CN102640905A - Method for extracting water-insoluble dietary fiber of osmunda cinnamomea - Google Patents
Method for extracting water-insoluble dietary fiber of osmunda cinnamomea Download PDFInfo
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- 235000013325 dietary fiber Nutrition 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 44
- 235000007889 Osmunda cinnamomea Nutrition 0.000 title abstract 8
- 241000196126 Osmundastrum cinnamomeum Species 0.000 title abstract 8
- 230000007062 hydrolysis Effects 0.000 claims abstract description 35
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 35
- 239000003513 alkali Substances 0.000 claims abstract description 27
- 102000004139 alpha-Amylases Human genes 0.000 claims abstract description 19
- 108090000637 alpha-Amylases Proteins 0.000 claims abstract description 19
- 229940024171 alpha-amylase Drugs 0.000 claims abstract description 19
- 238000012545 processing Methods 0.000 claims abstract description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 84
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 63
- 244000105017 Vicia sativa Species 0.000 claims description 51
- 239000007788 liquid Substances 0.000 claims description 36
- 238000005238 degreasing Methods 0.000 claims description 23
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 21
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 18
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 17
- 238000005406 washing Methods 0.000 claims description 16
- 239000012153 distilled water Substances 0.000 claims description 13
- 238000000605 extraction Methods 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 12
- 230000007935 neutral effect Effects 0.000 claims description 10
- 229960000583 acetic acid Drugs 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 238000001976 enzyme digestion Methods 0.000 claims description 9
- 239000012362 glacial acetic acid Substances 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 6
- 238000007654 immersion Methods 0.000 claims description 6
- UKLNMMHNWFDKNT-UHFFFAOYSA-M sodium chlorite Chemical compound [Na+].[O-]Cl=O UKLNMMHNWFDKNT-UHFFFAOYSA-M 0.000 claims description 6
- 229960002218 sodium chlorite Drugs 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 2
- 102000004169 proteins and genes Human genes 0.000 abstract description 9
- 108090000623 proteins and genes Proteins 0.000 abstract description 9
- 229920002472 Starch Polymers 0.000 abstract description 3
- 239000008107 starch Substances 0.000 abstract description 3
- 235000019698 starch Nutrition 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 2
- 230000010354 integration Effects 0.000 abstract 1
- 239000000835 fiber Substances 0.000 description 18
- 239000007787 solid Substances 0.000 description 9
- 230000002255 enzymatic effect Effects 0.000 description 8
- 229920005610 lignin Polymers 0.000 description 8
- 239000001913 cellulose Substances 0.000 description 7
- 229920002678 cellulose Polymers 0.000 description 7
- 238000013401 experimental design Methods 0.000 description 7
- 238000002791 soaking Methods 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 238000010298 pulverizing process Methods 0.000 description 6
- 229920002488 Hemicellulose Polymers 0.000 description 5
- 238000005904 alkaline hydrolysis reaction Methods 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 5
- 230000014759 maintenance of location Effects 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000005457 optimization Methods 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 238000005211 surface analysis Methods 0.000 description 4
- 239000004382 Amylase Substances 0.000 description 3
- 102000013142 Amylases Human genes 0.000 description 3
- 108010065511 Amylases Proteins 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 3
- 235000019418 amylase Nutrition 0.000 description 3
- 125000004122 cyclic group Chemical group 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 3
- 239000002689 soil Substances 0.000 description 3
- 238000000967 suction filtration Methods 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- 238000000540 analysis of variance Methods 0.000 description 2
- 238000003556 assay Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 235000019353 potassium silicate Nutrition 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000000611 regression analysis Methods 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- 235000013311 vegetables Nutrition 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 206010010774 Constipation Diseases 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 241000196127 Osmunda Species 0.000 description 1
- 206010033546 Pallor Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229940022682 acetone Drugs 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 230000037396 body weight Effects 0.000 description 1
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- 238000012937 correction Methods 0.000 description 1
- 230000002478 diastatic effect Effects 0.000 description 1
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- 230000037406 food intake Effects 0.000 description 1
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- 235000011187 glycerol Nutrition 0.000 description 1
- 235000008216 herbs Nutrition 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
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- 238000002386 leaching Methods 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 102000004196 processed proteins & peptides Human genes 0.000 description 1
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- 210000002784 stomach Anatomy 0.000 description 1
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Abstract
The invention relates to a method for extracting water-insoluble dietary fiber of osmunda cinnamomea. The osmunda cinnamomea is mainly processed through an enzyme-chemical integration mode, starch is removed by using alpha-amylase, the protein removing speed of alkali liquor is accelerated, and then protein and fat are removed by using the alkali liquor. An alpha-amylase enzymolysis process and an alkali liquor hydrolysis process are optimized by means of a response surface method and used for extracting the water-insoluble dietary fiber of the osmunda cinnamomea. The method for extracting the water-insoluble dietary fiber of the osmunda cinnamomea facilitates deep processing study of the osmunda cinnamomea, fully utilizes domestic osmunda cinnamomea resources and exploits a new field for processing and utilization of the osmunda cinnamomea.
Description
Technical field
The present invention relates to the vegetables processing technique field, specifically, relate to a kind of method of extracting common vetch dish water insoluble dietary fiber.
Background technology
Cellulose is one of the abundantest macromolecular organic compound of occurring in nature content, also is a kind of inexhaustible renewable resource.Cellulose contains great amount of hydroxy group, makes cellulose have good retentiveness through hydroxyl absorption polar water molecules.In general, the plain retention ability of high-quality water insoluble dietary fiber can be blocked swill and absorb large quantity of moisture at the enteron aisle inner cellulose up to more than 10 times, and the softening ight soil that expands increases the ight soil amount, stimulates the wriggling of enteron aisle, quickens ight soil and discharges.Thereby play the anti-effect that treats constipation,, help controlling body weight, prevent energy surplus because its good retention ability and full effect can increase the satiety of stomach, thereby reduce total food intake dose.
The common vetch dish is the trade name of osmund and brake, in classification, belongs to the perennial pteridophyte of Osmundaceae Osmunda.The crude fiber content of common vetch dish is higher, belongs to kind higher in the edible wild herbs, and the cellulosic content of water-insoluble can reach 35%.
Present stage.The main path that utilizes the common vetch dish is that its young stem and leaf blanching is dried then, and it is edible to process dried vegetable.In addition; Li Fengxia utilizes alkaline process to extract the research of the dietary fiber in the Dried Osmund; But the cellulosic purity of the water-insoluble in the water insoluble dietary fiber of its extraction is lower; The impurity that contains other like lignin, protein, hemicellulose etc., does not meet market to the cellulosic requirement of water-insoluble.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method of extracting common vetch dish water insoluble dietary fiber, and this method has higher insoluble diedairy fiber yield, and cellulosic purity is higher in the insoluble diedairy fiber for preparing.
The present invention solves the problems of the technologies described above the technical scheme that is adopted: a kind of method of extracting common vetch dish water insoluble dietary fiber may further comprise the steps:
Step 1) degreasing: make the degreasing of common vetch dish, oven dry, prepare the Dried Osmund after the degreasing;
Step 2) enzymolyzing alpha-amylase: the water logging bubble 20-60min doubly of the Dried Osmund quality 10-25 after the Dried Osmund that step 1) is obtained uses quality as degreasing; Add AMS then and carry out enzyme digestion reaction, filtration obtains the filter residue A behind the enzyme digestion reaction, and washing filter residue A is to neutral; Said AMS addition 0.6～0.8%; Enzymolysis pH value 5.8～6.5,30～40 ℃ of hydrolysis temperatures, enzymolysis time 0.5～1.5h; With
Step 3) alkali lye hydrolysis: make step 2) the filter residue A after the processing soaks 0.5～2h in 0.3mol/L～1mol/L sodium hydroxide solution; The addition of said NaOH is calculated with solid-liquid ratio 1: 8～20; Making the sodium hydroxide solution temperature in the immersion process is 60～75 ℃; Filtration obtains filter residue B, and washing filter residue B is to neutral, and the filter residue B of gained is common vetch dish water insoluble dietary fiber.
In the technique scheme, the quality that said AMS addition 0.6～0.8% is meant AMS is 0.6～0.8% with respect to the quality of Dried Osmund.
The method of extraction common vetch dish water insoluble dietary fiber of the present invention also comprises step 4) delignification: the filter residue B delignification after step 3) is handled obtains the common vetch dish water insoluble dietary fiber after the delignification.
Said delignified concrete steps are: press solid-liquid ratio 1: 10-20 among the filter residue B after said step 3) is handled and add distilled water, press solid-liquid ratio 1: 0.1-0.2 adding glacial acetic acid, press solid-liquid ratio 1: 0.1-0.2 adding sodium chlorite, the back that stirs is at 60-80 ℃ of water-bath heating 0.5-1.5h; Washing is to neutral then, and washing with acetone filters, and drying obtains filter residue C, promptly obtains the common vetch dish water insoluble dietary fiber after the delignification.
The concrete steps of said step 1) are: the common vetch dish is dried into Dried Osmund, Dried Osmund is pulverized, add ethyl acetate then and at room temperature soak 2h～8h, pulverize once more after the oven dry, cross 40 mesh sieves, obtain the Dried Osmund after the degreasing.Wherein, after Dried Osmund soaks and finishes, can to remove residual organic solvent, carry out drying again in ethyl acetate earlier with the distilled water washing.Said room temperature is meant 20 ℃～25 ℃.
Said step 2) in, said AMS addition 0.7%, enzymolysis pH value 5.8,35 ℃ of hydrolysis temperatures, enzymolysis time 1.0h.Adopt this enzyme digestion reaction condition, the enzymatic hydrolyzation maximum that obtains is 60.68%.
In the said step 3), said NaOH concentration is 0.5mol/L, and the temperature in the said immersion process is 65 ℃, and the time of said immersion is 2.0h, and the solid-liquid ratio of the addition of said NaOH is 1: 10.The insoluble diedairy fiber yield that adopts this basic hydrolysis condition to record is 38.86%.
Said drying can adopt this area method commonly used, like drying box etc., as puts into 60 ℃ drying box baking 5h oven dry.
" solid-liquid ratio " described in this paper notion, quality that refers to solid-state " material " and the ratio that adds as the volume of " liquid " of leaching liquor.The unit of " material " is with g, mg, and the unit of " liquid " is with L, mL, so there are g/L, mg/L, g/mL, mg/mL etc. in the unit of " solid-liquid ratio ".
In sum, the present invention compared with prior art has following advantage:
(1) inventor has studied the water insoluble dietary fiber extraction process of common vetch dish, chooses the enzyme-chemically combined techniques and handles the common vetch dish, removes starch with AMS, and alkali lye is removed protein and fat.Optimize enzymolyzing alpha-amylase technology and alkali lye hydrolysis process based on the response surface method, be used to extract common vetch dish water insoluble dietary fiber.Remove the lignin in the common vetch dish water insoluble dietary fiber then, obtain having the cellulosic insoluble diedairy fiber of higher degree.The removal efficiency of lignin can reach 80-85% in the inventive method, and the yield that the common vetch dish water insoluble dietary fiber that finally prepares is can reach 37.92%, and purity can reach 97.57%, its its retention ability 7.22 (g/g), swellbility 6.52 (ml/g).
(2) to be used for the raw material of separation and Extraction insoluble diedairy fiber be southern common vetch dish in the present invention.It is higher that south common vetch dish and northern common vetch dish are compared content of cellulose.The present invention helps promoting the deep processing research of common vetch dish, has made full use of the common vetch dish resource of China, is the new field of processing and utilization developing of common vetch dish.
Description of drawings
Fig. 1 and Fig. 2 are the response surface solid and the contour maps of amylase addition and hydrolysis temperature;
Fig. 3 and Fig. 4 are the response surface solid and the contour maps of pH value of solution value and hydrolysis temperature;
Fig. 5 and Fig. 6 are the response surface solid and the contour maps of pH value of solution value and enzymolysis time;
Fig. 7 and Fig. 8 are the response surface solid and the contour maps of alkali soak time and NaOH concentration;
Fig. 9 and Figure 10 are the response surface solid and the contour maps of solid-liquid ratio and NaOH concentration;
Figure 11 and Figure 12 are the response surface solid and the contour maps of solid-liquid ratio and alkali soaking temperature;
Figure 13 and Figure 14 are the response surface solid and the contour maps of solid-liquid ratio and alkali soak time.
The specific embodiment
Below in conjunction with specific embodiment the present invention is described further.Specialize like nothing, the used raw material of the present invention is commercial.
AMS, citric acid, NaOH, ethyl acetate, natrium carbonicum calcinatum, glacial acetic acid, sodium chlorite, acetone, ethanol; Test the enzyme 2000U/g of being alive of used AMS, it is pure that reagent is analysis.Instrument is mainly DZF-6210 type vacuum drying chamber, Neofuge23R type desk type high speed refrigerated centrifuge, FE20 type laboratory pH meter etc.
Be the convenient yield that calculates each step, following examples 1 and 2 are undertaken by flow process shown in Figure 2.
Embodiment 1 produces common vetch dish water insoluble dietary fiber
Extract the method for common vetch dish water insoluble dietary fiber, may further comprise the steps: (concrete parameter is seen table 1):
1) degreasing: Dried Osmund is pulverized Dried Osmund with pulverizer; Add ethyl acetate then and at room temperature soak 3h, remove residual organic solvent with distilled water again, after the suction filtration oven dry once more to its pulverizing; Cross 40 mesh sieves, it is subsequent use that the degreasing sample that obtains is put into drying basin.
2) α-Dian Fenmeishuixie; The Dried Osmund powder of 10g degreasing is placed the beaker of 500ml, add distilled water at 1: 20 and stir, soak 30min by solid-liquid ratio; The citric acid solution (or 1.0g/L sodium carbonate liquor) that adds 2.5g/L; The pH value is adjusted to certain numerical value, adds a certain amount of AMS, the thermostat water bath of putting into uniform temperature carries out enzymolysis; Filter then and obtain filter residue A, washing filter residue A is to neutral;
3) alkali lye hydrolysis: add certain density sodium hydroxide solution by certain solid-liquid ratio, the thermostat water bath of putting into uniform temperature is hydrolyzed, and then filters and obtain filter residue B, and cyclic washing filter residue B is until neutrality;
4) drying box of putting into 60 ℃ dries by the fire 5h, is common vetch dish water insoluble dietary fiber after the pulverizing;
5) remove lignin: in common vetch dish water insoluble dietary fiber sample, press solid-liquid ratio and add distilled water at 1: 13, press solid-liquid ratio adding in 1: 0.1 glacial acetic acid, press solid-liquid ratio adding in 1: 0.12 sodium chlorite; Seal with plastic sheeting after stirring; The thermostat water bath of putting into 75 ℃ heats, and body should be often shaken in attention.The glacial acetic acid and the clorox that add same ratio behind the 1h once more continue in water-bath, to heat 1h, repeat this step altogether 3 times; Be neutral with the distilled water cyclic washing until filtrating then; Then wash with acetone, the baking oven of putting into 60 ℃ is at last dried to constant weight, obtains filter residue C.
2, the method for assay
1) assay method of enzymolyzing alpha-amylase rate
The enzymolyzing alpha-amylase rate is calculated by following formula: enzymatic hydrolyzation=(M1-m1)/M1
In the formula: m1 for experiment after the quality of the water insoluble dietary fiber that obtains, unit is g; M1 is the Dried Osmund powder quality of the degreasing that after pretreatment of raw material, takes by weighing, and unit is g.
2) mensuration of water insoluble dietary fiber yield
The water insoluble dietary fiber yield of common vetch dish is calculated by following formula: water insoluble dietary fiber yield=m2/M1
In the formula: m2 is the quality of experiment back gained water insoluble dietary fiber, and unit is g; M1 is the Dried Osmund powder quality of the degreasing that after pretreatment of raw material, takes by weighing, and unit is g.
3) experimental design and data
Use response surface software Design-Expert and EXCEL
3, experimental result and analysis
3.1 the research that enzymolyzing alpha-amylase is handled
3.1.1 the response surface optimization that enzymolyzing alpha-amylase is handled is analyzed
Adopt the enzyme-chemically combined techniques to produce common vetch dish water insoluble dietary fiber and compare with only producing with chemical method, the finished product purity that makes is higher, better quality.Before basic hydrolysis, use AMS to handle Dried Osmund earlier, can remove the starch in its protein network structure, help alkali lye and infiltrate more apace, make the protein alkaline hydrolysis more complete, also reduce the time of basic hydrolysis to remove protein.
At the experiment of single factor of AMS as a result on the basis, according to the center combination experimental design principle of Box-Benhnken, with amylase concentration; Optimum pH; Optimum temperature, enzymolysis time are independent variable, and the enzymolyzing alpha-amylase rate is a response; Utilize Design-Exper software to design the quadratic regression equation match independent variable of four factors, three levels and the functional relation between the enzymolyzing alpha-amylase rate, utilize the response surface analysis method to optimize diastatic enzymolysis process.Response surface factor and level are chosen and are seen table 1, and experimental design and result see table 2, and table 3 is seen in variance analysis.
The response surface experimental factor water-glass of table 1 enzymolyzing alpha-amylase
Table 2 enzymolyzing alpha-amylase response surface experimental design and result
Table 3 enzymolyzing alpha-amylase response surface test analysis of variance table
Annotate: P＜0.05 is remarkable for influence, with " * " expression; P＜0.01 is extremely remarkable for influence, with " * * " expression.
Can know that by table 3 the descending arrangement of the influence degree of each factor is followed successively by enzymolysis time, pH value of solution value, amylase addition, hydrolysis temperature.Carry out the response surface regression analysis through software Design-Expert his-and-hers watches 4; The response surface analysis solid and the contour map of gained are seen Fig. 1 to Fig. 6; Data in the his-and-hers watches 4 are carried out regression fit simultaneously, and the quadratic regression equation that obtains is following: Y=-319.23725+410.15167A+74.83533B+1.36270C-3.55467D-4.05 AB+4.9AD-1.155AC+0.583BC+4.36BD-0.087CD-256.65A
2-8.246B
2-0.05851C
2-10.401D
2
Can be known that by table 3 the F value of this model is 61.73, P value＜0.01 explains that this model is extremely significant.A, B, C, D, BC, BD, A in this model in addition
2, B
2, C
2, D
2P value＜0.01, show the influence of enzymolyzing alpha-amylase extremely remarkable.P value＜0.05 of AC representes that its influence to enzymolyzing alpha-amylase is remarkable.Draw through the response surface software analysis, the value of this model signal to noise ratio Adeq Precision is 27.076, explains that this model can be used for prediction.The adjustment of model confirms that the value of coefficient Adj R-Squared is 0.9681, explains that this model can explain that 96.81% response changes.The value of definite coefficients R-Squared of model is 0.9841.
Can know that by Fig. 1 to Fig. 3 along with the increase of each factor, the response face amount also increases gradually.After the response face amount increased to extreme value, the response face amount reduced along with the increase of each factor gradually.Learn that through the analysis of response surface method optimal value the enzymatic hydrolyzation maximum in trial stretch is 60.45%, corresponding enzymolysis optimum process parameter is an AMS addition 0.69%, pH value of solution value 5.82,33.04 ℃ of hydrolysis temperatures, enzymolysis time 1.07h.
3, the prediction of optimum process condition and checking
According to the experimental model that response surface software draws, the optimum process condition that dopes under the theoretical condition is an AMS addition 0.69%, pH value of solution value 5.82, and 33.04 ℃ of hydrolysis temperatures, enzymolysis time 1.07h, corresponding enzymatic hydrolyzation maximum is 60.45%.Facility for practical operation is modified to optimal value: AMS addition 0.7%, pH value of solution value 5.8,35 ℃ of hydrolysis temperatures, enzymolysis time 1.0h.The actual enzymatic hydrolyzation maximum that records is 60.68%, is about 0.23% with the error of theoretical value.Therefore, based on the optimization extraction process parameter of response surface method gained accurately and reliably, has practical value.
Embodiment 2 basic hydrolysis Study on extraction process
1, basic hydrolysis extraction process response surface method optimization research
The purpose that adopts basic hydrolysis is the protein of removing in the common vetch dish and fat; Alkali lye through the short period low concentration is handled the amino acid that the protein in the common vetch dish is decomposed into small-molecular peptides and dissociates; Fat helps through filter wash it being removed because saponification is decomposed into the salt of glycerine and aliphatic acid.In addition, the AMS inactivation that the front is added that also has a purpose just to be.
Confirm the experiment of single factor that carries out basic hydrolysis on the basis of optimum process condition of enzymolyzing alpha-amylase through the response surface method; The experiment of single factor result of comprehensive then basic hydrolysis is according to the center combination experimental design principle of Box-Benhnken, with solid-liquid ratio; NaOH concentration; Alkali soak time, alkali soaking temperature are independent variable, and the insoluble diedairy fiber recovery rate is a response; Utilize Design-Expert software to design the quadratic regression equation match independent variable of four factors, three levels and the functional relation between the insoluble diedairy fiber recovery rate, adopt the response surface analysis method to optimize basic hydrolysis technology.Response surface factor and level are chosen and are seen table 4, and experimental design and result see table 5, and table 6 is seen in variance analysis.
The response surface experimental factor water-glass of table 4 basic hydrolysis
The response surface experimental design and the result of table 5 basic hydrolysis
The response surface test analysis of variance table of table 6 basic hydrolysis
Annotate: P＜0.05 is remarkable for influence, with " * " expression; P＜0.01 is extremely remarkable for influence, with " * * " expression.
Can know that by table 6 each factor is followed successively by the alkali soaking temperature to the influence degree size of basic hydrolysis, NaOH concentration, alkali soak time, solid-liquid ratio.Carry out the response surface regression analysis through software Design-Expert his-and-hers watches 5, the response surface analysis solid and the contour map of gained are seen Fig. 4 to Fig. 6, and be following according to the quadratic regression equation that the data of table 5 draw:
Y＝-144.49717+79.097A+2.70785B+11.63283C+13.56958D-0.101AB-7.42AC-1.66AD-0.0205BC+0.09875BD+3.335CD-43.90533A2-0.028603B2-10.26133C2-1.27908D2
Can know that according to table 6 the F value of this quadratic regression equation model is 150.76, P value＜0.01 this model of explanation is extremely significant.In this model, the P value of A, B, C, D, AC, AD, BD, CD, A2, B2, C2 explains that less than 0.01 these several the yield influences to insoluble diedairy fiber are extremely remarkable; The P value of D2 explains that less than 0.05 these several the yield influences to insoluble diedairy fiber are remarkable.Draw through the response surface software analysis, the adjustment of this model confirms that coefficient Adj R-Squared value is 0.9864, explains that this model can explain the variation of 98.64% response.In addition, the value of signal to noise ratio Adeq Precision is 39.434, explains that this model can be used for prediction.
Can know that by Fig. 4 to Fig. 6 the response face amount is that the yield of insoluble diedairy fiber increases along with the increase of the numerical value of each factor gradually.After the response face amount increased to extreme value, the response face amount reduced along with the increase of the numerical value of each factor gradually.Learn that through the analysis of response surface method optimal value the insoluble diedairy fiber yield maximum in trial stretch is 38.64%, analyze peak at A=0.47, B=63.01, C=1.95, D=9.98.The best alkaline hydrolysis technological parameter of promptly producing common vetch dish water insoluble dietary fiber is NaOH concentration 0.47mol/L, and the alkali soaking temperature is 63.01 ℃, and the alkali soak time is 1.95h, and solid-liquid ratio is 1: 9.98.
2, the prediction of optimum process condition and checking
The experimental model that draws according to response surface software; Dope that the best alkaline hydrolysis technological parameter of common vetch dish water insoluble dietary fiber is NaOH concentration 0.47mol/L under the theoretical condition; The alkali soaking temperature is 63.01 ℃; The alkali soak time is 1.95h, and solid-liquid ratio is 1: 9.98, and the maximum yield of insoluble diedairy fiber is 38.64%.Facility for practical operation is modified to optimal value: best alkaline hydrolysis technological parameter is NaOH concentration 0.5mol/L, and the alkali soaking temperature is 65 ℃, and the alkali soak time is 2h, and solid-liquid ratio is 1: 10.The actual yield value that records is 38.86%, is about 0.22% with the error of theoretical value.Therefore, based on the optimization extraction process parameter of response surface method gained accurately and reliably, has practical value.
Obviously, obtaining the revised technological parameter of enzymolysis processing through the response surface test is AMS addition 0.7%, pH value of solution value 5.8,35 ℃ of hydrolysis temperatures, enzymolysis time 1.0h.The actual enzymatic hydrolyzation maximum that records is 60.68%.The optimal processing parameter of alkaline hydrolysis correction is NaOH concentration 0.5mol/L, and the alkali soaking temperature is 65 ℃, and the alkali soak time is 2h, and solid-liquid ratio is 1: 10.The maximum yield of the actual insoluble diedairy fiber that records is 38.86%.And obtaining two quadratic equation models of handling each variable factors, this regression models is extremely remarkable, to the test better fitting, certain using value is arranged.
Embodiment 3
1) degreasing: Dried Osmund is pulverized Dried Osmund with pulverizer; Add ethyl acetate then and at room temperature soak 3h, remove residual organic solvent with distilled water again, after the suction filtration oven dry once more to its pulverizing; Cross 40 mesh sieves, it is subsequent use that the degreasing sample that obtains is put into drying basin.
Step 2) enzymolyzing alpha-amylase: the water logging bubble 20-60min doubly of the Dried Osmund quality 10-25 after using quality as degreasing the Dried Osmund after the degreasing; Add AMS then and carry out enzyme digestion reaction; Filtration obtains the filter residue A behind the enzyme digestion reaction, said AMS addition 0.7%, enzymolysis pH value 5.8; 35 ℃ of hydrolysis temperatures, enzymolysis time 1.0h; The enzymatic hydrolyzation that records behind this step enzymolysis is 60.68%.
Step 3) alkali lye hydrolysis: the sodium hydroxide solution that adds 0.5mol/L by 1: 10 solid-liquid ratio; The thermostat water bath of putting into 65 ℃ is hydrolyzed; And then filter and obtain filter residue B, cyclic washing filter residue B is until neutrality, and the filter residue B of gained is common vetch dish water insoluble dietary fiber.The filter residue B of gained puts into 60 ℃ drying box and dries by the fire 5h, and the common vetch dish water insoluble dietary fiber that is powdered after the pulverizing is plain.The insoluble diedairy fiber yield that adopts this basic hydrolysis condition to record is 38.86%.
4) remove lignin: press solid-liquid ratio among the filter residue B after said step 3) is handled and add distilled water at 1: 13, press solid-liquid ratio adding in 1: 0.1 glacial acetic acid, press solid-liquid ratio adding in 1: 0.12 sodium chlorite; Seal with plastic sheeting after stirring; The thermostat water bath of putting into 75 ℃ heats, and body should be often shaken in attention.The glacial acetic acid and the clorox that add same ratio behind the 1h once more continue in water-bath, to heat 1h, repeat this step altogether 3 times; Be neutral with the distilled water cyclic washing until filtrating then; Then wash with acetone, the baking oven of putting into 60 ℃ is at last dried to constant weight, obtains filter residue C.The removal efficiency of lignin can reach 80-85%, and the yield that obtains common vetch dish water insoluble dietary fiber and be is 37.92%, and purity reaches 97.57%.Obtain insoluble diedairy fiber and contain cellulose, hemicellulose A and hemicellulose B, its retention ability 7.22 (g/g), swellbility 6.52 (ml/g).
Embodiment 4
1) degreasing: Dried Osmund is pulverized Dried Osmund with pulverizer; Add ethyl acetate then and at room temperature soak 2h, remove residual organic solvent with distilled water again, after the suction filtration oven dry once more to its pulverizing; Cross 40 mesh sieves, it is subsequent use that the degreasing sample that obtains is put into drying basin.
Step 2) enzymolyzing alpha-amylase: the water logging bubble 20-60min doubly of the Dried Osmund quality 10-25 after using quality as degreasing the Dried Osmund after the degreasing; Add AMS then and carry out enzyme digestion reaction; Filtration obtains the filter residue A behind the enzyme digestion reaction, said AMS addition 0.6%, enzymolysis pH value 5.8; 30 ℃ of hydrolysis temperatures, enzymolysis time 1.0h; The enzymatic hydrolyzation maximum that obtains is 59.38%.
Step 3) alkali lye hydrolysis: the sodium hydroxide solution that adds 0.5mol/L by 1: 9 solid-liquid ratio; The thermostat water bath of putting into 55 ℃ is hydrolyzed; And then filter and obtain filter residue B, cyclic washing filter residue B is until neutrality, and the filter residue B of gained is common vetch dish water insoluble dietary fiber.The filter residue B of gained puts into 60 ℃ drying box and dries by the fire 5h, and the common vetch dish water insoluble dietary fiber that is powdered after the pulverizing is plain.The insoluble diedairy fiber yield that adopts this basic hydrolysis condition to record is 36.11%.
4) remove lignin: press solid-liquid ratio among the filter residue B after said step 3) is handled and add distilled water at 1: 13, press solid-liquid ratio adding in 1: 0.1 glacial acetic acid, press solid-liquid ratio adding in 1: 0.12 sodium chlorite; Seal with plastic sheeting after stirring; The thermostat water bath of putting into 75 ℃ heats, and body should be often shaken in attention.The glacial acetic acid and the clorox that add same ratio behind the 1h once more continue in water-bath, to heat 1h, repeat this step altogether 3 times; Be neutral with the distilled water cyclic washing until filtrating then; Then wash with acetone, the baking oven of putting into 60 ℃ is at last dried to constant weight, obtains filter residue C.The removal efficiency of lignin can reach 80-85%, and the yield that obtains common vetch dish water insoluble dietary fiber and be is 35.24%, and purity reaches 90.67%.Obtain insoluble diedairy fiber and contain cellulose, hemicellulose A and hemicellulose B, its retention ability 6.87 (g/g), swellbility 6.02 (ml/g).
Claims (6)
1. a method of extracting common vetch dish water insoluble dietary fiber is characterized in that, may further comprise the steps:
Step 1) degreasing: make the degreasing of common vetch dish, oven dry, prepare the Dried Osmund after the degreasing;
Step 2) enzymolyzing alpha-amylase: the water logging bubble 20-60min doubly of the Dried Osmund quality 10-25 after the Dried Osmund that step 1) is obtained uses quality as degreasing; Add AMS then and carry out enzyme digestion reaction, filtration obtains the filter residue A behind the enzyme digestion reaction, and washing filter residue A is to neutral; Said AMS addition 0.6～0.8%; Enzymolysis pH value 5.8～6.5,30～40 ℃ of hydrolysis temperatures, enzymolysis time 0.5～1.5h; With
Step 3) alkali lye hydrolysis: make step 2) the filter residue A after the processing soaks 0.5～2h in 0.3mol/L～1mol/L sodium hydroxide solution; The addition of said NaOH is calculated with solid-liquid ratio 1: 8～20; Making the sodium hydroxide solution temperature in the immersion process is 60～75 ℃; Filtration obtains filter residue B, and washing filter residue B is to neutral, and the filter residue B of gained is common vetch dish water insoluble dietary fiber.
2. the method for extraction common vetch dish water insoluble dietary fiber according to claim 1 is characterized in that, also comprises step 4) delignification: the filter residue B delignification after step 3) is handled obtains the common vetch dish water insoluble dietary fiber after the delignification.
3. the method for extraction common vetch dish water insoluble dietary fiber according to claim 2; It is characterized in that; Said delignified concrete steps are: press solid-liquid ratio 1: 10-20 among the filter residue B after said step 3) is handled and add distilled water, press solid-liquid ratio 1: 0.1-0.2 adding glacial acetic acid, press solid-liquid ratio 1: 0.1-0.2 adding sodium chlorite, the back that stirs is at 60-80 ℃ of water-bath heating 0.5-1.5h; Washing is to neutral then, and washing with acetone filters, and drying obtains filter residue C, promptly obtains the common vetch dish water insoluble dietary fiber after the delignification.
4. the method for extraction common vetch dish water insoluble dietary fiber according to claim 3; It is characterized in that the concrete steps of said step 1) are: the common vetch dish is dried into Dried Osmund, Dried Osmund is pulverized; Add ethyl acetate then and at room temperature soak 2h～8h; Pulverize once more after the oven dry, cross 40 mesh sieves, obtain the Dried Osmund after the degreasing.
5. the method for extraction common vetch dish water insoluble dietary fiber according to claim 4 is characterized in that said step 2) in, said AMS addition 0.7%, enzymolysis pH value 5.8,35 ℃ of hydrolysis temperatures, enzymolysis time 1.0h.
6. the method for extraction common vetch dish water insoluble dietary fiber according to claim 5; It is characterized in that; In the said step 3), said NaOH concentration is 0.5mol/L, and the temperature in the said immersion process is 65 ℃; The time of said immersion is 2.0h, and the solid-liquid ratio of the addition of said NaOH is 1: 10.
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| CN103211231A (en) * | 2013-05-07 | 2013-07-24 | 西北民族大学 | Process for producing dietary fibers and trace element leaf fertilizer by utilizing vegetable waste |
| CN103211231B (en) * | 2013-05-07 | 2014-04-30 | 西北民族大学 | Process for producing dietary fibers and trace element leaf fertilizer by utilizing vegetable waste |
| CN103652307A (en) * | 2013-12-03 | 2014-03-26 | 山西医科大学 | Method for extracting leaf proteins from broussonetia papyrifera leaf dry powder and comprehensive utilization of waste |
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| CN105919139A (en) * | 2016-05-03 | 2016-09-07 | 上海交通大学 | Method for improving highland barley dietary fiber extraction rate based on response surface method |
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| CN107280018A (en) * | 2017-08-15 | 2017-10-24 | 江南大学 | A kind of preparation method of rice bran insoluble diedairy fiber |
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