CN104278066A - Method for preparing wheat bran xylooligosaccharide by superpressure-enzyme combination process - Google Patents
Method for preparing wheat bran xylooligosaccharide by superpressure-enzyme combination process Download PDFInfo
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- CN104278066A CN104278066A CN201410496480.5A CN201410496480A CN104278066A CN 104278066 A CN104278066 A CN 104278066A CN 201410496480 A CN201410496480 A CN 201410496480A CN 104278066 A CN104278066 A CN 104278066A
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Abstract
The invention belongs to the field of resource development of subsidiary agricultural products, functional food additives and processing of nutrient health-care products, and particularly discloses a method for preparing wheat bran xylooligosaccharide by a superpressure-enzyme combination process. The method uses wheat bran as the raw material and is characterized by comprising the following steps: pulverizing and screening the wheat bran, adding water, carrying out ultrasonic treatment, carrying out composite enzyme treatment by using amylase, saccharifying enzyme and papain to obtain wheat bran dietary fiber, mixing the wheat bran dietary fiber and xylanase to carry out enzymolysis reaction under superpressure conditions, decolorizing the enzymolysis supernate, concentrating, and carrying out freeze-drying to obtain the xylooligosaccharide powder product. The method enhances the extraction rate of the wheat bran oligosaccharide, has the advantages of short time consumption and cost saving, and has great economic benefit.
Description
(1) technical field
The invention belongs to agricultural byproducts development of resources, functional food additives and dietary supplements manufacture field, particularly a kind of ultra-high voltage desmoenzyme legal system is for the method for Testa Tritici xylo-oligosaccharide.
(2) background technology
Testa Tritici is one of China's Three major grain crops, and containing important nutrition feature, total carbohydrates content is at about 45%-65%, and mainly cell wall polysaccharides, is also called non-starch polysaccharide.Cell wall polysaccharides forms primarily of piperylene, (1-3,1-4)-callose and Mierocrystalline cellulose.The content of piperylene in Testa Tritici is about 20%, is the good source preparing xylo-oligosaccharide (XOS).Functional XOS is the oligose be formed by connecting by β-(1-4) glycosidic link by 2-7 wood sugar, and its effective constituent is mainly xylo-bioses and xylotriose.Wherein the sugariness of xylo-bioses is 40% of sucrose, and content is that the sugariness of the XOS product of 50% is about 30% of sucrose, and taste is pure, similar sucrose.The structure of the oligose that the structure of Wheat Bran Pentosans complexity makes it decomposite is also complicated various, and then affects the functional performance of Testa Tritici oligose.Promote proliferation of probiotics, strengthen immunne response; The response to oxidative stress suppressing high lipid diet to cause, relaxes bowel, hypoglycemic; Antitumor; Anti-dental caries; Promote the absorption of the mineral elements such as magnesium, calcium, iron, zinc and some VITAMIN; Prevent diarrhoea, constipation, protection liver; At present, the research of the in-vitro multiplication effect that focuses mostly on to the research of Testa Tritici oligose functional performance, also has other functional performances many to require study discovery.
Traditional oligose extracts and is divided into following three kinds substantially: physical method (as hot water extraction), chemical process (as acid and alkali hydrolysis), biological process (i.e. enzyme process).Wherein physical method due to extraction efficiency low, energy expenditure is large, time long effort again; Acid hydrolysis process acid concentration is extremely difficult to be controlled, instrument very easily corrode by acid, basic hydrolysis extraction yield is high, but environmental pollution is serious; Production by Enzymes have technique power consumption less, the feature of green non-pollution gradually by vast enterprise and researcher admit, but single enzyme process Testa Tritici length consuming time, economic benefit is not high.So, work out a kind of short, environmental protection consuming time, the method preparing Testa Tritici oligose that target compound extraction yield is high is that pole has Social benefit and economic benefit.
China's Testa Tritici abundance, but due to many factors restriction, still fail so far to obtain abundant Appropriate application, major part is used as animal-feed.Meanwhile, the nutritive and health protection components of Testa Tritici and the active substance with outstanding physiological function are subject to the attention of domestic and international investigator in recent years, and relevant research is day by day deep.Therefore, accelerate the research and development of this resource, improve the utilization ratio of wheat Testa Tritici, utilize wheat bran more scientifically and rationally, enrich the kind of China's nutrition, protective foods, improve dietary nutrition and the health level of our people, improve the economic benefit of enterprise, tool is of great significance.
(3) summary of the invention
The present invention, in order to make up the deficiencies in the prior art, provides and a kind ofly pollutes the method for short, ultra-high voltage desmoenzyme legal system that extraction yield is high little, consuming time for Testa Tritici xylo-oligosaccharide.
The present invention is achieved through the following technical solutions:
A kind of ultra-high voltage desmoenzyme legal system is for the method for Testa Tritici xylo-oligosaccharide, take Testa Tritici as raw material, it is characterized in that: add water after being pulverized and sieved by Testa Tritici supersound process, employing amylase, saccharifying enzyme, papoid three kinds of prozyme process obtain wheat bran dietary fiber, under uht conditions, mixed with zytase by wheat bran dietary fiber and carry out enzyme digestion reaction, enzymolysis supernatant liquor, through decolouring, concentrated, lyophilize, prepares xylo-oligosaccharide powder product.
The present invention specifically comprises the steps:
(1) Testa Tritici is put into 80 DEG C of loft drier and be dried to constant weight, 20-40 eye mesh screen pulverized by pulverizer;
(2) in Testa Tritici powder, add water supersound process 20-30min, the weight ratio of Testa Tritici and water is 1:10-35;
(3) middle temperature amylase, saccharifying enzyme and papoid compound are added in the ultrasonic solution of Testa Tritici, enzymolysis 1-2h, temperature controls to control as 5.5-7.5 at 50-70 DEG C, pH, and the weight proportion of middle temperature amylase, saccharifying enzyme and papoid is 1.5-2.5:1.0-2.0:2.5-3.5:
(4) by enzymolysis solution through filter paper suction filtration, by drying treatment after distilled water washing and precipitating thing 4-6 time to constant weight, obtain wheat bran dietary fiber;
(5) wheat bran dietary fiber is mixed with the solid-liquid ratio of distilled water by 1g:15-35mL, regulate pH to 5-6, add zytase according to the ratio of 3.0-5.0g/L, under 150-350MPa pressure, react 10-30min immediately, temperature 35-55 DEG C, obtains turbid solution;
(6) go out turbid solution enzyme, and suction filtration gets filtrate, and by upper strata washing residue 5-6 time, merging filtrate carries out decolouring, concentrate, lyophilize, obtains product xylo-oligosaccharide powder.
More excellent technical scheme of the present invention is:
In step (3), the weight proportion of middle temperature amylase, saccharifying enzyme and papoid is 2:1:3.
In step (5), mixed by wheat bran dietary fiber with the solid-liquid ratio of distilled water by 1g:30mL, regulate pH to 5-6, add zytase according to the ratio of 4.0g/L, react 25min immediately under 250MPa pressure, temperature 40 DEG C, obtains turbid solution.
The Testa Tritici xylo-oligosaccharide content assaying method that the present invention obtains is HPLC.
Testa Tritici raw material of the present invention is easy to get, wide material sources, when utilizing the amylase of proportioning, saccharifying enzyme, protease composite enzyme hydrolyzed starch and protein, added saccharifying enzyme can will not be hydrolyzed or half starch be hydrolyzed, starch hydrolysate dextrin etc. further enzymolysis are water-soluble sugar, reach disposable thorough removal starch, used time 1.5h, remaining starch and protein content are respectively 0.2% and 4.5%; And utilize high temperature resistant ɑ-amylase and the Sumizyme MP of existing report process Testa Tritici respectively, used time 2.5h-3.5h, remaining starch and protein content are respectively 0.35% and 5.32%.Therefore, utilize three kinds of enzyme matching methods consuming time short, cost is less, and economic benefit improves.
When the present invention utilizes ultra-high voltage desmoenzyme legal system for wheat bran xylo-oligosaccharide, method is novel, and xylanase activity can be made to raise, and due to the raising of enzymic activity, enzymolysis time is decreased to 30min, and enzyme digestion reaction is thorough rapidly, and extraction rate reached is to 80%-85%.And the single enzyme solution of existing report, used time 12-24h, oligose extraction yield 50%-65%.Therefore, utilize ultra-high voltage to improve the extraction yield of wheat bran oligose in conjunction with enzyme process, consuming time short, provide cost savings, there is great economic benefit.
(4) accompanying drawing explanation
Below in conjunction with accompanying drawing, the present invention is further illustrated.
Fig. 1 is that liquid ratio of the present invention affects schematic diagram to wheat bran oligose extraction yield;
Fig. 2 is that enzyme concn of the present invention affects schematic diagram to wheat bran oligose extraction yield;
Fig. 3 is that pressure size of the present invention affects schematic diagram to wheat bran oligose extraction yield;
Fig. 4 is that temperature of the present invention affects schematic diagram to wheat bran oligose extraction yield;
Fig. 5 affects schematic diagram to wheat bran oligose extraction yield the ultra-high voltage lower time of the present invention;
Fig. 6 affects schematic diagram to wheat bran oligose extraction yield the normal pressure lower time of the present invention.
(5) embodiment
Below in conjunction with embodiment, method of the present invention is described further, but is not limited thereto.The Testa Tritici used in embodiment is provided by Shandong Feng Yu flour company limited, and non-starch polysaccharide content is about 30%.Various enzyme used provides by fermentation designing institute of Shandong Province, wherein amylase (3000U/g), saccharifying enzyme (1000U/g), proteolytic enzyme (1000U/g), zytase (10000U/g).
Embodiment 1:
(1) selection of best complex enzyme proportioning
Get 10g wheat bran, adding distil water 150mL, add amylase (1.5%-2.5%), saccharifying enzyme (1.0-2.0%), papoid (2.5%-3.5%) simultaneously, at 65 DEG C, pH is the Water Under solution 180min of 5.5, the residual quantity recording starch and albumen is respectively 0.2% and 4.5%, show that best complex enzyme proportioning is 2:1:3.
(2) ultra-high voltage is in conjunction with the selection of the best solid-liquid ratio of enzyme process
Due within the specific limits, concentration of substrate is larger, and more with the wheat bran amount of enzyme reaction in the unit time, namely enzyme ' s reaction speeding is faster, and when wheat bran amount is increased to a certain degree, rate is maximum, and extraction yield is the highest.As shown in Figure 1, under 200 MPa conditions, solid-liquid ratio is when 1:30 (g/mL) left and right, wheat bran oligose extraction yield is up to 83.8%, increase, extraction yield tends towards stability again, compare at ambient pressure, liquid ratio tends towards stability 81.9% at about 35:1 oligose extraction yield, more saves with water.
(3) ultra-high voltage is in conjunction with the selection of the best enzyme concn of enzyme process
From accompanying drawing 2, at 200MPa and at ambient pressure, when enzyme concn is at about 4.0g/L, oligose extraction rate reached, to maximum, is 83.4%, then increases enzyme amount content and also tend towards stability, but under 200MPa xylo-oligosaccharide extraction yield apparently higher than normal pressure.This impact due to high pressure treatments on enzyme activeness is mainly worked by the conformation and character that change enzyme and substrate, obviously under elevated pressure conditions enzyme and substrate reactions more thorough.
(4) ultra-high voltage is in conjunction with the selection of enzyme process optimum pressure condition
Solid-liquid ratio is 1:20 (g/mL), and enzyme concn is 3.5g/L, and temperature is 45 DEG C, and the time is 15min.
The chemical nature of most of enzyme is protein, show according to the study, the quaternary structure of protein maintained by hydrogen bond is to pressure and sensitivity thereof, the pressure of more than 200MPa can change tertiary protein structure, more than 700MPa can cause protein irreversible denaturation, therefore, the activity of enzyme will change along with the change of protein conformation.The effect of pressure to enzyme is dual, the activity of lower pressure (100-200MPa) meeting activating enzyme, the people such as Michael J summarize the activation research of high pressure to enzymic activity, and the activity of higher pressure (400-1000MPa) meeting inhibitory enzyme, raised temperature also effectively can accelerate the passivation of enzyme.Zhang Yu is studied with regard to the impact of ultra-high voltage on lipase activity, and show that uhp treatment lipase can make zymoprotein structure compacter, under high temperature, catalytic efficiency is higher.As shown in Figure 3, pressure difference will affect the extraction yield of wheat bran oligose, and reaching most high extraction at 250MPa, is 85.5%.This changes as catalytic site exposes because high pressure not only affects enzymatic structure, and it is loose that wheat bran structure is fluffed, and causes reaction more rapidly, thoroughly.Pressure size within the specific limits, has promoter action to reaction, and pressure is excessive, then can cause enzyme catalysis structural degeneration, enzyme event resolves.
(5) ultra-high voltage is in conjunction with the selection of enzyme process optimum temps
Temperature is one of important factor affecting enzymatic reaction, the too low enzymic activity of temperature is low, too high meeting sex change and inactivation, as shown in Figure 4, under 200MPa pressure, about 40 DEG C oligose extraction yields are 84.4% to the maximum, at ambient pressure, about 65 DEG C is best hydrolysis temperature, under under uht conditions, the optimum temperuture of zytase is less than normal pressure.This is because the inevitable heat effect in uhp treatment process causes, in pressurization, the heat of compression of water raises along with the rising of initial temperature, although pressure can be delivered evenly to food instantaneously, in the course of processing, inevitably produces thermograde.
(6) ultra-high voltage is in conjunction with the selection of enzyme process best dwell time
According to Le Chatelier's principle, pressurization can make reaction carry out to the direction of most compressed state, so pressure not only can affect the balance of reaction, also can affect the speed of reaction.Because wheat bran is " dead cell " structure, the cell walls of high fiber has concentrated a large amount of nutritive substances, consider enzymatic reaction, dwell time short reaction is insufficient, and time length can cause the waste of energy resource, as depicted in figures 5 and 6, under 200MPa, about 25min extraction yield is 83.2% to the maximum, and at ambient pressure, the time is that about 26h extraction rate reached is 82.2% to the maximum.
(7) preparation of wheat bran xylo-oligosaccharide powder
Above test draws the optimal treatment condition of ultra-high voltage in conjunction with enzyme process, then enzymolysis wheat-bran dietary fiber under the condition changing formula, solid-liquid ratio 1:30 (g/mL), enzyme concn 4.0g/L, pressure size 250MPa, pressurize temperature 40 DEG C, dwell time 25min.Under this Optimization Technology, the predictor of the extraction yield of Testa Tritici xylo-oligosaccharide is 85.21%, in proof test actual record Testa Tritici xylo-oligosaccharide extract yield be 85.46%.To be gone out enzyme by dirty solution after process, suction filtration gets filtrate, and by upper strata washing residue 5-6 time, merging filtrate carries out decolouring, concentrate, lyophilize obtains xylo-oligosaccharide powder.
Embodiment 2:
(1) pulverizer was dried to constant weight after pulverizing 40 eye mesh screens;
(2) get appropriate wheat bran adding distil water, wherein the weight ratio of Testa Tritici and water is 1:25.Add 2% amylase, 1% saccharifying enzyme, 3% papain enzymolysis wheat bran, at 65 DEG C, pH is the Water Under solution 180min of 5.5;
(3) after filter paper suction filtration, by drying treatment after distilled water washing and precipitating thing 3 times to constant weight, the wheat-bran dietary fiber containing 0.21% starch and 4.5% albumen is obtained;
(4) utilize ultra-high voltage in conjunction with the xylo-oligosaccharide in Enzymatic Extraction residue: to get wheat bran dietary fiber dry in step (3), add distilled water, control solid-liquid ratio at 1:30 (g/mL), zytase is added according to the ratio of 4.0g/L, 25min is reacted immediately under 250MPa pressure, pressurize temperature is 40 DEG C, and extraction yield is 84.67%;
(5) go out the dirty solution in step (4) enzyme, and suction filtration gets filtrate, and by upper strata washing residue 3 times, merging filtrate carries out decolouring, concentrate, lyophilize obtains xylo-oligosaccharide powder.
Claims (4)
1. a ultra-high voltage desmoenzyme legal system is for the method for Testa Tritici xylo-oligosaccharide, take Testa Tritici as raw material, it is characterized in that: add water after being pulverized and sieved by Testa Tritici supersound process, employing amylase, saccharifying enzyme, papoid three kinds of prozyme process obtain wheat bran dietary fiber, under uht conditions, mixed with zytase by wheat bran dietary fiber and carry out enzyme digestion reaction, enzymolysis supernatant liquor, through decolouring, concentrated, lyophilize, prepares xylo-oligosaccharide powder product.
2. ultra-high voltage desmoenzyme legal system according to claim 1 is for the method for Testa Tritici xylo-oligosaccharide, it is characterized by, and comprise the steps: that Testa Tritici is put into 80 DEG C of loft drier and is dried to constant weight by (1), 20-40 eye mesh screen pulverized by pulverizer; (2) in Testa Tritici powder, add water supersound process 20-30min, the weight ratio of Testa Tritici and water is 1:10-35; (3) middle temperature amylase, saccharifying enzyme and papoid compound are added in the ultrasonic solution of Testa Tritici, enzymolysis 1-2h, temperature controls at 50-70 DEG C, pH controls as 5.5-7.5, the weight proportion of middle temperature amylase, saccharifying enzyme and papoid is 1.5-2.5:1.0-2.0:2.5-3.5:(4) by enzymolysis solution through filter paper suction filtration, by distilled water washing and precipitating thing 4-6 rear drying treatment to constant weight, obtain wheat bran dietary fiber; (5) wheat bran dietary fiber is mixed with the solid-liquid ratio of distilled water by 1g:15-35mL, regulate pH to 5-6, add zytase according to the ratio of 3.0-5.0g/L, under 150-350MPa pressure, react 10-30min immediately, temperature 35-55 DEG C, obtains turbid solution; (6) go out turbid solution enzyme, and suction filtration gets filtrate, and by upper strata washing residue 5-6 time, merging filtrate carries out decolouring, concentrate, lyophilize, obtains product xylo-oligosaccharide powder.
3. ultra-high voltage desmoenzyme legal system according to claim 2 is for the method for Testa Tritici xylo-oligosaccharide, it is characterized in that: in step (3), and the weight proportion of middle temperature amylase, saccharifying enzyme and papoid is 2:1:3.
4. ultra-high voltage desmoenzyme legal system according to claim 3 is for the method for Testa Tritici xylo-oligosaccharide, it is characterized in that: in step (5), wheat bran dietary fiber is mixed with the solid-liquid ratio of distilled water by 1g:30mL, regulate pH to 5-6, zytase is added according to the ratio of 4.0g/L, under 250MPa pressure, react 25min immediately, temperature 40 DEG C, obtains turbid solution.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104894189A (en) * | 2015-07-06 | 2015-09-09 | 青岛嘉瑞生物技术有限公司 | Method for extracting xylooligosaccharide from wheat bran |
| CN104928331A (en) * | 2015-07-08 | 2015-09-23 | 青岛嘉瑞生物技术有限公司 | Technology for preparing functional xylo-oligosaccharide by comprehensively utilizing wheat straw |
| CN105795482A (en) * | 2016-03-29 | 2016-07-27 | 上海交通大学 | Water extraction method of highland barley dietary fibers by optimized by response surface method |
| CN105852140A (en) * | 2016-03-29 | 2016-08-17 | 上海交通大学 | Response surface method optimization of alkali extraction method of highland barley dietary fibers |
| CN106800609A (en) * | 2017-02-24 | 2017-06-06 | 天津挑战博德生物技术有限公司 | A kind of method that xylan is extracted from wheat bran |
| CN107988285A (en) * | 2018-01-03 | 2018-05-04 | 吉林农业大学 | A kind of method of super-pressure auxiliary preparing porous starch through enzyme method |
| CN107996967A (en) * | 2017-12-25 | 2018-05-08 | 广西兴业百谷米业有限公司 | A kind of processing of rice bran |
| CN109329730A (en) * | 2018-11-09 | 2019-02-15 | 想念食品股份有限公司 | Oat bran powder and preparation method, oat noodle and production method |
| CN109845958A (en) * | 2019-04-03 | 2019-06-07 | 沈阳师范大学 | A kind of wheat bran stabilizes and the method for quality improving |
| CN114557453A (en) * | 2022-01-25 | 2022-05-31 | 广东省农业科学院蚕业与农产品加工研究所 | Shaddock peel modified fiber and preparation method and application thereof |
| CN114847494A (en) * | 2022-04-20 | 2022-08-05 | 湖南农业大学 | Method for extracting dietary fiber from reed shoots |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104894189A (en) * | 2015-07-06 | 2015-09-09 | 青岛嘉瑞生物技术有限公司 | Method for extracting xylooligosaccharide from wheat bran |
| CN104928331A (en) * | 2015-07-08 | 2015-09-23 | 青岛嘉瑞生物技术有限公司 | Technology for preparing functional xylo-oligosaccharide by comprehensively utilizing wheat straw |
| CN105795482A (en) * | 2016-03-29 | 2016-07-27 | 上海交通大学 | Water extraction method of highland barley dietary fibers by optimized by response surface method |
| CN105852140A (en) * | 2016-03-29 | 2016-08-17 | 上海交通大学 | Response surface method optimization of alkali extraction method of highland barley dietary fibers |
| CN106800609A (en) * | 2017-02-24 | 2017-06-06 | 天津挑战博德生物技术有限公司 | A kind of method that xylan is extracted from wheat bran |
| CN106800609B (en) * | 2017-02-24 | 2019-08-27 | 天津挑战博德生物技术有限公司 | A method of extracting xylan from wheat bran |
| CN107996967A (en) * | 2017-12-25 | 2018-05-08 | 广西兴业百谷米业有限公司 | A kind of processing of rice bran |
| CN107988285A (en) * | 2018-01-03 | 2018-05-04 | 吉林农业大学 | A kind of method of super-pressure auxiliary preparing porous starch through enzyme method |
| CN109329730A (en) * | 2018-11-09 | 2019-02-15 | 想念食品股份有限公司 | Oat bran powder and preparation method, oat noodle and production method |
| CN109845958A (en) * | 2019-04-03 | 2019-06-07 | 沈阳师范大学 | A kind of wheat bran stabilizes and the method for quality improving |
| CN114557453A (en) * | 2022-01-25 | 2022-05-31 | 广东省农业科学院蚕业与农产品加工研究所 | Shaddock peel modified fiber and preparation method and application thereof |
| CN114847494A (en) * | 2022-04-20 | 2022-08-05 | 湖南农业大学 | Method for extracting dietary fiber from reed shoots |
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