CN105361187A - Modified cereal dietary fiber and preparation method thereof - Google Patents
Modified cereal dietary fiber and preparation method thereof Download PDFInfo
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- CN105361187A CN105361187A CN201510629161.1A CN201510629161A CN105361187A CN 105361187 A CN105361187 A CN 105361187A CN 201510629161 A CN201510629161 A CN 201510629161A CN 105361187 A CN105361187 A CN 105361187A
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- 235000013325 dietary fiber Nutrition 0.000 title claims abstract description 120
- 235000013339 cereals Nutrition 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 36
- 229940088598 enzyme Drugs 0.000 claims abstract description 35
- 230000004048 modification Effects 0.000 claims abstract description 32
- 238000012986 modification Methods 0.000 claims abstract description 32
- 108090000790 Enzymes Proteins 0.000 claims abstract description 20
- 102000004190 Enzymes Human genes 0.000 claims abstract description 20
- 108010059892 Cellulase Proteins 0.000 claims abstract description 18
- 229940106157 cellulase Drugs 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 238000012545 processing Methods 0.000 claims abstract description 7
- 238000000926 separation method Methods 0.000 claims abstract description 6
- 238000000498 ball milling Methods 0.000 claims abstract description 5
- 238000007670 refining Methods 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 29
- 239000002131 composite material Substances 0.000 claims description 23
- 235000005911 diet Nutrition 0.000 claims description 23
- 230000000378 dietary effect Effects 0.000 claims description 23
- 230000009144 enzymatic modification Effects 0.000 claims description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 235000007164 Oryza sativa Nutrition 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 235000009566 rice Nutrition 0.000 claims description 14
- 239000013049 sediment Substances 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 13
- 238000005119 centrifugation Methods 0.000 claims description 12
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 11
- 238000000605 extraction Methods 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 8
- 238000010298 pulverizing process Methods 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- 238000005238 degreasing Methods 0.000 claims description 7
- 244000046052 Phaseolus vulgaris Species 0.000 claims description 6
- 235000010627 Phaseolus vulgaris Nutrition 0.000 claims description 6
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical group O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 230000001376 precipitating effect Effects 0.000 claims description 6
- 238000002203 pretreatment Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- 235000015112 vegetable and seed oil Nutrition 0.000 claims description 5
- 239000008158 vegetable oil Substances 0.000 claims description 5
- 239000004382 Amylase Substances 0.000 claims description 4
- 102000013142 Amylases Human genes 0.000 claims description 4
- 108010065511 Amylases Proteins 0.000 claims description 4
- 239000004365 Protease Substances 0.000 claims description 4
- 240000008042 Zea mays Species 0.000 claims description 4
- 235000016383 Zea mays subsp huehuetenangensis Nutrition 0.000 claims description 4
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims description 4
- 235000019418 amylase Nutrition 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 235000009973 maize Nutrition 0.000 claims description 4
- 239000002893 slag Substances 0.000 claims description 4
- 235000015099 wheat brans Nutrition 0.000 claims description 4
- 108090000526 Papain Proteins 0.000 claims description 3
- 238000006911 enzymatic reaction Methods 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 229940055729 papain Drugs 0.000 claims description 3
- 235000019834 papain Nutrition 0.000 claims description 3
- 238000001556 precipitation Methods 0.000 claims description 3
- 238000012216 screening Methods 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 206010013786 Dry skin Diseases 0.000 claims description 2
- 239000012141 concentrate Substances 0.000 claims description 2
- 240000007594 Oryza sativa Species 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 15
- 239000010903 husk Substances 0.000 abstract description 3
- 101710121765 Endo-1,4-beta-xylanase Proteins 0.000 abstract description 2
- 239000006227 byproduct Substances 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- 239000002245 particle Substances 0.000 abstract description 2
- 238000002715 modification method Methods 0.000 abstract 4
- 150000001875 compounds Chemical class 0.000 abstract 1
- 230000003247 decreasing effect Effects 0.000 abstract 1
- 235000013305 food Nutrition 0.000 abstract 1
- 238000010187 selection method Methods 0.000 abstract 1
- HVYWMOMLDIMFJA-DPAQBDIFSA-N cholesterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 HVYWMOMLDIMFJA-DPAQBDIFSA-N 0.000 description 14
- 241000209094 Oryza Species 0.000 description 13
- 230000003321 amplification Effects 0.000 description 10
- 238000003199 nucleic acid amplification method Methods 0.000 description 10
- 229920005610 lignin Polymers 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- 238000010521 absorption reaction Methods 0.000 description 7
- 235000012000 cholesterol Nutrition 0.000 description 7
- 229920002678 cellulose Polymers 0.000 description 6
- 239000001913 cellulose Substances 0.000 description 6
- 229920002488 Hemicellulose Polymers 0.000 description 5
- 238000009413 insulation Methods 0.000 description 5
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 4
- 230000014759 maintenance of location Effects 0.000 description 4
- 239000006228 supernatant Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- 229920002472 Starch Polymers 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- 239000012634 fragment Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 235000019698 starch Nutrition 0.000 description 3
- 239000008107 starch Substances 0.000 description 3
- 235000019483 Peanut oil Nutrition 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 238000005422 blasting Methods 0.000 description 2
- 239000008280 blood Substances 0.000 description 2
- 210000004369 blood Anatomy 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000004128 high performance liquid chromatography Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000312 peanut oil Substances 0.000 description 2
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000012798 spherical particle Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 206010010774 Constipation Diseases 0.000 description 1
- 102000002322 Egg Proteins Human genes 0.000 description 1
- 108010000912 Egg Proteins Proteins 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- 108091005804 Peptidases Proteins 0.000 description 1
- 102100037486 Reverse transcriptase/ribonuclease H Human genes 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 235000010716 Vigna mungo Nutrition 0.000 description 1
- 240000004922 Vigna radiata Species 0.000 description 1
- 235000010721 Vigna radiata var radiata Nutrition 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000011088 calibration curve Methods 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 238000000205 computational method Methods 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 235000013345 egg yolk Nutrition 0.000 description 1
- 210000002969 egg yolk Anatomy 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000002389 environmental scanning electron microscopy Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 150000002333 glycines Chemical class 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000002218 hypoglycaemic effect Effects 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 239000002504 physiological saline solution Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 235000019419 proteases Nutrition 0.000 description 1
- 235000018102 proteins Nutrition 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000002040 relaxant effect Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000036186 satiety Effects 0.000 description 1
- 235000019627 satiety Nutrition 0.000 description 1
- JAJWGJBVLPIOOH-IZYKLYLVSA-M sodium taurocholate Chemical compound [Na+].C([C@H]1C[C@H]2O)[C@H](O)CC[C@]1(C)[C@@H]1[C@@H]2[C@@H]2CC[C@H]([C@@H](CCC(=O)NCCS([O-])(=O)=O)C)[C@@]2(C)[C@@H](O)C1 JAJWGJBVLPIOOH-IZYKLYLVSA-M 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
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- 238000004544 sputter deposition Methods 0.000 description 1
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- 229920001221 xylan Polymers 0.000 description 1
- 150000004823 xylans Chemical class 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
Abstract
The invention belongs to the technical field of deep processing of cereal byproducts, and particularly relates to modified cereal dietary fiber and a preparation method thereof. The preparation method comprises the steps that cereal husk residues serve as the raw material, dietary fiber is extracted after pretreatment and separation are conducted, and the modified dietary fiber is obtained through a bi-enzyme modification method and an enzyme and ball-milling modification method; high dietary fiber food is obtained by taking the modified dietary fiber as the raw material. The modified cereal dietary fiber and the preparation method thereof are characterized in that a modification treatment technology of the dietary fiber is provided, optimal selection methods comprise the bi-enzyme modification method and the enzyme and ball-milling modification method, water-insoluble dietary fiber is obtained through modification, and water-soluble dietary fiber and the water-insoluble dietary fiber are obtained through refining and drying. According to the modified cereal dietary fiber and the preparation method thereof, cellulase and xylanase are simultaneously utilized to conduct enzymolysis on the cereal dietary fiber, and the content of the water-insoluble dietary fiber in the cereal dietary fiber is significantly increased; the particle size of the cereal dietary fiber is decreased through a mechanical force-enzyme method, the specific surface area is increased, and the enzymolysis effect of compound enzyme on the dietary fiber is improved.
Description
Technical field
The invention belongs to grain processing and utilize technical field.Be specifically related to a kind of modification grain dietary fiber and preparation method.The present invention for raw material, obtains water-soluble dietary fiber product and water insoluble dietary fiber product and preparation method thereof by suitably processing with cereal processing byproduct.
Background technology
Rice bran, wheat bran, maize peel and beans skin slag etc. are the accessory substances of cereal processing, and dietary fiber content enriches, and having and increase satiety, Constipation, hypoglycemic, reducing blood lipid and the effect such as anticancer, is important dietary fiber sources.It is generally acknowledged, the viscosity of water-soluble dietary fiber (SDF) is higher, has reduction blood glucose response, reduces the functional characteristics such as cholesterolemia.But the SDF content of natural grain dietary fiber lower (≤3%).Chinese invention patent publication number is that the document of CN101564132A carries out modification by tight-face blasting technique to bean dregs dietary fiber, improve the content of SDF in bean dregs, but the starch needing high level in dietary fiber just can reach good tight-face blasting effect, thus causing the concentration of dietary fiber lower, effect is not obvious.Publication number is that the document of CN101785831A is by adding the content of SDF in cellulase raising rice bran dietary fiber, and in grain dietary fiber, cellulosic crystal region, and the binder course of hemicellulose and lignin formation is tightly wrapped in cellulose, all hinders enzyme to cellulosic effect.Publication number is that the document of CN102940262A is by successively adding the work of cellulase and 'beta '-mannase in order to improve the content of SDF in bean dregs, two enzyme successively effect can destroy the structure of combining closely between dietary fiber component, improve the modified effect to dietary fiber, but the method for this stepwise discretization is consuming time longer, and transformation efficiency is lower.Mechanical force can destroy cellulose, structure closely between hemicellulose and lignin, increases the specific area of dietary fiber, makes complex enzyme more abundant to the effect of substrate, the modified effect of raising cellulase and zytase.
Summary of the invention
The object of the invention is to the defect overcoming prior art, a kind of modification grain dietary fiber and preparation method thereof is provided.The present invention, by the enzymolysis of mechanical external force assisted recombination enzyme (such as cellulase and zytase), improves the modified effect to grain dietary fiber.
Realize concrete technical scheme of the present invention as follows:
One utilizes mechanical force-complex enzyme reaction to prepare the method for modified dietary fiber, the accessory substance rice bran being rich in dietary fiber produced with process of grain processing, wheat bran, maize peel and beans skin slag are for raw material, through pre-treatment, separation and Extraction, modifiedly obtain modification composite dietary, then obtain water-soluble and water-insoluble grain dietary fiber through steps such as refining, concentrate dryings; Preparation process is as follows:
(1) pre-treatment: by raw material screening, removal of impurities, pulverize after cross 60 order-80 mesh sieves, be then placed in 5-10 times of volume vegetable oil extraction solvent stir soak 1-3h, centrifugation, by air-dry for precipitation deviate from solvent, obtain degreasing material;
(2) separation and Extraction: mass fraction degreasing material being dipped in 8-12 times of volume is in the NaOH solution of 0.3%-0.6%, stir after soaking 2-4h, centrifugation, get lower sediment, add in the water of 2-5 times of volume, by HCl adjust ph to 5-7, the papain adding 1000u/g-4000u/g is at 30 DEG C-50 DEG C after stirring reaction 10min-30min, add the amylase of 100u/g-500u/g, stirring reaction 10min-35min at 40 DEG C-90 DEG C, be heated to the 10min that seethes with excitement again, then centrifugation, by water washing and precipitating 3-5 time, get lower sediment, obtain unmodified dietary fiber slip for subsequent use, or obtain unmodified composite dietary by after the unmodified dietary fiber slip drying of gained,
(3) modification:, the pH value unmodified dietary fiber slip being dipped in 2-5 times of volume is in the 0.08mol/L-0.1mol/L citric acid solution of 4-6, add 0.5u/g-5.0u/g cellulase and 40u/g-200u/g zytase, after mixing in ball mill, ball-milling medium is zirconia, filling rate 60%-80%, radius 0.6-0.8mm, rotating speed 300-800r/min, griding reaction 2-4h at 40 DEG C-60 DEG C; Or with abrasive disc formula fiberizer, rotating speed 2000-3000r/min, griding reaction 1 ~ 2h at 30 DEG C-55 DEG C, obtain the dietary fiber slip of mechanical force-complex enzyme modification after filtration, slip is dry, obtain the composite dietary of mechanical force-complex enzyme modification;
(4) refining: by the dietary fiber slip of mechanical force-complex enzyme modification in about 100 DEG C heating 5-20min, centrifugation, by hot water washing and precipitating 2-5 time of 60 DEG C-70 DEG C, collects liquid (a) and sediment (b) respectively;
(5) concentrated, dry: by collect the liquid (a) that obtains pressure be 0.03-0.08MPa, temperature is concentrated into the 1/2-1/3 of original volume under being the condition of 50-60 DEG C, by the liquid (a) after concentrated and add 2-8 times of volume 95% ethanol, leave standstill 0.5-5h after mixing, filter; The fluidized bed drying 0.2-10min that filter residue wind speed is 0.5-5m/s, temperature is 60 DEG C-110 DEG C, until water content is less than 13%, crosses 60-120 mesh sieve after pulverizing, obtains water-soluble dietary fiber; Or
Be 0.5-5m/s, the fluidized bed drying 0.2min-10min of 80 DEG C-110 DEG C by sediment (b) with wind speed, until water content is less than 13%, pulverized 60 order-120 mesh sieves, and obtained water insoluble dietary fiber.
Principle of the present invention destroys cellulose by mechanical force, structure closely between hemicellulose and lignin, increases the specific area of dietary fiber, make complex enzyme more abundant to the effect of substrate, the modified effect of raising cellulase and zytase.
Compare the present invention with prior art with product and there is following distinguishing feature:
1. the present invention adopts first degreasing, use alkali, enzyme (protease, amylase) to process de-albumen and starch again, improve the concentration of dietary fiber, simultaneously, high molecular relaxing such as the dietary fiber, protein, starch etc. that are conducive to combining closely is dissociated, and improves the purity of dietary fiber.
2. complex enzyme (mixed liquor of cellulase and the zytase) method of modifying of the present invention's employing, can act on different loci, thus significantly improve the yield of hydrolysis efficiency and water-soluble dietary fiber (SDF).
3. technique of the present invention adopts mechanical force+combined-enzyme method modification grain dietary fiber, mechanical external force effectively can reduce the particle diameter of grain dietary fiber, increase its specific area, destroy the structure of dietary fiber component, expose more enzyme action site, reduce reaction resistance, improve modification efficiency, improve modified effect.
Accompanying drawing explanation
fig. 1: be the microstructure utilizing various dietary fiber after different material and distinct methods modification or unmodified process
figure.
accompanying drawingdescription of symbols:
figure 1Awith
figure 1Bbe unmodified dietary fiber structure (wherein
figure 1Athe stereoscan photograph of amplification 700 times,
figure 1Bthe stereoscan photograph of amplification 3000 times);
fig. 1 Cwith
fig. 1 Dbe utilize cellulose enzyme modification dietary fiber structure (wherein
fig. 1 Cthe stereoscan photograph of amplification 700 times,
fig. 1 Dthe stereoscan photograph of amplification 3000 times);
fig. 1 Ewith
fig. 1 Fbe utilize xylan enzyme modification dietary fiber structure (wherein
fig. 1 Ethe stereoscan photograph of amplification 700 times,
fig. 1 Fthe stereoscan photograph of amplification 3000 times);
fig. 1 Gwith
fig. 1 Hbe dietary fiber structure after utilizing combined-enzyme method modification (wherein
fig. 1 Gthe stereoscan photograph of amplification 700 times,
fig. 1 Hthe stereoscan photograph of amplification 3000 times);
fig. 1 Iwith
fig. 1 Jbe dietary fiber structure after utilizing mechanical force-combined-enzyme method modification (wherein
fig. 1 Ithe stereoscan photograph of amplification 700 times,
fig. 1 Jthe stereoscan photograph of amplification 3000 times).
fig. 2: be the infrared of modification or the unmodified and dietary fiber that differently processes
figurespectrum.
accompanying drawingdescription of symbols, on the ordinate of right side digital 1-5 represent unmodified respectively, cellulase modification, zytase modification, combined-enzyme method modification, mechanical force-combined-enzyme method modification dietary fiber
Detailed description of the invention
The experiment material used in embodiment
as table 1shown in.
table 1the experiment material inventory used in embodiments of the invention
Embodiment middle finger target assay method and computational methods:
(1) basic index
The detection method of total dietary fiber, soluble dietary fiber, insoluble diedairy fiber content is with reference to Chinese people's republicanism
country of statethe method of standard GB/T5009.88-2008 " detection method of cellulose, hemicellulose, lignin is with reference to Xiong Sumin " (2005).
Dietary fiber yield is calculated as follows:
(2) microstructure
Get appropriate sample, after adopting sputter coating method to carry out surface gold-plating to sample, utilize ESEM carry out observing (Li Lun, 2009, the research [master thesis] of defatted rice bran dietary fiber. Wuxi: Southern Yangtze University).
(3) IR spectrum scanning
The potassium bromide powder getting 1-2mg sample and 100mg drying is in agate mortar, and under infrared lamp, abundant porphyrize mixing, is evenly placed in press mold device by ground powder, is pressed into certain thickness slide, put into rapidly instrument and scan.Scanning times 32, resolution ratio 4cm
-1.
(4) mensuration of oily power is held
Take 1g sample, fully mix after adding 20g peanut oil, at 37 DEG C after insulation vibration 1h, centrifugal 15min under the rotating speed of 4500r/min, abandons upper strata grease, blots the peanut oil of rice bran dietary fiber remained on surface, claims its quality, is calculated as follows and holds oily power:
(5) mensuration of expansive force
Take 0.5g sample, be placed in 10mL graduated cylinder, recording volume reading, accurately add 5mL distilled water, shaken well, be incubated 24h at 37 DEG C after, recording volume reading, is calculated as follows expansive force:
(6) mensuration of retention ability
Accurately take 1g sample and be placed in 100ml beaker, add 37 DEG C of distilled water insulation 24h, be transferred in Centrifuge Cup, under the speed of 4500r/min, centrifugal 15min takes out.Incline supernatant, claims quality, be calculated as follows retention ability:
(7) mensuration of cholesterol ability is adsorbed
Take 2g sample in triangular flask, add 50g fully beats dilution egg yolk emulsion with 9 times of quality distilled water, the pH value of system is adjusted to 2.0 and 7.0 respectively, insulation vibration 2h at 37 DEG C, centrifugal 15min under the rotating speed of 2000r/min, Aspirate supernatant 1mL, dilute with acetic acid the content that 5 times measure cholesterol afterwards, the adsorption capacity of cholesterol is calculated as follows:
A: the quality (mg) representing cholesterol in blank
B: the quality (mg) representing cholesterol in supernatant
(8) mensuration of natrium taurocholicum ability is adsorbed
Natrium taurocholicum (SodiumTaurocholate, STC) is dissolved in the physiological saline of pH6.5, is mixed with the solution that concentration is 2 μm of ol/mL.Accurately take 40mg dietary fiber, add 5mLSTC solution, at 37 DEG C after insulation vibration 1h, centrifugal 20min under the rotating speed of 4500r/min, with STC solution for blank, gets supernatant and carries out HPLC analysis, adopts peak area metering, according to B
sTCcalibration curve, calculates absorption STC ability according to the following formula:
HPLC condition:
Chromatographic column: ZORBAXEclipseXDBC
18(250mm × 4.6mm × 5um);
Column temperature: 35 DEG C;
Sample size: 10L;
Determined wavelength: 205nm;
Flow velocity: 1.0mL/min;
Mobile phase: acetonitrile/0.04%KH
2pO
4(70:30).
Embodiment 1 utilizes enzyme process to prepare modification composite dietary
(1) pre-treatment: with rice bran (
as table 1described) for raw material is after screening, removal of impurities, pulverizing, crossing 60 mesh sieves, the vegetable oil extraction solvent being placed in 6 times of volumes (is a kind of vegetable oil extraction solvent be purchased, see Chinese people's republicanism
country of statestandard, " vegetable oil extraction solvent ", standard No. GB16629-2008, published by China Standards Press, in September, 2008, Beijing) in, stir immersion 2 hours, centrifugation, by air-dry for precipitation deviate from solvent, obtain degreasing raw material.
(2) separation and Extraction: mass fraction degreasing raw material being dipped in 10 times of volumes is in the NaOH solution of 0.3%, stir after soaking 2h, centrifugation, gets lower sediment.Lower sediment being dipped in the water of 4 times of volumes, is 6 by the pH value of HCl regulation system, heating and thermal insulation 10min at 50 DEG C, add 3000u/g papain (
as table 1described) add after stirring reaction 30min at 50 DEG C 300u/g amylase (
as table 1described), stirring reaction 30min at 55 DEG C, then be heated to seethe with excitement 10min, then centrifugation, by water washing and precipitating 5 times, get lower sediment, obtain unmodified dietary fiber slip, by slip fluidized bed drying (preferred parameter: wind speed 10m/s, 60 DEG C, 10min), then carry out pulverizing 60 mesh sieves, obtain unmodified composite dietary.
(3) modification: the pH value unmodified composite dietary slip being dipped in 5 times of volumes is in the 0.08mol/L-0.1mol/L citric acid solution of 4.8, add respectively 1.0u/g cellulase (
as table 1described), the zytase of 50u/g (
as table 1described) and add the cellulase of 1.0u/g and the zytase of 50u/g simultaneously, respectively at 50 DEG C after stirring reaction 2h, material is boiled 10min at 100 DEG C, add the ethanol of 95% of 5 times of volumes, leave standstill 2h at 50 DEG C after, the dietary fiber slip of enzyme modification is obtained after filtration, by this slip fluidized bed drying (preferred parameter: wind speed 1m/s, 80 DEG C, 10min), carry out again pulverizing 60 mesh sieves, obtain the composite dietary of cellulase modification, zytase modification, complex enzyme modification.
table 2for dietary fiber yield prepared by distinct methods, by
table 2known, through cellulase, the yield of zytase and the modified composite dietary of complex enzyme is organized contrast do not have marked difference with blank.
table 3for the physico-chemical property of rice bran dietary fiber prepared by distinct methods, by
table 3known, through the dietary fiber of cellulase, zytase, complex enzyme modification retention ability and hold oily power and reduce gradually.The ability of expansive force, absorption natrium taurocholicum and the more unmodified dietary fiber of ability of absorption cholesterol are all significantly increased.
By
fig. 1 (a, B) known, unmodified dietary fiber is after cellulase process, and the spherical particle on surface disappears, and hole and the fragment on sheet dietary fiber surface increase, and quality is loose and coarse.
fig. 1 (e, F) reflect that unmodified composite dietary is after xylanase treatment, surface is residual spherical particle still, and dietary fiber surface limellar stripping is obvious, and fragment increases, rough surface.
fig. 1 (h, I) reflect that unmodified composite dietary is after complex enzyme process, significantly longitudinally peeling off and fracture appears in dietary fiber surface, and dietary fiber is granular more, occurs cellular dietary fiber fragment.
Embodiment 2 utilizes mechanical force-combined-enzyme method to prepare modification composite dietary
The pH value that the unmodified dietary fiber slip of preparation in embodiment 1 is dipped in 3 times of volumes is in the 0.08mol/L-0.1mol/L citric acid solution of 6, mix with the cellulase of 1.0u/g and the zytase of 50u/g, (preferred parameter: ball-milling medium is zirconia in ball mill again, filling rate 70%, radius 0.6-0.8mm, rotating speed 500r/min) griding reaction 3h, temperature controls at 50 DEG C; Or with abrasive disc formula fiberizer (preferred parameter: rotating speed 3000r/min, multicomponent alloy abrasive disc), griding reaction 2h at 50 DEG C, the dietary fiber slip of mechanical force-complex enzyme modification is obtained after filtration, slip is boiled 10min at 100 DEG C, after the ethanol adding 95% of 5 times of volumes leaves standstill 2h, the dietary fiber slip of mechanical force-complex enzyme modification is obtained after filtration, by the slip of gained fluidized bed drying (preferred parameter: wind speed 1m/s, 80 DEG C, 10min), then carry out pulverizing 60 mesh sieves, obtain the composite dietary of mechanical force-complex enzyme modification.Test effect is shown in
table 2.
By
table 2known, the composite dietary yield through abrasive disc-combined-enzyme method and ball milling-complex enzyme modification is organized contrast do not have marked difference with blank.
By
table 3known; the composite dietary physicochemical characteristic obtained with enzyme modification compares; through the composite dietary of abrasive disc-combined-enzyme method and ball milling-combined-enzyme method modification retention ability and hold oily power and slightly reduce; expansive force, the ability of absorption natrium taurocholicum and the ability of absorption cholesterol are significantly increased.
By
fig. 1in J
figureknown, due to the enzymolysis of violent extruding and rubbing action and complex enzyme, dietary fiber is fragmentation, honeycomb more, and complete dietary fiber bundle and lamella obviously reduce, and mechanical force-complex enzyme changed dramatically in the microscopic appearance of dietary fiber.
By
fig. 2known, after mechanical force-complex enzyme effect, at 1508-1509cm
-1place produces the characteristic absorption peak of lignin phenyl ring skeletal vibration, at 1108cm
-1hemicellulose and the cellulosic characteristic absorption peak at place weaken.The structure of lignin changes, and more characteristic group is exposed, and the content of lignin significantly declines.
Embodiment 3 utilizes distinct methods to prepare water-soluble dietary fiber and water insoluble dietary fiber
The dietary fiber slip of enzyme modification embodiment 1 and embodiment 2 prepared and the dietary fiber slip of mechanical force-enzyme modification are in 100 DEG C of heating 10min, centrifugation, by the hot water washing and precipitating 3 times of 60 DEG C, collect liquid (a) and sediment (b) respectively; By collect the liquid (a) that obtains pressure be 0.5MPa (absolute pressure), temperature is evaporated to 1/3 times of volume under being the condition of 50 DEG C, the ethanol of 95% of 5 times of volumes is added in liquid (a) after concentration, leave standstill 5h after mixing, filter; The fluidized bed drying 10min that filter residue wind speed is 1m/s, temperature is 80 DEG C, recording water content is 12.8%, crosses 60 mesh sieves, obtain water-soluble dietary fiber (SDF) after pulverizing;
Be 2m/s, the fluidized bed drying 5min of 90 DEG C by sediment (b) with wind speed, recording water content is less than 11.5%, then pulverizes 100 mesh sieves, obtains water insoluble dietary fiber (IDF);
By
table 2known, with blank, through cellulase modification, the modification of zytase modification and complex enzyme, water-soluble dietary fiber (SDF) yield of abrasive disc-complex enzyme modification and ball milling-complex enzyme modification significantly improves, and the yield of water insoluble dietary fiber (IDF) significantly reduces.
Embodiment 4 utilizes different material to prepare water-soluble dietary fiber and water insoluble dietary fiber
The manufacturing process of the present embodiment is identical with the step of water insoluble dietary fiber with mechanical force in embodiment 3+water-soluble dietary fiber is prepared in combined-enzyme method modification, just in the pre-treatment step of embodiment 1, respectively raw material is substituted rice bran with wheat bran, maize peel, green gram spermoderm, Testa Glycines, compare the feature that separate sources grain husk slag prepares dietary fiber.
Unmodified and through ball milling-complex enzyme modified soluble dietary fiber and water insoluble dietary fiber the yield of different material is shown in
table 4.By
table 4known, the yield of the water-soluble dietary fiber obtained through mechanical force-combined-enzyme method modification significantly rises.
table 2distinct methods prepare dietary fiber yield (n=3,
) (%)
Note: blank is unmodified composite dietary, and raw material is rice bran
table 3the physico-chemical property of rice bran composite dietary prepared by distinct methods (n=3,
)
Note: blank is unmodified composite dietary, and raw material is rice bran
table 4modified dietary fiber IDF prepared by different material and SDF yield (n=3,
) (%)
Leading reference
1. bear element is quick etc., cellulose in rice husk, the mensuration of hemicellulose and lignin. grain and feed industries, 2005,8 (2): 40-41.
2 Li Lun. the research [master thesis] of defatted rice bran dietary fiber. Wuxi: Southern Yangtze University
figurebook shop, 2009.
Claims (3)
1. the method utilizing mechanical force-complex enzyme reaction to prepare modified dietary fiber, it is characterized in that, the accessory substance rice bran being rich in dietary fiber produced with process of grain processing, wheat bran, maize peel and beans skin slag are for raw material, through pre-treatment, separation and Extraction, modifiedly obtain modification composite dietary, then obtain water-soluble and water-insoluble grain dietary fiber through steps such as refining, concentrate dryings; Preparation process is as follows:
(1) pre-treatment: by raw material screening, removal of impurities, crosses 60-80 mesh sieve after pulverizing, and the vegetable oil extraction solvent being then placed in 5-10 times of volume stirs and soaks 1-3h, centrifugation, by air-dry for precipitation deviate from solvent, obtain degreasing material;
(2) separation and Extraction: mass fraction degreasing material being dipped in 8-12 times of volume is in the NaOH solution of 0.3%-0.6%, stir after soaking 2-4h, centrifugation, get lower sediment, add in the water of 2-5 times of volume, by HCl adjust ph to 5-7, the papain adding 1000-4000u/g is at 30 DEG C-50 DEG C after stirring reaction 10-30min, add the amylase of 100u/g-500u/g, stirring reaction 10min-35min at 40 DEG C-90 DEG C, be heated to the 10min that seethes with excitement again, then centrifugation, by water washing and precipitating 3-5 time, get lower sediment, obtain unmodified dietary fiber slip for subsequent use, or obtain unmodified composite dietary by after the unmodified dietary fiber slip drying of gained,
(3) modification: the pH value unmodified dietary fiber slip being dipped in 2-5 times of volume is in the citric acid solution of the 0.08mol/L-0.1mol/L of 4-6, add 0.5u/g-5.0u/g cellulase and 40u/g-200u/g zytase, after mixing in ball mill, ball-milling medium is zirconia, filling rate 60-80%, radius 0.6-0.8mm, rotating speed 300r/min-800r/min, griding reaction 2-4h at 40 DEG C-60 DEG C; Or with abrasive disc formula fiberizer, rotating speed 2000-3000r/min, griding reaction 1 ~ 2h at 30 DEG C-55 DEG C, obtain the dietary fiber slip of mechanical force-complex enzyme modification after filtration, slip is dry, obtain the composite dietary of mechanical force-complex enzyme modification;
(4) refining: by the dietary fiber slip of mechanical force-complex enzyme modification in 100 DEG C of heating 5-20min, centrifugation, by hot water washing and precipitating 2-5 time of 60 DEG C-70 DEG C, collects liquid (a) and sediment (b) respectively;
(5) concentrated, dry: by collect the liquid (a) that obtains pressure be 0.03MPa-0.08MPa, temperature is concentrated into the 1/2-1/3 of original volume under being the condition of 50 DEG C-60 DEG C, the ethanol of 95% of 2-8 times of volume is added in volume after concentration, 0.5-5h is left standstill after mixing, filter, the fluidized bed drying 0.2min-10min that filter residue wind speed is 0.5-5m/s, temperature is 60 DEG C-110 DEG C, until water content is less than 13%, cross 60-120 mesh sieve after pulverizing, obtain water-soluble dietary fiber; Or
Be 0.5-5m/s, the fluidized bed drying 0.2min-10min of 80 DEG C-110 DEG C by sediment (b) with wind speed, until water content is less than 13%, pulverized 60 order-120 mesh sieves, and obtained water insoluble dietary fiber.
2. the composite dietary that the method that one according to claim 1 utilizes mechanical force-complex enzyme to react to prepare modified dietary fiber prepares or water-soluble dietary fiber or water insoluble dietary fiber product.
3. the method that one according to claim 1 utilizes mechanical force-complex enzyme reaction to prepare modified dietary fiber is preparing the application in composite dietary, water-soluble dietary fiber or water insoluble dietary fiber.
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