CN105795355B - Method for increasing content of soluble dietary fiber in black soybean hulls - Google Patents
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- A—HUMAN NECESSITIES
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Abstract
The invention discloses a method for improving the content of soluble dietary fiber in black bean curd skin, and particularly provides a method for improving the content of soluble dietary fiber in black bean curd skin, which comprises the following steps: (i) providing black bean curd skin; (ii) under an alkaline condition, mixing the black bean skin with an alkaline solution to obtain a first mixed solution, wherein the concentration of the alkaline hydrogen peroxide solution is 8-30%; and (iii) drying the first mixed liquor obtained in step (ii), thereby obtaining a modified black soybean hull having an increased content of soluble dietary fibers. The soluble dietary fiber obtained by the method of the invention is up to 16.15% on average.
Description
Technical Field
The invention relates to the technical field of biology, in particular to a method for improving the content of soluble dietary fibers in black bean skins.
Background
The black beans are black seeds of soybeans of leguminous plants, the black bean skins are generally waste materials in the food industry, the research on the black bean skins in the prior art focuses on the extraction and property research of pigments, such as anthocyanin, haematochrome and some glucoside, of the black bean skins, and reports that the extract of the black bean skins can improve the absorption of iron elements in organisms are also provided. However, there are few studies on the direction of dietary fiber in black bean skin.
The dietary fiber is carbohydrate which can hardly generate heat, is essentially polysaccharide substances which cannot be decomposed by digestive enzymes of a human body in the carbohydrate, and has certain physiological functions, such as reducing blood fat, regulating blood sugar, preventing colon cancer, regulating body immunity and the like. Dietary fiber can be classified into Soluble Dietary Fiber (SDF) and Insoluble Dietary Fiber (IDF) according to its water solubility; many studies have shown that soluble dietary fibers not only have better physicochemical properties, but also have a stronger physiological function in many respects than insoluble dietary fibers. Therefore, modification studies on dietary fibers at present mostly focus on improving the content or extraction rate of soluble dietary fibers, and enzymatic modification, chemical modification and physical modification are commonly adopted.
In the conventional dietary fiber modification method, the enzyme method is mild, but the cost is high and the efficiency is low; chemical modification may result in residues; the physical modification requires large-scale equipment, such as ultrahigh pressure equipment, blasting extrusion equipment and the like. Since the great majority of dietary fibers contained in the black bean skin are insoluble dietary fibers, there is a strong need in the art to develop a method for increasing the content of soluble dietary fibers in the black bean skin.
Disclosure of Invention
The invention aims to provide a method for improving the content of soluble dietary fiber in black bean skin.
In a first aspect of the present invention, there is provided a method for increasing the soluble dietary fiber content in black soybean hulls, comprising the steps of:
(i) providing black bean curd skin;
(ii) under an alkaline condition, mixing the black bean skin with an alkaline solution to obtain a first mixed solution containing the black bean skin and the alkaline solution, wherein the mass concentration of the alkaline solution is 8-30%; and
(iii) (iii) drying the first mixed liquor obtained in step (ii) to obtain a modified black soybean hull having an increased content of soluble dietary fibers.
In another preferred example, the black bean skin is ground black bean skin.
In another preferred example, the black bean curd skin is black bean curd skin sieved by a 40-mesh sieve.
In another preferred embodiment, in step (ii), the pH of the alkaline condition is 8 to 13, preferably 9 to 12, more preferably 10 to 12.
In another preferred embodiment, in step (ii), the alkaline solution is selected from the group consisting of: hydrogen peroxide solution, sodium hydroxide solution, or a combination thereof.
In another preferred embodiment, the alkaline solution comprises a hydrogen peroxide solution.
In another preferred example, in the step (ii), the feed-to-liquid ratio of the black bean curd skin to the alkaline solution is 1:10 to 1:20, preferably 1:11 to 1:19, and more preferably 1:12 to 1: 18.
In another preferred embodiment, the concentration of the alkaline solution is 10-20% by mass, preferably 12-18% by mass, more preferably 14-16% by mass, and most preferably 15% by mass.
In another preferred embodiment, the step (ii) further comprises a step of stirring at room temperature.
In another preferred embodiment, the stirring time is 0.1 to 5 hours, preferably 0.3 to 3 hours, more preferably 0.5 to 1 hour.
In another preferred embodiment, the step (iii) further comprises the steps of adjusting the pH of the first mixed solution to neutral (pH6 to 8) and performing suction filtration.
In another preferred embodiment, the pH of the first mixed solution is adjusted to neutral with an acid in the step (iii).
In another preferred embodiment, the acid is selected from the group consisting of: hydrochloric acid, sulfuric acid, acetic acid, or a combination thereof.
In another preferred embodiment, the filter residue obtained after the suction filtration is washed with pure water in an amount of 2 to 20 times (preferably, 5 to 15 times, and more preferably, 10 times) the mass of the black soybean hull.
In another preferred embodiment, the method further comprises step (iv): (iv) detecting the content of the soluble dietary fiber in the modified black bean curd skin with the increased content of the soluble dietary fiber obtained in the step (iii).
It is to be understood that within the scope of the present invention, the above-described features of the present invention and those specifically described below (e.g., in the examples) may be combined with each other to form new or preferred embodiments. Not to be reiterated herein, but to the extent of space.
Drawings
Fig. 1 shows a graph comparing the Soluble Dietary Fiber (SDF) extracted from black soybean hulls modified by the alkaline hydrogen peroxide modification method of the present invention with the SDF extracted from black soybean hulls as they are (i.e., not modified) in terms of quality, wherein a is the SDF extracted from black soybean hulls as they are; and B is SDF extracted from modified black bean skin.
Detailed Description
The inventor of the invention has conducted extensive and intensive studies for a long time and unexpectedly found a method for increasing the content of soluble dietary fibers in black soybean hulls, which comprises mixing the black soybean hulls with an alkaline solution (such as a hydrogen peroxide solution) with a mass concentration of 8-30% at a pH of 8-13, and performing suction filtration and drying to obtain modified black soybean hulls with an average soluble dietary fiber content of 16.15% or even more 17.34%. On this basis, the inventors have completed the present invention.
Soluble Dietary Fiber (SDF)
As used herein, the term "soluble dietary fiber" refers to that portion of dietary fiber which is not digested by digestive enzymes secreted from the human digestive tract, but which is soluble in warm or hot water and which in aqueous solution is reprecipitated by an amount equivalent to four times the amount of ethanol. The soluble dietary fiber can better play the metabolic role in the aspect of physiological function than the insoluble dietary fiber, and has obvious effects in promoting the growth of probiotics in intestinal tracts and preventing related diseases such as coronary heart disease, arteriosclerosis, hyperlipidemia, diabetes, obesity and the like.
Ratio of material to liquid
As used herein, the term "feed-to-liquid ratio" refers to the mass (g) of black soybean hull and H at a certain pH value and a certain concentration2O2Volume of solution (mL). In the invention, the ratio of the material to the liquid is 1:10-1:20, preferably, 1:11-1:19, more preferably, 1:12-1: at 18, the soluble dietary fiber content of the obtained modified black bean skin is higher. In a preferred embodiment, the content of the soluble dietary fiber in the obtained modified black bean curd skin is up to 17.34% when the feed-liquid ratio is 1: 18.
The main advantages of the invention include:
(1) the invention firstly modifies the black soybean hull dietary fiber by an alkaline hydrogen peroxide method.
(2) By the method, the extraction rate of the soluble dietary fiber in the black bean skin is greatly improved from 7.85 percent of the original extraction rate (namely the content of the soluble dietary fiber is directly extracted and measured from the black bean skin without any treatment) to 16.15 percent (even to 17.34 percent).
(3) The method is a chemical modification method which is simple to operate, low in cost, free of large-scale instruments and free of residues, and promotes the soluble dietary fibers in cell walls to dissolve out and simultaneously promotes the glycosidic bond of insoluble macromolecular polymers such as cellulose and insoluble hemicellulose to be broken and converted into the soluble dietary fibers by breaking the cross-linked structure of the black soybean hull cell wall polysaccharide, so that the content of the Soluble Dietary Fibers (SDF) in the black soybean hulls is increased.
(4) The hydrogen peroxide used in the invention is a clean and efficient oxidant, can be decomposed into oxygen and water, and has no residue problem caused by other chemical modifications. In addition, the alkaline hydrogen peroxide has a bleaching effect, and can improve the color state of the black soybean hulls and the soluble dietary fibers of the black soybean hulls, thereby improving the sensory quality of the black soybean hulls and the soluble dietary fibers of the black soybean hulls.
In addition, the operation method is simple, large instruments and equipment are not involved, and the cost is low.
Method for extracting Soluble Dietary Fiber (SDF) from black bean skin
(1) And (3) sample enzymolysis:
firstly, accurately weighing (1.000 +/-0.005) g of sample, and placing the sample in a goblet beaker.
② adding 40mL MES-TRIS buffer solution into the beaker, stirring on a magnetic stirrer until the sample is completely dispersed (preventing the formation of lumps, and enabling the test object to be fully contacted with the enzyme).
Thirdly, carrying out enzymolysis treatment by using thermostable amylase: add 100. mu.L of thermostable amylase solution and stir at low speed. Covering the beaker with an aluminum foil, and reacting in a water bath at 95-100 ℃ for 30min (the initial temperature of the water bath is 95 ℃).
Cooling: all beakers were removed from the water bath and allowed to air to 60 ℃. The aluminum foil lid was opened and the mesh at the edge of the beaker and the gel at the bottom of the beaker were scraped off with a spatula to allow complete enzymatic digestion of the sample. The beaker walls and spatula were rinsed with 10mL of distilled water.
Carrying out enzymolysis treatment by using protease: mu.L of protease solution was added to each beaker. Covered with aluminum foil, and reacted at 60 ℃ for 30min with shaking (the temperature of the water bath should reach 60 ℃ at the beginning) to react sufficiently.
Sixthly, pH determination: after 30min, the aluminum foil lid was opened and 5mL of 0.561mol/L HCl was added to the beaker while stirring. The final pH is adjusted to 4.0-4.7 at 60 ℃ with a solution or 1mol/L HCl solution (pH is detected and adjusted when the solution is 60 ℃ because pH is higher at lower temperatures).
And (c) carrying out enzymolysis treatment by using an amyloglucosidase solution: add 100. mu.L of amyloglucosidase solution while stirring. Covered with aluminum foil and reacted at 60 ℃ for 30min with constant temperature at 60 ℃.
(2) Extraction assay
The buchner funnel was laid 3 layers of filter paper and the filter paper was completely adsorbed on the buchner funnel surface by water wet suction. The enzymatic hydrolysate was filtered and the beaker washed, the residue was washed 2 times with 10mL of 70 ℃ water and then filtered again, the whole filtrate was transferred to a 600mL stemmed beaker, and about 4 times the amount of 95% ethanol that had been preheated to 60 ℃ was added to the filtrate. Precipitation was carried out at room temperature for 1 h. Centrifuging after precipitation, combining precipitates, and freeze-drying. The lyophilized product was SDF.
EXAMPLE 1 alkaline Hydrogen peroxide modification method of the invention
The experimental method comprises the following steps:
1. picking black bean skins, and removing weeds and black beans;
2. grinding the black bean skin, and sieving with a 40-mesh sieve;
3. preparation H2O2Mixing alkaline hydrogen peroxide solution with the mass concentration of 10-20% and the pH value of 9-11 with the black bean skin according to the material-liquid ratio of 1:12-1:18, and reacting for 0.5-1.5h on a magnetic stirrer at room temperature;
4. after the reaction is finished, adjusting the pH value to be neutral (pH6-8) by hydrochloric acid;
5. performing suction filtration, and washing filter residues twice by using pure water with the mass 10 times that of the black bean hull powder;
6. and drying the filter residue in an oven at 55 ℃ for later use.
7. And (3) determining the content of Soluble Dietary Fiber (SDF) in the modified black bean skin by referring to a national standard GB/T5009.88-2008 method.
(II) optimization of modification conditions
Four variables are selected for optimization, i.e. H2O2The concentrations, pH, reaction time, feed-to-liquid ratios, factor levels are shown in Table 1.
TABLE 1 factor level table
By using L9(34) Orthogonal tables orthogonal tests were performed and the results are analyzed in table 2.
TABLE 2H2O2Orthogonal test results and analysis of SDF extraction from processed black bean skin
As can be seen from tables 1 and 2, pH is the most dominant factor, followed by H2O2The concentration and the feed-liquid ratio have the minimum influence, and the following conditions are selected: pH 10, 20% H2O2The average extraction rate of SDF is the highest and reaches 17.34 percent when the reaction time is 0.5h and the material-liquid ratio is 1: 18.
Example 3 comparison with other modification methods
HCl-ethanol modification method
Samples were weighed, 5g each, and soaked in 50mL of HCl-ethanol of different concentrations for 3 days. The solution was made neutral with NaOH solution (10M). Filtration was carried out and the filter residue was washed twice with 50mL of 95% ethanol. And drying the washed filter residue in a 60 ℃ oven for later use. The modified SDF was extracted by the extraction method of example 1, and the SDF extraction yield after treatment with HCl-ethanol solutions of different concentrations is shown in Table 3.
The results show that at very high HCl-ethanol concentrations, the SDF extraction rate was partially increased, but only up to about 10%, and it was found experimentally that at high HCl-ethanol concentrations of 23.04%, the black soybean hulls had been excessively degraded, conditions were too severe to be suitable as a method for modifying the dietary fiber of the black soybean hulls.
TABLE 3 Effect of HCl-ethanol solution treatment at different concentrations on the extraction yield of soluble dietary fiber from Black Soybean Peel
(II) enzymatic modification
Weighing 4g of black bean skin powder, adding 40mL of citric acid-sodium citrate buffer solution with pH of 4.5, adding a certain amount of compound plant hydrolase (Viscozyme L), and carrying out a water bath oscillation reaction at 50 ℃ for 2 h. Heating to 95 deg.C, and inactivating for 5 min. Suction filtration is carried out, and filter residue is washed 2 times by 40mL of 95% ethanol. And transferring the washed filter residue to a 60 ℃ oven for drying for later use.
Weighing 4g of black bean hull powder, adding 40mL of citric acid-sodium citrate buffer solution with pH of 5.0, adding 1.5L of a certain amount of cellulase (Celluclast), and carrying out water bath oscillation reaction at 50 ℃ for 2 h. Heating to 95 deg.C, and inactivating for 5 min. Suction filtration is carried out, and filter residue is washed 2 times by 40mL of 95% ethanol. And transferring the washed filter residue to a 60 ℃ oven for drying for later use.
The SDF was extracted as in example 1.
TABLE 4 Effect of Viscozyme L addition on the extraction yield of soluble dietary fiber from black bean skin
TABLE 5 Effect of Celluclast 1.5L addition on extraction of soluble dietary fiber from Black Soybean Peel
The results are shown in tables 4 and 5. Results show that the two enzymes Viscozyme L and Celluclast 1.5L have no ideal enzymolysis effect on the black soybean hull, the improvement range of the soluble dietary fiber after enzymolysis treatment is not obvious, and the enzyme method has higher cost, so the enzyme method modification is not suitable for large-scale industrial production.
Example 4 Effect of alkaline Hydrogen peroxide modification Process of the invention on Soluble Dietary Fiber (SDF) quality
The Soluble Dietary Fiber (SDF) extracted from the black bean hull modified by the alkaline hydrogen peroxide modification method of the invention has obvious improvement on the color, and is changed from original tan (namely the color of the SDF extracted from the black bean hull as it is) to light white, as shown in figure 1.
The results show that the Soluble Dietary Fiber (SDF) obtained by the alkaline hydrogen peroxide modification method has better quality and is more beneficial to application in the food industry.
All documents referred to herein are incorporated by reference into this application as if each were individually incorporated by reference. Furthermore, it should be understood that various changes and modifications of the present invention can be made by those skilled in the art after reading the above teachings of the present invention, and these equivalents also fall within the scope of the present invention as defined by the appended claims.
Claims (11)
1. A method for increasing the content of soluble dietary fiber in black soybean hulls is characterized by comprising the following steps:
(i) providing black bean curd skin;
(ii) under an alkaline condition, mixing the black bean skin with an alkaline solution to obtain a first mixed solution containing the black bean skin and the alkaline solution, wherein the mass concentration of the alkaline solution is 12-18%; and
(iii) (iii) drying the first mixed liquor obtained in step (ii) to obtain a modified black soybean hull having an increased content of soluble dietary fibers;
and, the step (ii) further comprises a step of stirring at room temperature; the stirring time is 0.5-1 h;
and, the alkaline solution is an alkaline hydrogen peroxide solution;
the pH of the alkaline condition is 10-12;
the material-liquid ratio of the black bean skin to the alkaline solution is 1:10-1: 20.
2. The method according to claim 1, wherein in the step (ii), the feed-to-liquid ratio of the black bean hull to the alkaline solution is 1:11-1: 19.
3. The method of claim 2, wherein in step (ii), the feed-to-liquid ratio of the black bean hull to the alkaline solution is 1:12 to 1: 18.
4. The method of claim 1, wherein the alkaline solution has a mass concentration of 14-16%.
5. The method of claim 1, wherein step (iii) further comprises the steps of adjusting the pH of the first mixed liquor to neutral and suction filtering.
6. The method according to claim 5, wherein the pH of the first mixed solution is adjusted to neutral with an acid in the step (iii).
7. The method of claim 6, wherein the acid is selected from the group consisting of: hydrochloric acid, sulfuric acid, acetic acid, or a combination thereof.
8. The method as claimed in claim 5, wherein the filter residue obtained after the suction filtration is washed with pure water 2-20 times the mass of the black soybean hull.
9. The method as claimed in claim 8, wherein the filter residue obtained after the suction filtration is washed with pure water of 5-15 times of the mass of the black soybean hull.
10. The method as claimed in claim 9, wherein the filter residue obtained after the suction filtration is washed with pure water of which the mass is 10 times that of the black soybean hull.
11. The method of claim 1, further comprising step (iv): (iv) detecting the content of the soluble dietary fiber in the modified black bean curd skin with the increased content of the soluble dietary fiber obtained in the step (iii).
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