forbid individually that the streptococcus mutant xenogeneic increases, thereby alleviates the infection rate of carious tooth.At first be low polyxylose alcohol can not be produced carious tooth in the oral cavity fermentation using bacteria utilization, suppress the generation of streptococcus growth and acid; Secondly it can promote salivation, slows down the pH value and descends, and has reduced the acid etching of tooth, prevents the generation of carious tooth and minimizing dental plaque, consolidates and promote repairing naturally of tooth.8. do not increase blood sugar concentration.Low polyxylose alcohol does not rely on Regular Insulin, and rising the blood index is zero, is that the diabetics is suitable for functional Sugar Alcohol.9. has excellent compatibility.Add a small amount of low polyxylose alcohol in the food, just can embody health-care effect, when low polyxylose alcohol and calcium are taken in simultaneously, it not only can not influence the absorption of body to calcium, can play a driving role on the contrary, test-results shows, absorbs 2～3% xylo-oligosaccharide alcohol solutions arbitrarily, and body has improved 15～30% to the retention rate of calcium after 7 days.10. have anti-body oxidation, keep the effect of the young attitude of enteron aisle.
The functional low polyxylose alcohol that what is more important the method for the invention makes has kept the original unique physiology characteristic of xylo-oligosaccharide fully: be difficult for being digested and assimilated in human intestinal, arrive large intestine and utilized, have significant bifidus bacillus multiplication capacity by bifidus bacillus.Effectively intake is few, only needs every day just can play the effect of propagation bifidus bacillus, effectively the relief of constipation symptom about oral 1g.Low polyxylose alcohol can not be become monose such as glucose, the fructose etc. of tackyness equally by bacterial degradation such as Streptococcus mutans in the oral cavity, can stop sucrose to be generated tartar with sucrose and time spent, so no carious tooth and tool anti-dental caries; Can promote the receipts of body to calcium; Can reduce serum cholesterol and content of triglyceride, can not cause after the absorption that blood glucose value raises in the body.So low polyxylose alcohol can be made the desirable feedstock of patients' such as old age, children and pregnant woman, hypertension, diabetes, obesity functional food additives.
The functional low polyxylose alcohol that the method for the invention makes is applied to the growth immunomodulatory of varieties of food items, healthcare products, medicine and plant as food ingredients or effective component.Particularly at the product of intestinal health as in the products such as treatment constipation, bacterial diarrhea; Also can add be used for toxin-expelling and face nourishing, the absorption that has additional nutrients, healthy products such as build up resistance.Because the low polyxylose alcohol physico-chemical property is stable, difficult and other material reacts, and can directly add in the product, and not need to change original operational path, only need add according to recommended amounts and nourishing function to get final product.
The use-case of product has:
Example 1, ten thousand certain, 35 years old, be hyperlipemic patients, serum total cholesterol (TC) content TC〉5.7mmoL/L (220mg/d1), take functional low polyxylose alcohol that the inventive method makes after 4 weeks, the total serum cholesterol can reduce 30d1, the diastole drops 5mmHg.
Example 2, in certain, 28 years old, the woman, 70 kilograms of body weight have regular constipation symptom, take functional low polyxylose alcohol that the inventive method makes after 2 weeks, and it is normal that stool is tending towards, and body weight has also reduced 2 kilograms.
Embodiment
Embodiment 1
The refractive power of getting the public offering that Shandong Longli Biology Science and Technology Co., Ltd produces is 70.8% xylo-oligosaccharide slurry (xylo-oligosaccharide account for total reducing sugar ratio 70%) 0.90kg, add pure water solid content is transferred to 16%, add Raney's nickel catalyst 57g, stir, use sheet alkali NaOH adjust pH to 7.2 again, open reactor, the xylo-oligosaccharide solution that mixes up is poured in the still, close kettle cover, with air and pressure testing in the nitrogen replacement still, feed hydrogen more earlier, begin heating, pressure is transferred to 12MPa pays close attention to pressure in whole hydrogenation process variation, according to the carrying out of reaction, timely supplementary pressure, when temperature rises to 70 ℃, the reaction beginning stops heating when temperature rises to 125 ℃, the beginning heat-insulation pressure keeping, pick up counting, 20min detects DE value 0.18%; 30min detects DE value 0.075%; Reaction finishes.The beginning discharging.After the discharging, refractive power 16.3%, the DE value is 0.075%.Material is decoloured, handles, concentrates from handing over or the dry low polyxylose alcohol liquid or solid product that gets.
Embodiment 2
The refractive power of getting the public offering that Shandong Longli Biology Science and Technology Co., Ltd produces is 70.5% xylo-oligosaccharide slurry (xylo-oligosaccharide account for total reducing sugar ratio 70%) 3.0kg, add pure water solid content water is transferred to 53%, add Raney's nickel catalyst 253g, stir, use sheet alkali NaOH adjust pH to 8.0 again, open reactor, the xylo-oligosaccharide solution that mixes up is poured in the still, close kettle cover, with air and pressure testing in the nitrogen replacement still, feed hydrogen more earlier, begin heating, pressure is transferred to 11MPa pays close attention to pressure in whole hydrogenation process variation, according to the carrying out of reaction, timely supplementary pressure, when temperature rises to 70 ℃, the reaction beginning stops heating when temperature rises to 110 ℃, the beginning heat-insulation pressure keeping, pick up counting, 20min detects DE value 0.73%; 30min detects DE value 0.40%; 40min detects DE value 0.21; 50min detects DE value 0.086%; Reaction finishes.The beginning discharging, after the discharging, refractive power 53%, the DE value is 0.086%.To material decolour, from handing over, concentrate or dry low polyxylose alcohol liquid or solid product.
Embodiment 3
The refractive power of getting the public offering that Shandong Longli Biology Science and Technology Co., Ltd produces is 70.5% xylo-oligosaccharide slurry (xylo-oligosaccharide account for total reducing sugar ratio 70%) 2.5kg, add pure water solid content water is transferred to 45%, add Raney's nickel catalyst 123.5g, stir, use sheet alkali NaOH adjust pH to 7.9 again, open reactor, the xylo-oligosaccharide solution that mixes up is poured in the still, close kettle cover, with air and pressure testing in the nitrogen replacement still, feed hydrogen more earlier, begin heating, pressure is transferred to 9MPa pays close attention to pressure in whole hydrogenation process variation, according to the carrying out of reaction, timely supplementary pressure, when temperature rises to 70 ℃, the reaction beginning stops heating when temperature rises to 100 ℃, the beginning heat-insulation pressure keeping, pick up counting, 20min detects DE value 0.36%; 30min detects DE value 0.12%; 40min detects DE value 0.085; Reaction finishes.The beginning discharging, after the discharging, refractive power 45.2%, the DE value is 0.085%.To material decolour, from handing over, concentrate or dry low polyxylose alcohol liquid or solid product.
Embodiment 4
The refractive power of getting the public offering that Shandong Longli Biology Science and Technology Co., Ltd produces is 71% xylo-oligosaccharide slurry (xylo-oligosaccharide account for total reducing sugar ratio 95%) 2.5kg, add pure water solid content water is transferred to 35%, add Raney's nickel catalyst 125g, stir, use sheet alkali NaOH adjust pH to 7.8 again, open reactor, the xylo-oligosaccharide solution that mixes up is poured in the still, close kettle cover, with air and pressure testing in the nitrogen replacement still, feed hydrogen more earlier, begin heating, pressure is transferred to 9MPa pays close attention to pressure in whole hydrogenation process variation, according to the carrying out of reaction, timely supplementary pressure, when temperature rises to 70 ℃, the reaction beginning stops heating when temperature rises to 100 ℃, the beginning heat-insulation pressure keeping, pick up counting, 20min detects DE value 0.37%; 30min detects DE value 0.14%; 50min detects DE value 0.056; Reaction finishes.The beginning discharging, after the discharging, refractive power 45.2%, the DE value is 0.055%.To material decolour, from handing over, concentrate or dry low polyxylose alcohol liquid or solid product.
Conclusion:
In this test first three case raw materials used be same raw material, each component is tested with HPLC, three embodiment product HPLC test results such as table 1:
Table 1
Embodiment 4 test result such as tables 2:
From the data that detect as can be seen, when temperature reached 125 ℃, certain decomposition took place in the component of xylo-oligosaccharide, and Xylitol content obviously increases, and this might reduce the cultivation effect of product to bifidus bacillus, this be we do not want to see.And each component all changes not quite in scheme 2, scheme 3 and the scheme 4.We wish few variation that influences component of trying one's best in the process of hydrogenation, oligomeric part content ratio is high more, because the influence that viscosity increases, material reaction concentration should suitably be lowerd, show that according to the correlative study data xylo-bioses is best to the cultivation effect of bifidus bacillus, thereby, we wish in the product that with the master that increases to of xylo-bioses alkoxide component, Xylitol content preferably remains unchanged or reduces.
Claims (2)
1, a kind of preparation method of functional low polyxylose alcohol, it is characterized in that, it is a raw material with common xylo-oligosaccharide, may further comprise the steps: 1) utilizing solid content is 5%～60% xylo-oligosaccharide solution, add the catalyzer that accounts for xylo-oligosaccharide solid quality 1%～15%, the conditioned reaction system pH is squeezed into the hydrogenation still in the 4.0-9.0 scope jointly with it; 2) logical High Purity Hydrogen in the hydrogenation still, reaction system is warming up to 60 ℃, hydrogenation begins, and stops heating when temperature rises to 90 ℃～125 ℃, reaction pressure remains in the 7Mpa-12Mpa scope, reaction time 20min～120min; 3) the reducing sugar quality accounts for 0.2% of total reducing sugar and finishes reaction when following in the reaction system, with nitrogen that the hydrogen exchange of remnants is clean, blowing, sedimentation then, again to feed liquid decolour, ion-exchange, concentrate the low polyxylose alcohol liquid product, or carry out drying treatment and get solid phase prod.
2, a kind of preparation method of functional low polyxylose alcohol, it is characterized in that, it is raw material with the xylo-oligosaccharide, may further comprise the steps: 1) utilizing solid content is 30%～50% xylo-oligosaccharide solution, add the catalyzer that accounts for xylo-oligosaccharide solid quality 7%～9%, the conditioned reaction system pH is squeezed into the hydrogenation still in the 6.5-8.5 scope jointly with it; 2) logical High Purity Hydrogen in the hydrogenation still, reaction system is warming up to 60 ℃, hydrogenation begins, and stops heating when temperature rises to 90 ℃～110 ℃, reaction pressure remains in the 9Mpa-11Mpa scope, reaction time 30min～50min; 3) the reducing sugar quality accounts for 0.2% of total reducing sugar and finishes reaction when following in the reaction system, with nitrogen that the hydrogen exchange of remnants is clean, blowing, sedimentation then, again to feed liquid decolour, ion-exchange, concentrate the low polyxylose alcohol liquid product, or carry out drying treatment and get solid phase prod.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101904484A (en) * | 2010-09-10 | 2010-12-08 | 山东福田药业有限公司 | Method for preparing liquid xylitol with xylitol purity of 50 percent |
| US10759727B2 (en) | 2016-02-19 | 2020-09-01 | Intercontinental Great Brands Llc | Processes to create multiple value streams from biomass sources |
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| BR0301678A (en) * | 2003-06-10 | 2005-03-22 | Getec Guanabara Quimica Ind S | Process for the production of crystalline xylose from sugarcane bagasse, high purity crystalline xylose produced by said process, process for the production of crystalline xylitol from the high purity crystalline xylose and thus obtained |
| CN1850833A (en) * | 2006-05-22 | 2006-10-25 | 夏云丽 | Method for preparing xylosic alcohol using corn core |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101904484A (en) * | 2010-09-10 | 2010-12-08 | 山东福田药业有限公司 | Method for preparing liquid xylitol with xylitol purity of 50 percent |
| CN101904484B (en) * | 2010-09-10 | 2012-11-28 | 山东福田药业有限公司 | Method for preparing liquid xylitol with xylitol purity of 50 percent |
| US10759727B2 (en) | 2016-02-19 | 2020-09-01 | Intercontinental Great Brands Llc | Processes to create multiple value streams from biomass sources |
| US11840500B2 (en) | 2016-02-19 | 2023-12-12 | Intercontinental Great Brands Llc | Processes to create multiple value streams from biomass sources |
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