CN105361187B - A kind of modified grain dietary fiber and preparation method thereof - Google Patents
A kind of modified grain dietary fiber and preparation method thereof Download PDFInfo
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- CN105361187B CN105361187B CN201510629161.1A CN201510629161A CN105361187B CN 105361187 B CN105361187 B CN 105361187B CN 201510629161 A CN201510629161 A CN 201510629161A CN 105361187 B CN105361187 B CN 105361187B
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- 235000013325 dietary fiber Nutrition 0.000 title claims abstract description 104
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 230000009144 enzymatic modification Effects 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 238000000605 extraction Methods 0.000 claims abstract description 10
- 230000008569 process Effects 0.000 claims abstract description 9
- 238000002203 pretreatment 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
- 239000006227 byproduct Substances 0.000 claims abstract description 5
- 235000005911 diet Nutrition 0.000 claims description 25
- 239000002002 slurry Substances 0.000 claims description 23
- 235000013339 cereals Nutrition 0.000 claims description 19
- 239000002131 composite material Substances 0.000 claims description 19
- 230000000378 dietary effect Effects 0.000 claims description 19
- 235000007164 Oryza sativa Nutrition 0.000 claims description 14
- 235000009566 rice Nutrition 0.000 claims description 14
- 239000013049 sediment Substances 0.000 claims description 13
- 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
- 238000001035 drying Methods 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 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 9
- 238000001556 precipitation Methods 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- 238000005238 degreasing Methods 0.000 claims description 7
- 230000037213 diet Effects 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 235000019441 ethanol Nutrition 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
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims description 4
- 235000019418 amylase Nutrition 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 235000015112 vegetable and seed oil Nutrition 0.000 claims description 4
- 239000008158 vegetable oil Substances 0.000 claims description 4
- 235000015099 wheat brans Nutrition 0.000 claims description 4
- 108090000526 Papain Proteins 0.000 claims description 3
- 235000016383 Zea mays subsp huehuetenangensis Nutrition 0.000 claims description 3
- 238000009835 boiling Methods 0.000 claims description 3
- 239000012141 concentrate Substances 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 3
- 235000009973 maize Nutrition 0.000 claims description 3
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical group [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 3
- 229940055729 papain Drugs 0.000 claims description 3
- 235000019834 papain Nutrition 0.000 claims description 3
- 238000012216 screening Methods 0.000 claims description 3
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 3
- 108010084185 Cellulases Proteins 0.000 claims description 2
- 102000005575 Cellulases Human genes 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims description 2
- 238000006911 enzymatic reaction Methods 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims description 2
- 240000007594 Oryza sativa Species 0.000 claims 1
- 229940088598 enzyme Drugs 0.000 abstract description 32
- 108090000790 Enzymes Proteins 0.000 abstract description 21
- 102000004190 Enzymes Human genes 0.000 abstract description 21
- 108010059892 Cellulase Proteins 0.000 abstract description 16
- 229940106157 cellulase Drugs 0.000 abstract description 16
- 230000004048 modification Effects 0.000 abstract description 12
- 238000012986 modification Methods 0.000 abstract description 12
- 239000002893 slag Substances 0.000 abstract description 4
- 239000010903 husk Substances 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 2
- 235000013305 food Nutrition 0.000 abstract description 2
- 230000007062 hydrolysis Effects 0.000 abstract description 2
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 2
- 238000002715 modification method Methods 0.000 abstract 4
- 238000007670 refining Methods 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 17
- 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 9
- 238000003199 nucleic acid amplification method Methods 0.000 description 9
- 239000000243 solution Substances 0.000 description 9
- 229920002678 cellulose Polymers 0.000 description 8
- 239000001913 cellulose Substances 0.000 description 8
- 239000000835 fiber Substances 0.000 description 8
- 229920005610 lignin Polymers 0.000 description 8
- 235000012000 cholesterol Nutrition 0.000 description 7
- 238000012545 processing Methods 0.000 description 7
- 229920002488 Hemicellulose Polymers 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 6
- 244000046052 Phaseolus vulgaris Species 0.000 description 5
- 235000010627 Phaseolus vulgaris Nutrition 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 5
- 235000012054 meals Nutrition 0.000 description 5
- 230000014759 maintenance of location Effects 0.000 description 4
- 238000004321 preservation Methods 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
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 3
- 229920002472 Starch Polymers 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- 239000012634 fragment Substances 0.000 description 3
- 230000010355 oscillation Effects 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
- 208000012287 Prolapse Diseases 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 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
- 238000002474 experimental method Methods 0.000 description 2
- 238000004128 high performance liquid chromatography Methods 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
- 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 2
- 239000012798 spherical particle Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000010408 sweeping Methods 0.000 description 2
- 229920001221 xylan Polymers 0.000 description 2
- 150000004823 xylans Chemical class 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
- 241000196324 Embryophyta Species 0.000 description 1
- 101710121765 Endo-1,4-beta-xylanase 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
- 239000007836 KH2PO4 Substances 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- 108091005804 Peptidases Proteins 0.000 description 1
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- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 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
- 235000005824 Zea mays ssp. parviglumis 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
- 238000004458 analytical method Methods 0.000 description 1
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- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 235000013345 egg yolk Nutrition 0.000 description 1
- 210000002969 egg yolk Anatomy 0.000 description 1
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- 238000013467 fragmentation Methods 0.000 description 1
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- 239000008103 glucose Substances 0.000 description 1
- 150000002333 glycines Chemical class 0.000 description 1
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- 238000010438 heat treatment Methods 0.000 description 1
- 230000002218 hypoglycaemic effect Effects 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910000402 monopotassium phosphate Inorganic materials 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 235000019198 oils Nutrition 0.000 description 1
- 230000001151 other effect Effects 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
- GNSKLFRGEWLPPA-UHFFFAOYSA-M potassium dihydrogen phosphate Chemical compound [K+].OP(O)([O-])=O GNSKLFRGEWLPPA-UHFFFAOYSA-M 0.000 description 1
- 235000019419 proteases Nutrition 0.000 description 1
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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
Landscapes
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The invention belongs to grain byproducts deep process technology fields, and in particular to a kind of modified grain dietary fiber and preparation method thereof.Using grain husk slag as raw material, through pre-treatment, separation, extraction dietary fiber, using double enzyme modification methods and enzyme process ball milling modification method, modified dietary fiber is obtained；Again using modified dietary fiber as raw material, foods with high dietary fiber is obtained.The invention is characterised in that the modification process of dietary fiber, preferred method is double enzyme modification methods and enzyme process ball milling modification method, and water insoluble dietary fiber is obtained, then by refining and being dried to obtain water-soluble dietary fiber and water insoluble dietary fiber by modified.The present invention simultaneously digests grain dietary fiber using cellulase and zytase, significantly improves the content of water insoluble dietary fiber in grain dietary fiber；The grain size of grain dietary fiber is reduced using mechanical force enzyme process, increases its specific surface area, improves hydrolysis result of the complex enzyme to dietary fiber.
Description
Technical field
The invention belongs to grain processing with utilizing technical field.More particularly to a kind of modified grain dietary fiber and preparation side
Method.The present invention obtains water-soluble dietary fiber product and water-insoluble using cereal processing byproduct as raw material, by suitably processing
Diet fiber product and preparation method thereof.
Background technology
Rice bran, wheat bran, maize peel and beans skin slag etc. are the by-products of cereal processing, and dietary fiber content is enriched, had
Increase satiety, Constipation, hypoglycemic, reducing blood lipid and anticancer and other effects, be important dietary fiber sources.It is generally believed that
The viscosity of water-soluble dietary fiber (SDF) is higher, and having reduces blood glucose response, reduces the functional characteristics such as cholesterolemia.However day
The SDF contents of right grain dietary fiber are relatively low (≤3%).The document of Chinese invention patent Publication No. CN 101564132A leads to
Tight-face blasting technique is crossed to be modified bean dregs dietary fiber, improve bean dregs in SDF content, but needed in dietary fiber compared with
The starch of high-content can be only achieved preferable tight-face blasting effect, effect unobvious relatively low so as to cause the concentration of dietary fiber.
The document of 101785831 A of Publication No. CN by add cellulase improve rice bran dietary fiber in SDF content, and
In grain dietary fiber, the binder course that the crystal region of cellulose and hemicellulose and lignin are formed tightly is wrapped in fiber
Element all hinders effect of the enzyme to cellulose.The document of 102940262 A of Publication No. CN adds cellulase by priority
Effect with 'beta '-mannase to improve the content of SDF in bean dregs, the successively effect of double enzymes can destroy dietary fiber component it
Between the structure combined closely, improve the modified effect to dietary fiber, but the method for the stepwise discretization takes longer, conversion effect
Rate is relatively low.Mechanical force can destroy cellulose, close structure between hemicellulose and lignin, increase the ratio table of dietary fiber
Area makes complex enzyme more abundant to the effect of substrate, improves the modified effect of cellulase and zytase.
Invention content
The defects of it is an object of the invention to overcome the prior art, provides a kind of modified grain dietary fiber and its preparation side
Method.The present invention is improved by the enzymolysis of mechanical external force assisted recombination enzyme (such as cellulase and zytase) to cereal
The modified effect of dietary fiber.
Realize that the specific technical solution of the present invention is as follows：
A kind of method for preparing modified dietary fiber using mechanical force-compound enzyme reaction, is generated with process of grain processing
By-product rice bran, wheat bran, maize peel and beans skin slag rich in dietary fiber are raw material, through pre-treatment, separation and Extraction, modified
Modified composite dietary is obtained, is made water-soluble using refined, concentrate drying and water-insoluble grain meal is fine
Dimension；Preparation process is as follows：
(1) pre-treatment：By raw material screening, removal of impurities, -80 mesh of 60 mesh sieve is smashed it through, is subsequently placed in the plant of 5-10 times of volume
1-3h is impregnated in stirring in object oil extraction solvent, centrifuges, and precipitation is air-dried prolapse solvent, obtains degreasing material；
(2) separation and Extraction：Degreasing material is dipped in NaOH solution of the mass fraction for 0.3%-0.6% of 8-12 times of volume
In, it after 2-4h is impregnated in stirring, centrifuges, takes lower sediment, add in the water of 2-5 times of volume, pH value is adjusted to 5-7 with HCl,
After the papain of addition 1000u/g-4000u/g is stirred to react 10min-30min at 30 DEG C -50 DEG C, 100u/g- is added in
The amylase of 500u/g is stirred to react 10min-35min at 40 DEG C -90 DEG C, is again heated to boiling 10min, is then centrifuged for point
From washing with water precipitation 3-5 times, take lower sediment, it is spare or by the unmodified of gained to obtain unmodified dietary fiber slurry
Dietary fiber slurry drying after obtain unmodified composite dietary；
(3) it is modified：, by unmodified dietary fiber slurry be dipped in 2-5 times of volume pH value be 4-6 0.08mol/L-
In 0.1mol/L citric acid solutions, 0.5u/g-5.0u/g cellulases and 40u/g-200u/g zytases are added in, is uniformly mixed
After in ball mill, ball-milling medium is zirconium oxide, filling rate 60%-80%, radius 0.6-0.8mm, rotating speed 300-800r/min,
The griding reaction 2-4h at 40 DEG C -60 DEG C；Or with grinding formula fiberizer, rotating speed 2000-3000r/min is ground at 30 DEG C -55 DEG C
Mill 1~2h of reaction, obtains the dietary fiber slurry of mechanical force-compound enzyme modification, slurry is dried, obtains machinery after filtering
The composite dietary of power-compound enzyme modification；
(4) it refines：The dietary fiber slurry of mechanical force-compound enzyme modification is heated into 5-20min, centrifugation in 100 DEG C or so
Separation cleans precipitation 2-5 times with 60 DEG C -70 DEG C of hot water, collects liquid (a) and sediment (b) respectively；
(5) it concentrates, is dry：Obtained liquid (a) will be collected pressure is 0.03-0.08MPa, temperature is 50-60 DEG C
Under the conditions of be concentrated into the 1/2-1/3 of original volume, by 95% ethyl alcohol that is liquid (a) and adding in 2-8 times of volume after concentration,
0.5-5h is stood after mixing, is filtered；Filter residue with wind speed is 0.5-5m/s, the fluidized bed drying 0.2- that temperature is 60 DEG C -110 DEG C
10min sieves hereinafter, smashing it through 60-120 mesh until water content is 13%, obtains water-soluble dietary fiber；Or
With wind speed it is 0.5-5m/s by sediment (b), 80 DEG C -110 DEG C of fluidized bed drying 0.2min-10min, until containing
Water is 13% sieves hereinafter, crushed -120 mesh of 60 mesh, obtains water insoluble dietary fiber.
The principle of the present invention is to destroy cellulose by mechanical force, close structure between hemicellulose and lignin increases
The specific surface area of big dietary fiber, makes complex enzyme more abundant to the effect of substrate, improves changing for cellulase and zytase
Property effect.
The present invention has following distinguishing feature compared with the prior art and product：
1. the present invention takes off albumen and starch using first degreasing, then with alkali, enzyme (protease, amylase) processing, meals are improved
The concentration of fiber is eaten, meanwhile, be conducive to the high molecular relaxation dissociation such as the dietary fiber, protein, starch combined closely, improve
The purity of dietary fiber.
2. complex enzyme (mixed liquor of cellulase and zytase) method of modifying that the present invention uses, can act on not
Same site, thus significantly improve the yield of hydrolysis efficiency and water-soluble dietary fiber (SDF).
3. the technique of the present invention is modified grain dietary fiber using mechanical force+combined-enzyme method, mechanical external force can effectively drop
The grain size of low grain dietary fiber increases its specific surface area, destroys the structure of dietary fiber component, the more enzyme effect positions of exposure
Point reduces reaction resistance, improves modification efficiency, improves modified effect.
Description of the drawings
Fig. 1：It is the microstructure using various dietary fibers after different material and distinct methods modification or unmodified processing
Figure.
Reference sign：Figure 1A and Figure 1B is that (wherein Figure 1A is sweeping for 700 times of amplification to unmodified dietary fiber structure
Electromicroscopic photograph is retouched, Figure 1B is the stereoscan photograph of 3000 times of amplification)；Fig. 1 C and Fig. 1 D are the meals using cellulose enzyme modification
Food fibre structure (wherein Fig. 1 C are the stereoscan photographs of 700 times of amplification, and Fig. 1 D are the stereoscan photographs of 3000 times of amplification)；
Fig. 1 E and Fig. 1 F be using xylan enzyme modification dietary fiber structure (wherein Fig. 1 E be amplify 700 times scanning electron microscope shine
Piece, Fig. 1 F are the stereoscan photographs of 3000 times of amplification)；Fig. 1 G and Fig. 1 H are fine using the diet after combined-enzyme method modification
Dimension structure (wherein Fig. 1 G are the stereoscan photographs of 700 times of amplification, and Fig. 1 H are the stereoscan photographs of 3000 times of amplification)；Fig. 1 I
It is that (wherein Fig. 1 I are sweeping for 700 times of amplification using the dietary fiber structure after mechanical force-combined-enzyme method modification with Fig. 1 J
Electromicroscopic photograph is retouched, Fig. 1 J are the stereoscan photographs of 3000 times of amplification).
Fig. 2：It is the infared spectrum of dietary fiber that is modified or unmodified and being treated variously for.
Reference sign, number 1-5 represents unmodified respectively, cellulase is modified, zytase on the ordinate of right side
Modified, combined-enzyme method modification, the dietary fiber of mechanical force-combined-enzyme method modification
Specific embodiment
The experiment material used in embodiment is as shown in table 1.
The experiment material inventory used in 1 the embodiment of the present invention of table
Embodiment middle finger target assay method and computational methods：
(1) basic index
Total dietary fiber, soluble dietary fiber, insoluble diedairy fiber content detection method be total to reference to the Chinese people
With state standard GB/T/T 5009.88-2008《Cellulose, hemicellulose, lignin detection method refer to Xiong Sumin》
(2005) method.
Dietary fiber yield is calculated as follows：
(2) microstructure
Suitable sample is taken, after carrying out surface gold-plating to sample using sputter coating method, is observed using scanning electron microscope
(Li Lun, 2009, research [master thesis] the Wuxis of defatted rice bran dietary fiber:Southern Yangtze University).
(3) IR spectrum scanning
The potassium bromide powder that 1-2mg samples and 100mg are dried is taken in agate mortar, it is fully finely ground mixed under infrared lamp
It is even, ground powder is homogeneously disposed in press mold device, is pressed into certain thickness slide, is put into instrument is swept rapidly
It retouches.Scanning times 32, resolution ratio 4cm-1。
(4) measure of oily power is held
1g samples are weighed, add in abundant mixing after 20g peanut oil, at 37 DEG C after heat preservation oscillation 1h, 4500r/min's
15min is centrifuged under rotating speed, abandons upper strata grease, blots the peanut oil of rice bran dietary fiber remained on surface, claims its quality, counts as the following formula
Oily power is held in calculation：
(5) measure of expansive force
0.5g samples are weighed, are placed in 10mL graduated cylinders, record volume reading, accurately addition 5mL distilled water, shaken well,
After being kept the temperature for 24 hours at 37 DEG C, volume reading is recorded, expansive force is calculated as follows：
(6) measure of retention ability
It accurately weighs 1g samples to be placed in 100ml beakers, adds 37 DEG C of distilled water heat preservations for 24 hours, be transferred in Centrifuge Cup,
15min is centrifuged under the speed of 4500r/min to take out.Incline supernatant, claims quality, retention ability is calculated as follows：
(7) measure of cholesterol ability is adsorbed
2g samples are weighed in triangular flask, 50g is added in and fully beats diluted egg yolk breast with 9 times of quality distilled water
The pH value of system is adjusted to 2.0 and 7.0 by liquid respectively, and heat preservation oscillation 2h, centrifuges under the rotating speed of 2000r/min at 37 DEG C
15min, Aspirate supernatant 1mL, the content that cholesterol is measured after 5 times is diluted with acetic acid, and the adsorption capacity of cholesterol is counted as the following formula
It calculates：
A：Represent the quality (mg) of cholesterol in blank
B：Represent the quality (mg) of cholesterol in supernatant
(8) measure of natrium taurocholicum ability is adsorbed
Natrium taurocholicum (Sodium Taurocholate, STC) is dissolved in the physiological saline of pH6.5, is configured to concentration
Solution for 2 μm of ol/mL.It is accurate to weigh 40mg dietary fibers, 5mL STC solution is added in, at 37 DEG C after heat preservation oscillation 1h,
20min is centrifuged under the rotating speed of 4500r/min, using STC solution as blank, supernatant is taken to carry out HPLC analyses, using peak area meter
Amount, according to BSTCStandard curve calculates absorption STC abilities according to the following formula：
HPLC conditions：
Chromatographic column：ZORBAX Eclipse XDB C18(250mm×4.6mm×5um)；
Column temperature：35℃；
Sample size：10L；
Detection wavelength：205nm；
Flow velocity：1.0mL/min；
Mobile phase：Acetonitrile/0.04%KH2PO4(70:30)。
Embodiment 1 prepares modified composite dietary using enzyme process
(1) pre-treatment：With rice bran it is (as described in Table 1) for raw material through screening, cleaning, crush, cross 60 mesh sieve after, be placed in 6 times
Volume vegetable oil extraction solvent (for a kind of commercially available vegetable oil extraction solvent, referring to National Standard of the People's Republic of China,
" vegetable oil extraction solvent ", standard No. GB16629-2008, published by China Standards Press, in September, 2008, Beijing) in, stirring
It impregnates 2 hours, centrifuges, precipitation is air-dried into prolapse solvent, obtains degreasing raw material.
(2) separation and Extraction：It is stirring in 0.3% NaOH solution by the mass fraction that degreasing raw material is dipped in 10 times of volumes
After impregnating 2h, centrifuge, take lower sediment.Lower sediment is dipped in the water of 4 times of volumes, with the pH value of HCl regulation systems
It is 6, the heating and thermal insulation 10min at 50 DEG C, the papain (as described in Table 1) for adding in 3000u/g is stirred to react at 50 DEG C
The amylase (as described in Table 1) of 300u/g is added in after 30min, 30min is stirred to react at 55 DEG C, is again heated to boiling 10min,
It is then centrifuged for detaching, washes with water precipitation 5 times, take lower sediment, obtain unmodified dietary fiber slurry, slurry is fluidized
Dry (the preferred parameter of bed：Wind speed 10m/s, 60 DEG C, 10min), then 60 mesh sieve was crushed, obtain unmodified compound diet
Fiber.
(3) it is modified：By unmodified composite dietary slurry be dipped in 5 times of volumes pH value be 4.8 0.08mol/L-
In 0.1mol/L citric acid solutions, the cellulase (as described in Table 1) of 1.0u/g, zytase (such as table of 50u/g are added respectively
Described in 1) and the cellulase of 1.0u/g and the zytase of 50u/g are added simultaneously, after being stirred to react 2h at 50 DEG C respectively,
Material at 100 DEG C is boiled into 10min, adds in 95% ethyl alcohol of 5 times of volumes, after standing 2h at 50 DEG C, is obtained after filtering
The dietary fiber slurry of enzyme modification, by slurry fluidized bed drying (preferred parameter：Wind speed 1m/s, 80 DEG C, 10min), then into
Row crushed 60 mesh sieve, obtain the composite dietary of modified cellulase, zytase modification, compound enzyme modification.
Table 2 is dietary fiber yield prepared by distinct methods, as shown in Table 2, through cellulase, zytase and complex enzyme
The yield of modified composite dietary compares no marked difference with blank group.
The physico-chemical property for the rice bran dietary fiber that table 3 is prepared for distinct methods, as shown in Table 3, through cellulase, xylan
Enzyme, compound enzyme modification dietary fiber retention ability and hold oily power and be gradually reduced.Expansive force, adsorb natrium taurocholicum ability and
The more unmodified dietary fiber of ability of absorption cholesterol is significantly increased.
By Fig. 1 (A, B) it is found that unmodified dietary fiber is after cellulase is handled, the spherical particle on surface disappears,
The hole and fragment on sheet dietary fiber surface increase, and quality is loose and coarse.Fig. 1 (E, F) reflects unmodified compound meals
Fiber is eaten after xylanase treatment, surface still remains spherical particle, and dietary fiber surface limellar stripping is apparent, and fragment increases
It is more, rough surface.Fig. 1 (H, I) reflects unmodified composite dietary after compound enzymatic treatment, and dietary fiber surface goes out
Now apparent vertical peeling is more made fine with fracture, dietary fiber, cellular dietary fiber fragment occurs.
Embodiment 2 prepares modified composite dietary using mechanical force-combined-enzyme method
By the unmodified dietary fiber slurry prepared in embodiment 1 be dipped in 3 times of volumes pH value be 6 0.08mol/L-
In 0.1mol/L citric acid solutions, it is uniformly mixed with the cellulase of 1.0u/g and the zytase of 50u/g, in ball mill
(preferred parameter：Ball-milling medium is zirconium oxide, filling rate 70%, radius 0.6-0.8mm, rotating speed 500r/min) griding reaction 3h,
Temperature is controlled at 50 DEG C；Or with grinding formula fiberizer (preferred parameter：Rotating speed 3000r/min, multicomponent alloy grinding), in 50 DEG C
Lower griding reaction 2h obtains the dietary fiber slurry of mechanical force-compound enzyme modification after filtering, slurry is boiled at 100 DEG C
10min after adding in the 95% ethyl alcohol standing 2h of 5 times of volumes, obtains the dietary fiber material of mechanical force-compound enzyme modification after filtering
Slurry, by the slurry of gained fluidized bed drying (preferred parameter：Wind speed 1m/s, 80 DEG C, 10min), then 60 mesh sieve was crushed,
Obtain the composite dietary of mechanical force-compound enzyme modification.Test effect is shown in Table 2.
As shown in Table 2, by the composite dietary yield and blank of grinding-combined-enzyme method and ball milling-compound enzyme modification
Group compares no marked difference.
As shown in Table 3, the composite dietary physicochemical characteristic obtained with enzyme modification is compared, by grinding-it is compound
The retention ability for the composite dietary that enzyme process and ball milling-combined-enzyme method are modified adsorbs ox sulphur with the slightly reduction of oily power, expansive force is held
The ability of sodium taurocholate and the ability of absorption cholesterol are significantly increased.
By the J figures in Fig. 1 it is found that since violent compresses and rubs against effect and the enzymolysis of complex enzyme, diet is fine
Dimension more fragmentation, honeycomb, complete dietary fiber beam is significantly reduced with lamella, and mechanical force-complex enzyme changed dramatically meals
Eat the microscopic appearance of fiber.
As shown in Figure 2, after mechanical force-compound enzyme effect, in 1508-1509cm-1Place generates lignin phenyl ring skeleton
The characteristic absorption peak of vibration, in 1108cm-1The hemicellulose at place and the characteristic absorption peak of cellulose weaken.The structure hair of lignin
Raw to change, more characteristic groups are exposed, and the content of lignin is remarkably decreased.
Embodiment 3 prepares water-soluble dietary fiber and water insoluble dietary fiber using distinct methods
The dietary fiber slurry of enzyme modification prepared by embodiment 1 and embodiment 2 and the dietary fiber of mechanical force-enzyme modification
Slurry heats 10min in 100 DEG C, centrifuges, and cleans precipitation 3 times with 60 DEG C of hot water, collects liquid (a) and sediment respectively
(b)；Obtained liquid (a) will be collected to be concentrated under reduced pressure under conditions of pressure is 0.5MPa (absolute pressure), temperature is 50 DEG C
1/3 times of volume adds in 95% ethyl alcohol of 5 times of volumes in liquid (a) after concentration, stands 5h after mixing, filter；Filter residue is used
The fluidized bed drying 10min that wind speed is 1m/s, temperature is 80 DEG C, it is 12.8% to measure water content, smashes it through 60 mesh sieve, obtains
Water-soluble dietary fiber (SDF)；
With wind speed be 2m/s by sediment (b), 90 DEG C of fluidized bed drying 5min, measure water content as 11.5% hereinafter,
It crushes and sieves with 100 mesh sieve again, obtain water insoluble dietary fiber (IDF)；
As shown in Table 2, it with blank, is modified by cellulase, at zytase modification and the modification of complex enzyme
Water-soluble dietary fiber (SDF) yield of reason, grinding-compound enzyme modification and ball milling-compound enzyme modification significantly improves, and water is not
The yield of soluble dietary fiber (IDF) substantially reduces.
Embodiment 4 prepares water-soluble dietary fiber and water insoluble dietary fiber using different material
The manufacturing process of the present embodiment and mechanical force+combined-enzyme method modification in embodiment 3 prepare water-soluble dietary fiber and
The step of water insoluble dietary fiber, is identical, only in the pre-treatment step of embodiment 1, respectively by raw material with wheat bran, corn
Skin, green gram spermoderm, Testa Glycines substitute rice bran, compare the characteristics of separate sources grain husk slag prepares dietary fiber.
Different material is unmodified and through ball milling-complex enzyme modified soluble dietary fiber and water insoluble dietary fiber
Yield is shown in Table 4.As shown in Table 4, on the yield of the water-soluble dietary fiber being modified by mechanical force-combined-enzyme method is notable
It rises.
2 distinct methods of table prepare dietary fiber yield (n=3,) (%)
Note：Blank is unmodified composite dietary, and raw material is rice bran
3 distinct methods of table prepare rice bran composite dietary physico-chemical property (n=3,)
Note：Blank is unmodified composite dietary, and raw material is rice bran
4 different material of table prepare modified dietary fiber IDF and SDF yield (n=3,) (%)
Leading reference
1. bear element is quick etc., cellulose in rice husk, the measure grain and feed industries of hemicellulose and lignin, and 2005,8
(2):40-41.
Research [master thesis] the Wuxis of 2 Li Lun defatted rice bran dietary fibers:Library of Southern Yangtze University, 2009.
Claims (1)
- A kind of 1. method for preparing modified dietary fiber using mechanical force-compound enzyme reaction, which is characterized in that processed with cereal The by-product rice bran rich in dietary fiber that process generates, wheat bran, one kind in maize peel are raw material, through pre-treatment, detach and carry Take, it is modified obtain modified composite dietary, using it is refined, be concentrated and dried step be made water-soluble grain dietary fiber or Water-insoluble grain dietary fiber；Preparation process is as follows：(1) pre-treatment：By raw material screening, removal of impurities, 60-80 mesh sieve is smashed it through, the vegetable oil for being subsequently placed in 5-10 times of volume is taken out In extraction solvent, 1-3h is impregnated in stirring, centrifuges, and removes solvent after precipitation is air-dried, obtains degreasing material；(2) separation and Extraction：By degreasing material be dipped in 8-12 times of volume mass fraction be 0.3%-0.6% NaOH solution in, It after 2-4h is impregnated in stirring, centrifuges, takes lower sediment, add in the water of 2-5 times of volume, adjust pH value to 5-7 with HCl, add Enter 1000-4000u/g papain be stirred to react 10-30min at 30 DEG C -50 DEG C after, add in 100u/g-500u/g's Amylase is stirred to react 10min-35min at 40 DEG C -90 DEG C, is again heated to boiling 10min, is then centrifuged for detaching, clear with water It washes precipitation 3-5 times, takes lower sediment, it is spare or the unmodified diet of gained is fine to obtain unmodified dietary fiber slurry Unmodified composite dietary is obtained after dimension slurry drying；(3) it is modified：The pH value that unmodified dietary fiber slurry or unmodified composite dietary are dipped in 2-5 times of volume is In the citric acid solution of the 0.08mol/L-0.1mol/L of 4-6,0.5u/g-5.0u/g cellulases and 40u/g-200u/g are added in Zytase is uniformly mixed after in ball mill, and ball-milling medium is zirconium oxide, filling rate 60-80%, radius 0.6- 0.8mm, rotating speed 300r/min-800r/min, the griding reaction 2-4h at 40 DEG C -60 DEG C；Or with grinding formula fiberizer, rotating speed For 2000-3000r/min, 1~2h of griding reaction at 30 DEG C -55 DEG C obtains the diet of mechanical force-compound enzyme modification after filtering Me fibrous slurry；(4) it refines：The dietary fiber slurry of mechanical force-compound enzyme modification is heated into 5-20min in 100 DEG C, is centrifuged, with 60 DEG C -70 DEG C of hot water cleaning precipitation 2-5 time, collects liquid (a) and sediment (b) respectively；(5) it concentrates, is dry：It is 0.03MPa-0.08MPa that obtained liquid (a), which will be collected, in pressure, and temperature is 50 DEG C -60 DEG C Under the conditions of be concentrated into the 1/2-1/3 of original volume, 95% ethyl alcohol of 2-8 times of volume is added in volume after concentration, after mixing 0.5-5h is stood, filtering, filter residue with wind speed is 0.5-5m/s, the fluidized bed drying 0.2min- that temperature is 60 DEG C -110 DEG C 10min sieves hereinafter, smashing it through 60-120 mesh until water content is 13%, obtains water-soluble dietary fiber；OrWith wind speed it is 0.5-5m/s, 80 DEG C -110 DEG C of fluidized bed drying 0.2min-10min by sediment (b), until water content For 13% hereinafter, crushed -120 mesh of 60 mesh sieve, water insoluble dietary fiber is obtained.
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