CN102640905B - 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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- 238000000034 method Methods 0.000 title claims abstract description 46
- 235000013325 dietary fiber Nutrition 0.000 title claims abstract description 45
- 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 15
- 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 62
- 244000105017 Vicia sativa Species 0.000 claims description 50
- 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 14
- 239000012153 distilled water Substances 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 12
- 238000000605 extraction Methods 0.000 claims description 11
- 238000002791 soaking Methods 0.000 claims description 11
- 229960000583 acetic acid Drugs 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 239000012362 glacial acetic acid Substances 0.000 claims description 9
- 238000001976 enzyme digestion Methods 0.000 claims description 8
- 230000007935 neutral effect Effects 0.000 claims description 8
- 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
- 239000008236 heating water Substances 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
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- 238000013401 experimental design 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
- 238000011160 research Methods 0.000 description 5
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- 239000003960 organic solvent Substances 0.000 description 4
- 239000002994 raw material Substances 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
- 238000013461 design Methods 0.000 description 3
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- 229920006255 plastic film Polymers 0.000 description 3
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- 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
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- 238000011084 recovery Methods 0.000 description 2
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- 238000010993 response surface methodology 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
- 238000005211 surface analysis Methods 0.000 description 2
- 235000013311 vegetables Nutrition 0.000 description 2
- 206010010774 Constipation Diseases 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
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- 241000196127 Osmunda Species 0.000 description 1
- 206010033546 Pallor Diseases 0.000 description 1
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- 239000002253 acid Substances 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, is also a kind of inexhaustible renewable resource.Cellulose contains great amount of hydroxy group, adsorbs polar water molecules by hydroxyl and makes cellulose have good retentiveness.In general, the retention ability of high-quality water insoluble dietary fiber element 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, accelerates ight soil and discharges.Thereby play the anti-effect that treats constipation, due to its good retention ability and full effect, can increase the satiety of stomach, thereby reduce total food intake dose, be conducive to control body weight, prevent energy surplus.
The common vetch dish is the trade name of osmund and brake, belongs to the perennial pteridophyte of Osmundaceae Osmunda in classification.The crude fiber content of common vetch dish is higher, belongs to kind higher in 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 then its young stem and leaf blanching is dried, and makes dried vegetable edible.In addition, Li Fengxia utilizes alkaline process to extract the research of the dietary fiber in 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, as lignin, protein, hemicellulose etc., do 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 the method has higher insoluble diedairy fiber yield, and in the insoluble diedairy fiber for preparing, cellulosic purity is higher.
The present invention solves the problems of the technologies described above the technical scheme that adopts: a kind of method of extracting common vetch dish water insoluble dietary fiber comprises the following steps:
Step 1) degreasing: make the degreasing of common vetch dish, oven dry, prepare the Dried Osmund after degreasing;
Step 2) the Dried Osmund quality that enzymolyzing alpha-amylase: with step 1) obtains is the Dried Osmund quality 10-25 water soaking 20-60min doubly after degreasing, then add AMS to carry out enzyme digestion reaction, filtration obtains the filter residue A after enzyme digestion reaction, washing filter residue A is to neutral, described 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 processing soaks 0.5～2h in 0.3mol/L～1mol/L sodium hydroxide solution, the addition of described NaOH is calculated with solid-liquid ratio 1: 8～20, making the sodium hydroxide solution temperature in immersion process is 60～75 ℃, filtration obtains filter residue B, washing filter residue B is to neutral, and the filter residue B of gained is common vetch dish water insoluble dietary fiber.
In technique scheme, the quality that described AMS addition 0.6～0.8% refers to 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: make step 3) filter residue B delignification after processing, obtain the common vetch dish water insoluble dietary fiber after delignification.
Described delignified concrete steps are: to described step 3) in filter residue B after processing by solid-liquid ratio 1: 10-20 add distilled water, by solid-liquid ratio 1: 0.1-0.2 add glacial acetic acid, by solid-liquid ratio 1: 0.1-0.2 adds sodium chlorite, stirs afterwards at 60-80 ℃ of heating water bath 0.5-1.5h; Then be washed to neutrality, acetone washing is filtered, and drying obtains filter residue C, namely obtains the common vetch dish water insoluble dietary fiber after delignification.
Described step 1) concrete steps are: the common vetch dish is dried into Dried Osmund, Dried Osmund is pulverized, then add ethyl acetate at room temperature to soak 2h～8h, again pulverize after oven dry, cross 40 mesh sieves, obtain the Dried Osmund after degreasing.Wherein, after Dried Osmund soaks in ethyl acetate and finishes, can be first with the distilled water washing, removing residual organic solvent, then carry out drying.Described room temperature refers to 20 ℃～25 ℃.
Described step 2) in, described AMS addition 0.7%, enzymolysis pH value 5.8,35 ℃ of hydrolysis temperatures, enzymolysis time 1.0h.Adopt this reaction conditions, the enzymatic hydrolyzation maximum that obtains is 60.68%.
Described step 3) in, described NaOH concentration is 0.5mol/L, and the temperature in described immersion process is 65 ℃, and the time of described immersion is 2.0h, and the solid-liquid ratio of the addition of described NaOH is 1: 10.The insoluble diedairy fiber yield that adopts this basic hydrolysis condition to record is 38.86%.
Described drying can adopt this area method commonly used, as drying box etc., as puts into the drying box baking 5h oven dry of 60 ℃.
Described " solid-liquid ratio " concept herein, the quality that refers to solid-state " material " and the ratio that adds as the volume of " liquid " of leaching liquor.The unit of " material " g, mg, 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 processes the common vetch dish, removes starch with AMS, and alkali lye is removed protein and fat.Optimize enzymolyzing alpha-amylase technique and alkali lye hydrolysis process based on the response surface method, be used for extracting common vetch dish water insoluble dietary fiber.Then remove the lignin in common vetch dish water insoluble dietary fiber, obtain having the cellulosic insoluble diedairy fiber of higher degree.In the inventive method, the removal efficiency of lignin can reach 80-85%, the yield that the common vetch dish water insoluble dietary fiber that finally prepares is can reach 37.92%, purity 97.57%, its its retention ability 7.22 (g/g), swellbility 6.52 (ml/g).
(2) the present invention is southern common vetch dish for separating of the raw material that extracts insoluble diedairy fiber.It is higher that south common vetch dish and northern common vetch dish are compared content of cellulose.The present invention is conducive to promote the deep processing research of common vetch dish, takes full advantage 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 response surface solid and the contour maps of amylase addition and hydrolysis temperature;
Fig. 3 and Fig. 4 are response surface solid and the contour maps of pH and hydrolysis temperature;
Fig. 5 and Fig. 6 are response surface solid and the contour maps of pH and enzymolysis time;
Fig. 7 and Fig. 8 are response surface solid and the contour maps of alkali soak time and NaOH concentration;
Fig. 9 and Figure 10 are response surface solid and the contour maps of solid-liquid ratio and NaOH concentration;
Figure 11 and Figure 12 are response surface solid and the contour maps of solid-liquid ratio and alkali soaking temperature;
Figure 13 and Figure 14 are response surface solid and the contour maps of solid-liquid ratio and alkali soak time.
The specific embodiment
The present invention is described further below in conjunction with specific embodiment.Specialize as nothing, the present invention's raw material used 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 AMS used, it is pure that reagent is analysis.Instrument is mainly DZF-6210 type vacuum drying chamber, Neofuge23R type table-type high-speed refrigerated centrifuge, FE20 type laboratory pH meter etc.
Calculate for convenience the yield of 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, comprise the following steps: (design parameter sees Table 1):
1) degreasing: Dried Osmund is pulverized Dried Osmund with pulverizer, then add ethyl acetate at room temperature to soak 3h, then remove residual organic solvent with distilled water, after the suction filtration oven dry again to its pulverizing, cross 40 mesh sieves, the degreasing sample that obtains is put into drying basin standby.
2) α-amylasehydrolysis; The Dried Osmund powder of 10g degreasing is placed in the beaker of 500ml, adds distilled water at 1: 20 and stir by solid-liquid ratio, soak 30min; 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, then filter 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 pulverizing;
5) remove lignin: add distilled water at 1: 13, add glacial acetic acid at 1: 0.1, add sodium chlorite at 1: 0.12 by solid-liquid ratio by solid-liquid ratio by solid-liquid ratio in common vetch dish water insoluble dietary fiber sample, the rear plastic film sealing of using stirs, 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 again add same ratio after 1h continue to heat 1h in water-bath, altogether repeat this step 3 times, then with the distilled water cyclic washing until filtrate is neutral, then wash with acetone, the baking oven of putting at last 60 ℃ is 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 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 takes after pretreatment of raw material, 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 formula: m2 is the quality of the rear gained water insoluble dietary fiber of experiment, and unit is g; M1 is the Dried Osmund powder quality of the degreasing that takes after pretreatment of raw material, unit is g.
3) experimental design and data are processed
Use response surface software Design-Expert and EXCEL
3, experimental result and analysis
3.1 the research that enzymolyzing alpha-amylase is processed
3.1.1 the response surface optimization that enzymolyzing alpha-amylase is processed 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.First use AMS to process Dried Osmund before basic hydrolysis, can remove the starch in its protein network structure, be conducive to alkali lye and infiltrate more rapidly to remove protein, make the protein alkaline hydrolysis more complete, also reduce the time of basic hydrolysis.
At the experiment of single factor of AMS as a result on the basis, center combination experimental design principle according to Box-Benhnken, with amylase concentration, optimum pH, optimum temperature, enzymolysis time are independent variable, and the enzymolyzing alpha-amylase rate is response, utilize the quadratic regression equation match independent variable of Design-Exper Software for Design four factor three levels and the functional relation between the enzymolyzing alpha-amylase rate, utilize Response surface methodology to optimize diastatic enzymolysis process.Response surface factor and level are chosen and are seen Table 1, experimental design and the results are shown in Table 2, and variance analysis sees Table 3.
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 impact, with " * " expression; P＜0.01 is extremely remarkable for impact, with " * * " expression.
As shown in Table 3, the descending arrangement of the influence degree of each factor is followed successively by enzymolysis time, pH, amylase addition, hydrolysis temperature.Carry out the response surface regression analysis by software Design-Expert his-and-hers watches 4, response surface analysis solid and the contour map of gained are seen Fig. 1 to Fig. 6, data in his-and-hers watches 4 are carried out regression fit simultaneously, and the quadratic regression equation that obtains is as follows: 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
As shown in Table 3, the F value of this model is 61.73, P value＜0.01, illustrates 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 impact of enzymolyzing alpha-amylase extremely remarkable.The P value of AC＜0.05 represents that its impact on enzymolyzing alpha-amylase is remarkable.Draw by the response surface software analysis, the value of this model signal to noise ratio Adeq Precision is 27.076, illustrates that this model can be used for prediction.The value of the adjustment Coefficient of determination Adj R-Squared of model is 0.9681, illustrates that this model can explain that 96.81% response changes.The value of definite coefficients R-Squared of model is 0.9841.
By Fig. 1 to Fig. 3 as can be known, 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 gradually along with the increase of each factor.Learn by the analysis of response surface method optimal value, the enzymatic hydrolyzation maximum in trial stretch is 60.45%, and corresponding enzymolysis optimal procedure parameters is AMS addition 0.69%, pH 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 theoretical condition is AMS addition 0.69%, pH 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 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 Optimized Extraction Process parameter of response surface method gained accurately and reliably, has practical value.
The research of embodiment 2 basic hydrolysis extraction processes
1, basic hydrolysis extraction process response surface method optimization research
The purpose that adopts basic hydrolysis is the protein and fat of removing in the common vetch dish, process by the alkali lye of short period low concentration the protein in the common vetch dish is decomposed into small-molecular peptides and free amino acid, fat is decomposed into the salt of glycerine and aliphatic acid due to saponification, be conducive to by filter wash, it be removed.In addition, also has the AMS inactivation that adds previously that makes that a purpose is just.
determine the experiment of single factor that carries out basic hydrolysis on the basis of optimum process condition of enzymolyzing alpha-amylase by the response surface method, then the experiment of single factor result of comprehensive basic hydrolysis, center combination experimental design principle according to Box-Benhnken, with solid-liquid ratio, NaOH concentration, the alkali soak time, the alkali soaking temperature is independent variable, the insoluble diedairy fiber recovery rate is response, utilize the quadratic regression equation match independent variable of Design-Expert Software for Design four factor three levels and the functional relation between the insoluble diedairy fiber recovery rate, adopt Response surface methodology to optimize basic hydrolysis technique.Response surface factor and level are chosen and are seen Table 4, experimental design and the results are shown in Table 5, and variance analysis sees Table 6.
The response surface experimental factor water-glass of table 4 basic hydrolysis
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 impact, with " * " expression; P＜0.01 is extremely remarkable for impact, with " * * " expression.
As shown in 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 by software Design-Expert his-and-hers watches 5, response surface analysis solid and the contour map of gained are seen Fig. 4 to Fig. 6, and be as follows 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
According to table 6 as can be known, the F value of this quadratic regression equation model is that 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 illustrates that less than 0.01 these several the yield impacts on insoluble diedairy fiber are extremely remarkable; The P value of D2 illustrates that less than 0.05 these several the yield impacts on insoluble diedairy fiber are remarkable.Draw by the response surface software analysis, the adjustment Coefficient of determination Adj R-Squared value of this model is 0.9864, illustrates 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, illustrates that this model can be used for prediction.
By Fig. 4 to Fig. 6 as can be known, the response face amount is yield increase gradually along with the increase of the numerical value of each factor of insoluble diedairy fiber.After the response face amount increased to extreme value, the response face amount reduced gradually along with the increase of the numerical value of each factor.Learn by the analysis of response surface method optimal value, the insoluble diedairy fiber yield maximum in trial stretch is 38.64%, analyzes peak at A=0.47, B=63.01, C=1.95, D=9.98.The best alkaline hydrolysis technological parameter of namely 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 under theoretical condition, the best alkaline hydrolysis technological parameter of common vetch dish water insoluble dietary fiber is NaOH concentration 0.47mol/L, the alkali soaking temperature is 63.01 ℃, the alkali soak time is 1.95h, 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 Optimized Extraction Process parameter of response surface method gained accurately and reliably, has practical value.
Obviously, test by response surface that to obtain the revised technological parameter of enzymolysis processing be AMS addition 0.7%, pH 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 processing each variable factors, this model returns extremely remarkable, and is better to the test match, and certain using value is arranged.
Embodiment 3
1) degreasing: Dried Osmund is pulverized Dried Osmund with pulverizer, then add ethyl acetate at room temperature to soak 3h, then remove residual organic solvent with distilled water, after the suction filtration oven dry again to its pulverizing, cross 40 mesh sieves, the degreasing sample that obtains is put into drying basin standby.
Step 2) enzymolyzing alpha-amylase: be Dried Osmund quality 10-25 water soaking 20-60min doubly after degreasing with the Dried Osmund quality after degreasing, then add AMS to carry out enzyme digestion reaction, filtration obtains the filter residue A after enzyme digestion reaction, described AMS addition 0.7%, enzymolysis pH value 5.8,35 ℃ of hydrolysis temperatures, enzymolysis time 1.0h; The enzymatic hydrolyzation that records after this step enzymolysis is 60.68%.
Step 3) alkali lye hydrolysis: the sodium hydroxide solution that adds 0.5mol/L by the solid-liquid ratio of 1: 10, 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 the drying box of 60 ℃ and dries by the fire 5h, is the common vetch dish water insoluble dietary fiber element of dry powder-shaped after pulverizing.The insoluble diedairy fiber yield that adopts this basic hydrolysis condition to record is 38.86%.
4) removal lignin: to described step 3) add distilled water at 1: 13, add glacial acetic acid at 1: 0.1, add sodium chlorite at 1: 0.12 by solid-liquid ratio by solid-liquid ratio by solid-liquid ratio in the filter residue B after processing, the rear plastic film sealing of using stirs, 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 again add same ratio after 1h continue to heat 1h in water-bath, altogether repeat this step 3 times, then with the distilled water cyclic washing until filtrate is neutral, then wash with acetone, the baking oven of putting at last 60 ℃ is 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).
1) degreasing: Dried Osmund is pulverized Dried Osmund with pulverizer, then add ethyl acetate at room temperature to soak 2h, then remove residual organic solvent with distilled water, after the suction filtration oven dry again to its pulverizing, cross 40 mesh sieves, the degreasing sample that obtains is put into drying basin standby.
Step 2) enzymolyzing alpha-amylase: be Dried Osmund quality 10-25 water soaking 20-60min doubly after degreasing with the Dried Osmund quality after degreasing, then add AMS to carry out enzyme digestion reaction, filtration obtains the filter residue A after enzyme digestion reaction, described 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 the solid-liquid ratio of 1: 9, 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 the drying box of 60 ℃ and dries by the fire 5h, is the common vetch dish water insoluble dietary fiber element of dry powder-shaped after pulverizing.The insoluble diedairy fiber yield that adopts this basic hydrolysis condition to record is 36.11%.
4) removal lignin: to described step 3) add distilled water at 1: 13, add glacial acetic acid at 1: 0.1, add sodium chlorite at 1: 0.12 by solid-liquid ratio by solid-liquid ratio by solid-liquid ratio in the filter residue B after processing, the rear plastic film sealing of using stirs, 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 again add same ratio after 1h continue to heat 1h in water-bath, altogether repeat this step 3 times, then with the distilled water cyclic washing until filtrate is neutral, then wash with acetone, the baking oven of putting at last 60 ℃ is 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 (5)
1. a method of extracting common vetch dish water insoluble dietary fiber, is characterized in that, comprises the following steps:
Step 1) degreasing: make the degreasing of common vetch dish, oven dry, prepare the Dried Osmund after degreasing;
Step 2) enzymolyzing alpha-amylase: the Dried Osmund quality that step 1) is obtained is the Dried Osmund quality 10-25 water soaking 20-60min doubly after degreasing, then add AMS to carry out enzyme digestion reaction, filtration obtains the filter residue A after enzyme digestion reaction, washing filter residue A is to neutral, described 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 processing soaks 0.5～2h in 0.3mol/L～1mol/L sodium hydroxide solution, the addition of described NaOH is calculated with solid-liquid ratio 1:8～20, making the sodium hydroxide solution temperature in immersion process is 60～75 ℃, filtration obtains filter residue B, washing filter residue B is to neutral, and the filter residue B of gained is common vetch dish water insoluble dietary fiber;
Step 4) delignification: the filter residue B delignification after step 3) is processed obtains the common vetch dish water insoluble dietary fiber after delignification.
2. the method for extraction common vetch dish water insoluble dietary fiber according to claim 1, it is characterized in that, described delignified concrete steps are: add distilled water, add glacial acetic acid, add sodium chlorite by solid-liquid ratio 1:0.1-0.2 by solid-liquid ratio 1:0.1-0.2 by solid-liquid ratio 1:10-20 in the filter residue B after processing to described step 3), stir rear at 60-80 ℃ of heating water bath 0.5-1.5h; Then be washed to neutrality, acetone washing is filtered, and drying obtains filter residue C, namely obtains the common vetch dish water insoluble dietary fiber after delignification.
3. the method for extraction common vetch dish water insoluble dietary fiber according to claim 2, it is characterized in that, the concrete steps of described step 1) are: the common vetch dish is dried into Dried Osmund, Dried Osmund is pulverized, then add ethyl acetate at room temperature to soak 2h～8h, again pulverize after oven dry, cross 40 mesh sieves, obtain the Dried Osmund after degreasing.
4. the method for extraction common vetch dish water insoluble dietary fiber according to claim 3, is characterized in that described step 2) in, described AMS addition 0.7%, enzymolysis pH value 5.8,35 ℃ of hydrolysis temperatures, enzymolysis time 1.0h.
5. the method for extraction common vetch dish water insoluble dietary fiber according to claim 4, it is characterized in that, in described step 3), described NaOH concentration is 0.5mol/L, temperature in described immersion process is 65 ℃, the time of described immersion is 2.0h, and the solid-liquid ratio of the addition of described NaOH is 1:10.
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