CN101756174B - Method for extracting sweet buckwheat dietary fibers - Google Patents
Method for extracting sweet buckwheat dietary fibers Download PDFInfo
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- CN101756174B CN101756174B CN201010013611A CN201010013611A CN101756174B CN 101756174 B CN101756174 B CN 101756174B CN 201010013611 A CN201010013611 A CN 201010013611A CN 201010013611 A CN201010013611 A CN 201010013611A CN 101756174 B CN101756174 B CN 101756174B
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Abstract
The invention discloses a method for extracting sweet buckwheat dietary fibers, which comprises an enzyme method and an alkaline method for extracting the dietary fibers in kernels and shells of the sweet buckwheat and makes the visual color of the obtained dietary fibers more acceptable by people and improves the application value of the dietary fibers by the decoloring and modification treatments. Currently, most processing residues of the buckwheat are generally abandoned or put away cheaply so as to cause the waste of a large amount of buckwheat resource. The invention adopts different methods to extract and carry out decoloring treatment to prepare the sweet buckwheat dietary fibers with higher activity and few hazardous substance residuals, applies the prepared buckwheat dietary fibers to the food industry, and applies the prepared buckwheat dietary fibers into other fields by modification. The invention can solve the technical problems of extraction, decoloring, modification and the like of the sweet buckwheat dietary fibers, can improve the competitive advantage of the economy of the buckwheat production place, realizes the industrialization development and utilization of the sweet buckwheat dietary fibers, and promotes the economy development of the buckwheat production place.
Description
Technical field
The invention belongs to food processing field, be specifically related to a kind of method for extracting sweet buckwheat dietary fibers.
Background technology
Along with expanding economy; Living standards of the people improve day by day; Very big change has taken place in eating habit, and " rich man's disease " (obesity, hypertension, coronary heart disease, diabetes, the colon cancer etc.) that cause because of meals imbalance or overnutrition have become the principal disease of harm China people ' s health.The experimental results shows, dietary fiber intake deficiency is relevant in the rising of " rich man's disease " incidence of disease and the diet.Therefore, big quantity research has been done to the physiological function of dietary fiber by China, has confirmed that at present it can prevent and treat multiple disease, has different physiological roles, is called as " the 7th nutrient ".
The processed and applied of current sweet buckwheat is mainly with its powder process, and the dietary fiber in shell and the benevolence is used as feed or offal treatment, causes the great wasting of resources.Buckwheat shell is not also found other purposes except being used as pillow.
Current definition different researchers to dietary fiber has different opinions; Authority's definition is the edible part of plant; Or similar carbohydrate, they can not be decomposed by the enzyme of human body alimentary canal, but just in oral cavity, stomach and small intestine, are not digested; Can all or part of fermentation in large intestine (in this sense, strict the saying of the net energy of dietary fiber is not equal to zero).It comprises polysaccharide, oligosaccharide, lignin and plant substrates, but do not comprise in the animal food can not portion.
The chemical composition of dietary fiber has determined it to have some unique physicochemical characteristics.Put it briefly, dietary fiber has fermentable, high retentiveness, absorption affinity, and the cation exchange effect, noenergy is filled the physicochemical characteristic of this five aspect.This also will determine its physiological function and purposes using value, and the physiological function of dietary fiber comprises the following aspects: increase faecal volume, prevention constipation; Prevention of arterial sclerosis, high fat of blood and gall stone; Can regulate the absorption of enteron aisle, delay the rapid rising of blood sugar, make level of postprandial blood sugar stable, help the diabetic to control symptom glucide; Can make stool increment, softening, stimulation intestines peristalsis, it can combine the back to discharge with ight soil with carcinogenic substance in the enteron aisle simultaneously, thereby reduces the carcinogenic concentration of large intestine; The effect of prevention of obesity and fat-reducing: it has replaced a part of nutritional labeling in the food, and the intake of food is reduced; Owing to increase and to chew, prolong feed and reduced the intake of food, promote and increased saliva and secretion of digestive juice; Have filling effect and make the people produce satiety; Reduced the absorptivity of small intestine to fat; Can remove nitrite ion and cadmium ion and Cu, the Zn ion of Hg, Pb, Ca ion and high concentration also had scavenging action, harmful substance is together excreted with dietary fiber; The effect that brings high blood pressure down; Change microbiologic population's composition in the intestinal tract; Non-oxidizability and the effect of removing free radical; The incidence of disease and the occurring degree of diseases such as the shortage of dietary fiber and appendicitis, intermittent hernia, kidney stone, vesical calculus, duodenal ulcer and ulcerative colitis have very big relation.
In recent years, worldwide started the research boom of one functional food, dietary fiber has become the focus of research as the important base-material of functional food.If the dietary fiber in the buckwheat is extracted, not only can develop this abundant plant resources, and, have important practical significance for improving the poor and backward looks of outlying mountain area, development of resources has great potential as functional food.
U.S. cereal chemistry association of man (AACC) to the definition of DF is: DF is the edible part of plant; Or similar carbohydrate; They can not be decomposed by the enzyme of human body alimentary canal; But just in oral cavity, stomach and small intestine, do not digested, can all or part of fermentation in large intestine (in this sense, the net energy of dietary fiber is not strict equals zero).It comprises polysaccharide, oligosaccharide, lignin and plant substrates, but do not comprise in the animal food can not portion.Now people recognize that DF a kind ofly has the nutrient of positive role to human body, and lacking DF can produce harmful effect to health.The nutritionist classifies it as " the 7th nutrient ", and WHO expert group was also recommended DF into " crowd's diet nutritional target " in Geneva in 1991.Dietary fiber is a kind of mixture of complicacy, has very big difference with different its compositions in source.The chemical composition of dietary fiber has determined it to have some unique physicochemical characteristics.Put it briefly, dietary fiber has fermentable, high retentiveness, absorption affinity, and the cation exchange effect, noenergy is filled the physicochemical characteristic of this five aspect.The physiological function of dietary fiber mainly comprises following several respects: increase faecal volume, prevention constipation; Prevention of arterial sclerosis, high fat of blood and gall stone; The prevention diabetes; Antitumaous effect; Prevention of obesity disease; Remove the external source harmful substance; The effect that brings high blood pressure down; Change microbiologic population's composition in the intestinal tract; Non-oxidizability and the effect of removing free radical; The incidence of disease and the occurring degree of diseases such as the shortage of dietary fiber and appendicitis, intermittent hernia, kidney stone, vesical calculus, duodenal ulcer and ulcerative colitis have very big relation.Though dietary fiber is closely related with health, be not The more the better yet.If the dietary fiber intake is too much, not only can cause uncomfortablely, also can influence human body to fat, protein, inorganic salts and some trace elements absorbed.The intake deficiency of these nutrients can cause the infringement of organ functions such as anatomy, heart, blood, reduces the human immunological competence.
Lignin is not a polysaccharide material, but has the non-carbon compound of aromatic series of phenylpropyl alcohol alkane skeleton, is difficult in the plant cell wall separate with cellulose because lignin is present in, so in the constituent of dietary fiber, comprised lignin.Humans and animals all can not digest lignin, and it is to influence the major reason that the product fermentation rate descends, and the attenuation degree of DF and its physiological function are closely related, so the content influence of lignin is to the physiological function of DF.Because the dissolubility of the content of hemicellulose and lignin and buckwheat dietary fibers carboxymethyl-modification is closely related, its content is high more, and then dissolubility is poor more.
Sodium carboxymethylcellulose has particular performances, and multiple functions such as union thickening, suspension, emulsification, stable, film forming, expanded, fresh-keeping, acidproof and health care can replace the effect in food of gelatin, agar, sodium alginate, pectin.CMC solution is pseudoplastic fluid, and its apparent viscosity descends with the increase of shear rate, and irrelevant with shear time, when shearing stops, returning to original viscosity immediately.Raise with temperature, viscosity descends, and recover the cooling back, but long-time high temperature possibly cause the CMC degraded and cause viscosity to reduce; Reduce with the pH value, viscosity descends, and this is because under the acid condition, carboxyl is suppressed ionization and causes viscosity to descend.CMC is an anionic polymer, can interact with some positively charged protein (like casein), generates the stable protein dispersion, thus expansion protein solution pH value scope.Sodium carboxymethylcellulose (CMC) is that output is maximum in the cellulose ethers, purposes is the widest, the product of use most convenient, is commonly called as to be " industrial monosodium glutamate ".The key property of CMC be form full-bodied colloidal solution, adhesion, thickening, flow, emulsification dispersion, figuration, water conservation, film forming, acidproof, salt tolerant, outstanding characteristic such as turbid; And physiology is harmless, therefore in fields such as food, medicine, daily use chemicals, oil, papermaking, weaving, building produce, is used widely.In actual industrial production, may be used on being used for the probing of oil, natural gas, engineering such as dig well; CMC as sizing agent, is used for the fine gauze starching of strong things such as cotton, silk hair, chemical fibre, blending; Be used for paper industry CMC and in paper industry, can make paper smooth agent, sizing agent; In ceramic industry, can do suspending agent, color-fixing agent of adhesive, plasticizer, the glaze of blank etc.; CMC can be used as set retarder, water-loss reducer, thickener and binding agent, makes the ceramic outward appearance of producing good, the gentle bubble of no fault; In jam, syrup, dessert, ice cream beverage as thickener, binding agent.Because dietary fiber has the plurality of health care functions effect, but in buckwheat deep processing and utilization process, is not fully utilized, and causes the considerable part wasting of resources.
Summary of the invention
The object of the present invention is to provide a kind of method for extracting sweet buckwheat dietary fibers that has nutritional health function, good appearance color and luster, makes things convenient for preservation to use.
For achieving the above object, the technical scheme that the present invention adopts is:
1) preliminary treatment: get sweet buckwheat shell and benevolence and after 60 ℃～80 ℃ oven dry, pulverize respectively, cross 60～120 mesh sieves;
2) extract: adopt AMS and papain classification enzymolysis or adopt NaOH solution alkaline hydrolysis;
Wherein the condition of dietary fiber is in the Enzymatic Extraction buckwheat shell: in buckwheat shell, add the enzymolyzing alpha-amylase 30min～90min of buckwheat shell quality 0.3%～0.5%, add the papain enzymolysis 45min～90min of buckwheat shell quality 0.2%～0.4% again;
Alkaline process extracts that the dietary fiber condition is in the buckwheat shell: buckwheat shell and mass fraction are that 2%～4% sodium hydroxide solution liquid mixes by 1: 12～16g/ml, at 45 ℃～75 ℃ alkaline hydrolysis 60min～90min;
The condition of dietary fiber is in the Enzymatic Extraction shelled buckwheat: in shelled buckwheat, add the enzymolyzing alpha-amylase 60min～120min of shelled buckwheat quality 0.2%～0.5%, add the papain enzymolysis 45～90min of shelled buckwheat quality 0.3%～0.5% again;
Alkaline process extracts that the dietary fiber condition is in the shelled buckwheat: in shelled buckwheat, adding behind the enzymolyzing alpha-amylase 45min～75min of shelled buckwheat quality 0.2%～0.4% with shelled buckwheat and mass fraction is 2%～4% the sodium hydroxide solution mixed by 1g: 12～16ml again, at 45 ℃～75 ℃ alkaline hydrolysis 60min～90min;
3) separation and purification: with step 2) buckwheat shell and benevolence suction filtration or the centrifugation after the extraction, filter residue gets insoluble diedairy fiber IDF with absolute ethyl alcohol, washing with acetone respectively; Filtrating is to filter behind 95% the precipitation with alcohol with volume fraction; Filter residue washs to such an extent that soluble dietary fiber SDF or filtrating are 3.8 with the NaOH solution adjusting pH value of the HCl solution of 1mol/l and 0.5mol/l respectively with absolute ethyl alcohol and acetone; Centrifugation once more; Discard precipitation; Supernatant is transferred to neutrality with the HCl solution of 1mol/l and the NaOH solution of 0.5mol/l; 4 times of volume fractions of adding concentrate are 95% ethanol alcohol precipitation 1h after concentrating; Suction filtration, filter residue get SDF with absolute ethyl alcohol, washing with acetone respectively;
4) decolouring: adopt H
2O
2IDF is decoloured H
2O
2Mass fraction is 8%～12%, regulates H
2O
2PH be 8～12,50 ℃～70 ℃ of bleaching temperatures, bleaching time is 1.5h～3.5h; Adopt ethanol that SDF is decoloured, the volume fraction of ethanol is 40%～60%, uses ammoniacal liquor to regulate ethanol pH and 6～11 carries out pure ammonia process decolouring;
5) remove lignin: the IDF that gets after 1g decolours adds 13ml distilled water, 0.1ml glacial acetic acid, 0.12ml clorox; Shake up, seal, place 50 ℃～80 ℃ water bath with thermostatic control ultrasonic Treatment 10min～20min; Filter, filter residue the same terms is handled 1～4 time down;
6) modification: using volume fraction is that 30%～50% ethanolic solution preparation mass fraction is alkali-ethanolic solution of 5%～13%, and the IDF that the SDF after the step 4) decolouring and step 5) are removed lignin places alkali-ethanolic solution to react 1.5h～2.5h at 35 ℃～55 ℃ dietary fiber is alkalized;
Using volume fraction is that 25%～45% ethanolic solution preparation mass concentration is 10%～20% chloroacetic acid solution, and the dietary fiber after will alkalizing then places chloroacetic acid solution at 50 ℃～70 ℃ etherificate 1.5h～3.0h;
7) dietary fiber after the etherificate is adopted vacuum freeze drying, pulverize sweet buckwheat dietary fibers.
The centrifugal rotational speed of the centrifugation of said step 3) is: 2500～4000r/min.
The vacuum pressure of said step 7) vacuum freeze drying is 60.0～70.0Pa, and thickness of feed layer is 1cm, below the precooling temperature-45 ℃.
The present invention adopts enzyme process and alkaline process to extract dietary fiber in sweet shelled buckwheat, the shell, and more is prone to greatly improved by people's acceptance, using value through the sense organ color and luster that decolours, the dietary fiber that makes is handled in modification.At present, most of buckwheat process residues casted away usually need not or cheap the processing, this has just caused the waste of a large amount of buckwheat resources.And DF is a kind of just human body is had the nutrient of positive role, lacking DF can produce harmful effect to health, and it is human body " the 7th nutrient ", and dietary fiber intake deficiency has direct relation in rising of " rich man's disease " incidence of disease and the diet.The present invention adopts diverse ways to extract and decolouring Processing of Preparation activity is higher, the residual few sweet buckwheat dietary fibers of harmful substance is applied to food service industry, and makes it be applied to other field through modification.The present invention can solve the problem of extraction, decolouring and the modification of sweet buckwheat dietary fibers, and method dietary fiber yield of the present invention is high; Color obviously shoals, becomes light beige; The substitution value of modified dietary fiber is high.Its recovery rate can reach 0.6353～0.9437, and the color whiteness reaches 7.22～10.44, and the modification substitution value reaches 0.478～0.676.
The specific embodiment
Below with specific embodiment technology of preparing scheme of the present invention is described, but protection scope of the present invention is not limited to following examples:
Embodiment 1:1) preliminary treatment: get sweet buckwheat shell and benevolence and after 60 ℃～80 ℃ oven dry, pulverize respectively, cross 60 mesh sieves;
2) extract: the condition of dietary fiber is in the Enzymatic Extraction buckwheat shell: in buckwheat shell, add the enzymolyzing alpha-amylase 30min of buckwheat shell quality 0.3%, add the papain enzymolysis 45min of buckwheat shell quality 0.2% again;
The condition of dietary fiber is in the Enzymatic Extraction shelled buckwheat: in shelled buckwheat, add the enzymolyzing alpha-amylase 120min of shelled buckwheat quality 0.2%, add the papain enzymolysis 45min of shelled buckwheat quality 0.5% again;
3) separation and purification: with step 2) buckwheat shell and the benevolence suction filtration after the extraction, filter residue gets IDF with absolute ethyl alcohol, washing with acetone respectively; It is to filter behind 95% the precipitation with alcohol that filtrating is used volume fraction, filter residue with absolute ethyl alcohol and acetone wash respectively SDF;
4) decolouring: adopt H
2O
2IDF is decoloured H
2O
2Mass fraction is 10%, regulates H
2O
2PH be 10,50 ℃ of bleaching temperatures, bleaching time are 1.5h～3.5h; Adopt ethanol that SDF is decoloured, the volume fraction of ethanol is 40%, uses ammoniacal liquor to regulate ethanol pH and 6 carries out pure ammonia process decolouring;
5) remove lignin: the IDF that presses after 1g decolours adds 13ml distilled water, 0.1ml glacial acetic acid, 0.12ml clorox, shakes up, and seals, and places 60 ℃ of water bath with thermostatic control ultrasonic Treatment 10min～20min, filters, and filter residue the same terms is handled 1～4 time down;
6) modification: using volume fraction is that 50% ethanolic solution preparation mass fraction is alkali-ethanolic solution of 10%, and the IDF that the SDF after the step 4) decolouring and step 5) are removed lignin places alkali-ethanolic solution to react 1.5h～2.5h at 35 ℃ dietary fiber is alkalized;
Using volume fraction is that 30% ethanolic solution preparation mass concentration is 10% chloroacetic acid solution, and the dietary fiber after will alkalizing then places chloroacetic acid solution at 70 ℃ of etherificate 1.5h～3.0h;
7) be 66.0Pa with the dietary fiber after the etherificate in vacuum pressure, thickness of feed layer is 1cm, carries out vacuum freeze drying below the precooling temperature-45 ℃, powder pure sweet buckwheat dietary fibers.
Embodiment 2:1) preliminary treatment: get sweet buckwheat shell and benevolence and after 60 ℃～80 ℃ oven dry, pulverize respectively, cross 120 mesh sieves;
2) extract: the condition of dietary fiber is in the Enzymatic Extraction buckwheat shell: in buckwheat shell, add the enzymolyzing alpha-amylase 60min of buckwheat shell quality 0.5%, add the papain enzymolysis 70min of buckwheat shell quality 0.3% again;
Alkaline process extracts that the dietary fiber condition is in the shelled buckwheat: in shelled buckwheat, add behind the enzymolyzing alpha-amylase 75min of shelled buckwheat quality 0.2% again with shelled buckwheat and mass fraction be 4% sodium hydroxide solution liquid by 1: the mixed of 16g/ml, at 75 ℃ of alkaline hydrolysis 60min;
3) separation and purification: with step 2) buckwheat shell and the benevolence suction filtration after the extraction, filter residue gets IDF with absolute ethyl alcohol, washing with acetone respectively; It is 3.8 that filtrating is used the HCl solution of 1mol/l and the NaOH solution adjusting pH value of 0.5mol/l; Centrifugation once more; Discard deposition, supernatant is transferred to neutrality with the HCl solution of 1mol/l and the NaOH solution of 0.5mol/l, 4 times of volume fractions of adding concentrate are 95% ethanol alcohol precipitation 1h after concentrating; Suction filtration, filter residue get SDF with absolute ethyl alcohol, washing with acetone respectively;
4) decolouring: adopt H
2O
2IDF is decoloured H
2O
2Mass fraction is 12%, regulates H
2O
2PH be 12,60 ℃ of bleaching temperatures, bleaching time are 1.5h～3.5h; Adopt ethanol that SDF is decoloured, the volume fraction of ethanol is 50%, uses ammoniacal liquor to regulate ethanol pH and 10 carries out pure ammonia process decolouring;
5) remove lignin: the IDF that presses after 1g decolours adds 13ml distilled water, 0.1ml glacial acetic acid, 0.12ml clorox, shakes up, and seals, and places 80 ℃ of water bath with thermostatic control ultrasonic Treatment 10min～20min, filters, and filter residue the same terms is handled 1～4 time down;
6) modification: using volume fraction is that 40% ethanolic solution preparation mass fraction is alkali-ethanolic solution of 13%, and the IDF that the SDF after the step 4) decolouring and step 5) are removed lignin places alkali-ethanolic solution to react 1.5h～2.5h at 55 ℃ dietary fiber is alkalized;
Using volume fraction is that 40% ethanolic solution preparation mass concentration is 15% chloroacetic acid solution, and the dietary fiber after will alkalizing then places chloroacetic acid solution at 50 ℃ of etherificate 1.5h～3.0h;
7) be 60Pa with the dietary fiber after the etherificate in vacuum pressure, thickness of feed layer is 1cm, carries out vacuum freeze drying below the precooling temperature-45 ℃, powder pure sweet buckwheat dietary fibers.
Embodiment 3:1) preliminary treatment: get sweet buckwheat shell and benevolence and after 60 ℃～80 ℃ oven dry, pulverize respectively, cross 100 mesh sieves;
2) extract: the condition of dietary fiber is in the Enzymatic Extraction buckwheat shell: in buckwheat shell, add the enzymolyzing alpha-amylase 90min of buckwheat shell quality 0.4%, add the papain enzymolysis 90min of buckwheat shell quality 0.4% again;
The condition of dietary fiber is in the Enzymatic Extraction shelled buckwheat: in shelled buckwheat, add the enzymolyzing alpha-amylase 90min of shelled buckwheat quality 0.3%, add the papain enzymolysis 70min of shelled buckwheat quality 0.4% again;
3) separation and purification: with step 2) buckwheat shell after the extraction and benevolence are in 2500～4000r/min centrifugation, and filter residue gets IDF with absolute ethyl alcohol, washing with acetone respectively; It is to filter behind 95% the precipitation with alcohol that filtrating is used volume fraction, filter residue with absolute ethyl alcohol and acetone wash respectively SDF;
4) decolouring: adopt H
2O
2IDF is decoloured H
2O
2Mass fraction is 8%, regulates H
2O
2PH be 8,70 ℃ of bleaching temperatures, bleaching time are 1.5h～3.5h; Adopt ethanol that SDF is decoloured, the volume fraction of ethanol is 55%, uses ammoniacal liquor to regulate ethanol pH and 11 carries out pure ammonia process decolouring;
5) remove lignin: the IDF that presses after 1g decolours adds 13ml distilled water, 0.1ml glacial acetic acid, 0.12ml clorox, shakes up, and seals, and places 50 ℃ of water bath with thermostatic control ultrasonic Treatment 10min～20min, filters, and filter residue the same terms is handled 1～4 time down;
6) modification: using volume fraction is that 36% ethanolic solution preparation mass fraction is alkali-ethanolic solution of 8%, and the IDF that the SDF after the step 4) decolouring and step 5) are removed lignin places alkali-ethanolic solution to react 1.5h～2.5h at 45 ℃ dietary fiber is alkalized;
Using volume fraction is that 36% ethanolic solution preparation mass concentration is 20% chloroacetic acid solution, and the dietary fiber after will alkalizing then places chloroacetic acid solution at 60 ℃ of etherificate 1.5h～3.0h;
7) be 70Pa with the dietary fiber after the etherificate in vacuum pressure, thickness of feed layer is 1cm, carries out vacuum freeze drying below the precooling temperature-45 ℃, powder pure sweet buckwheat dietary fibers.
Embodiment 4:1) preliminary treatment: get sweet buckwheat shell and benevolence and after 60 ℃～80 ℃ oven dry, pulverize respectively, cross 80 mesh sieves;
2) extract: alkaline process extracts that the dietary fiber condition is in the buckwheat shell: buckwheat shell and mass fraction be 4% sodium hydroxide solution liquid by 1: 12g/ml mixes, at 75 ℃ of alkaline hydrolysis 60min;
The condition of dietary fiber is in the Enzymatic Extraction shelled buckwheat: in shelled buckwheat, add the enzymolyzing alpha-amylase 60min of shelled buckwheat quality 0.5%, add the papain enzymolysis 90min of shelled buckwheat quality 0.3% again;
3) separation and purification: with step 2) buckwheat shell and the benevolence suction filtration after the extraction, filter residue gets IDF with absolute ethyl alcohol, washing with acetone respectively; It is to filter behind 95% the precipitation with alcohol that filtrating is used volume fraction, filter residue with absolute ethyl alcohol and acetone wash respectively SDF;
4) decolouring: adopt H
2O
2IDF is decoloured H
2O
2Mass fraction is 11%, regulates H
2O
2PH be 11,52 ℃ of bleaching temperatures, bleaching time are 1.5h～3.5h; Adopt ethanol that SDF is decoloured, the volume fraction of ethanol is 45%, uses ammoniacal liquor to regulate ethanol pH and 8 carries out pure ammonia process decolouring;
5) remove lignin: the IDF that presses after 1g decolours adds 13ml distilled water, 0.1ml glacial acetic acid, 0.12ml clorox, shakes up, and seals, and places 70 ℃ of water bath with thermostatic control ultrasonic Treatment 10min～20min, filters, and filter residue the same terms is handled 1～4 time down;
6) modification: using volume fraction is that 45% ethanolic solution preparation mass fraction is alkali-ethanolic solution of 5%, and the IDF that the SDF after the step 4) decolouring and step 5) are removed lignin places alkali-ethanolic solution to react 1.5h～2.5h at 40 ℃ dietary fiber is alkalized;
Using volume fraction is that 25% ethanolic solution preparation mass concentration is 18% chloroacetic acid solution, and the dietary fiber after will alkalizing then places chloroacetic acid solution at 52 ℃ of etherificate 1.5h～3.0h;
7) be 62Pa with the dietary fiber after the etherificate in vacuum pressure, thickness of feed layer is 1cm, carries out vacuum freeze drying below the precooling temperature-45 ℃, powder pure sweet buckwheat dietary fibers.
Embodiment 5:1) preliminary treatment: get sweet buckwheat shell and benevolence and after 60 ℃～80 ℃ oven dry, pulverize respectively, cross 90 mesh sieves;
2) extract: alkaline process extracts that the dietary fiber condition is in the buckwheat shell: buckwheat shell and mass fraction be 3% sodium hydroxide solution liquid by 1: 14g/ml mixes, at 60 ℃ of alkaline hydrolysis 70min;
Alkaline process extracts that the dietary fiber condition is in the shelled buckwheat: in shelled buckwheat, add behind the enzymolyzing alpha-amylase 60min of shelled buckwheat quality 0.3% again with shelled buckwheat and mass fraction be 3% sodium hydroxide solution liquid by 1: the mixed of 14g/ml, at 60 ℃ of alkaline hydrolysis 70min;
3) separation and purification: with step 2) buckwheat shell after the extraction and benevolence are in 2500～4000r/min centrifugation, and filter residue gets IDF with absolute ethyl alcohol, washing with acetone respectively; It is 3.8 that filtrating is used the HCl solution of 1mol/l and the NaOH solution adjusting pH value of 0.5mol/l; Centrifugation once more; Discard deposition, supernatant is transferred to neutrality with the HCl solution of 1mol/l and the NaOH solution of 0.5mol/l, 4 times of volume fractions of adding concentrate are 95% ethanol alcohol precipitation 1h after concentrating; Suction filtration, filter residue get SDF with absolute ethyl alcohol, washing with acetone respectively;
4) decolouring: adopt H
2O
2IDF is decoloured H
2O
2Mass fraction is 9%, regulates H
2O
2PH be 9,65 ℃ of bleaching temperatures, bleaching time are 1.5h～3.5h; Adopt ethanol that SDF is decoloured, the volume fraction of ethanol is 60%, uses ammoniacal liquor to regulate ethanol pH and 7 carries out pure ammonia process decolouring;
5) remove lignin: the IDF that presses after 1g decolours adds 13ml distilled water, 0.1ml glacial acetic acid, 0.12ml clorox, shakes up, and seals, and places 65 ℃ of water bath with thermostatic control ultrasonic Treatment 10min～20min, filters, and filter residue the same terms is handled 1～4 time down;
6) modification: using volume fraction is that 30% ethanolic solution preparation mass fraction is alkali-ethanolic solution of 11%, and the IDF that the SDF after the step 4) decolouring and step 5) are removed lignin places alkali-ethanolic solution to react 1.5h～2.5h at 50 ℃ dietary fiber is alkalized;
Using volume fraction is that 45% ethanolic solution preparation mass concentration is 13% chloroacetic acid solution, and the dietary fiber after will alkalizing then places chloroacetic acid solution at 65 ℃ of etherificate 1.5h～3.0h;
7) be 62Pa with the dietary fiber after the etherificate in vacuum pressure, thickness of feed layer is 1cm, carries out vacuum freeze drying below the precooling temperature-45 ℃, powder pure sweet buckwheat dietary fibers.
Embodiment 6:1) preliminary treatment: get sweet buckwheat shell and benevolence and after 60 ℃～80 ℃ oven dry, pulverize respectively, cross 110 mesh sieves;
2) extract: alkaline process extracts that the dietary fiber condition is in the buckwheat shell: buckwheat shell and mass fraction be 2% sodium hydroxide solution liquid by 1: 16g/ml mixes, at 45 ℃ of alkaline hydrolysis 90min;
Alkaline process extracts that the dietary fiber condition is in the shelled buckwheat: in shelled buckwheat, add behind the enzymolyzing alpha-amylase 45min of shelled buckwheat quality 0.4% again with shelled buckwheat and mass fraction be 2% sodium hydroxide solution liquid by 1: the mixed of 12g/ml, at 45 ℃ of alkaline hydrolysis 90min;
3) separation and purification: with step 2) buckwheat shell and the benevolence suction filtration after the extraction, filter residue gets IDF with absolute ethyl alcohol, washing with acetone respectively; It is to filter behind 95% the precipitation with alcohol that filtrating is used volume fraction, filter residue with absolute ethyl alcohol and acetone wash respectively SDF;
4) decolouring: adopt H
2O
2IDF is decoloured H
2O
2Mass fraction is 10%, regulates H
2O
2PH be 10,58 ℃ of bleaching temperatures, bleaching time are 1.5h～3.5h; Adopt ethanol that SDF is decoloured, the volume fraction of ethanol is 52%, uses ammoniacal liquor to regulate ethanol pH and 9 carries out pure ammonia process decolouring;
5) remove lignin: the IDF that presses after 1g decolours adds 13ml distilled water, 0.1ml glacial acetic acid, 0.12ml clorox, shakes up, and seals, and places 55 ℃ of water bath with thermostatic control ultrasonic Treatment 10min～20min, filters, and filter residue the same terms is handled 1～4 time down;
6) modification: using volume fraction is that 33% ethanolic solution preparation mass fraction is alkali-ethanolic solution of 7%, and the IDF that the SDF after the step 4) decolouring and step 5) are removed lignin places alkali-ethanolic solution to react 1.5h～2.5h at 55 ℃ dietary fiber is alkalized;
Using volume fraction is that 38% ethanolic solution preparation mass concentration is 16% chloroacetic acid solution, and the dietary fiber after will alkalizing then places chloroacetic acid solution at 57 ℃ of etherificate 1.5h～3.0h;
7) be 68Pa with the dietary fiber after the etherificate in vacuum pressure, thickness of feed layer is 1cm, carries out vacuum freeze drying below the precooling temperature-45 ℃, powder pure sweet buckwheat dietary fibers.
Carry out quantitative package after the micro mist essence as required.
In addition, sweet buckwheat dietary fibers of the present invention can be different based on the field of using, and can be used as additive and use with the processing base-material.
Be noted that at last: above embodiment is the unrestricted technology of preparing scheme of the present invention in order to explanation only; Although the present invention is specified with reference to the foregoing description; But as it should be appreciated by those skilled in the art: still can make amendment or be equal to replacement to the present invention; And not breaking away from any modification or the localized variation of the spirit and scope of the present invention, it all should be encompassed in the middle of the claim scope of the present invention.
Claims (3)
1. method for extracting sweet buckwheat dietary fibers is characterized in that may further comprise the steps:
1) preliminary treatment: get sweet buckwheat shell and benevolence and after 60 ℃～80 ℃ oven dry, pulverize respectively, cross 60～120 mesh sieves;
2) extract: adopt AMS and papain classification enzymolysis or adopt NaOH solution alkaline hydrolysis;
Wherein the condition of dietary fiber is in the Enzymatic Extraction buckwheat shell: in buckwheat shell, add the enzymolyzing alpha-amylase 30min～90min of buckwheat shell quality 0.3%～0.5%, add the papain enzymolysis 45min～90min of buckwheat shell quality 0.2%～0.4% again;
Alkaline process extracts that the dietary fiber condition is in the buckwheat shell: buckwheat shell and mass fraction are 2%～4% sodium hydroxide solution by 1g: 12～16ml mixes, at 45 ℃～75 ℃ alkaline hydrolysis 60min～90min;
The condition of dietary fiber is in the Enzymatic Extraction shelled buckwheat: in shelled buckwheat, add the enzymolyzing alpha-amylase 60min～120min of shelled buckwheat quality 0.2%～0.5%, add the papain enzymolysis 45～90min of shelled buckwheat quality 0.3%～0.5% again;
Alkaline process extracts that the dietary fiber condition is in the shelled buckwheat: in shelled buckwheat, adding behind the enzymolyzing alpha-amylase 45min～75min of shelled buckwheat quality 0.2%～0.4% with shelled buckwheat and mass fraction is 2%～4% the sodium hydroxide solution mixed by 1g: 12～16ml again, at 45 ℃～75 ℃ alkaline hydrolysis 60min～90min;
3) separation and purification: with step 2) buckwheat shell and benevolence suction filtration or the centrifugation after the extraction, filter residue gets insoluble diedairy fiber (IDF) with absolute ethyl alcohol, washing with acetone respectively; Filtrating is to filter behind 95% the precipitation with alcohol with volume fraction; Filter residue washs to such an extent that soluble dietary fiber (SDF) or filtrating are 3.8 with the NaOH solution adjusting pH value of the HCl solution of 1mol/l and 0.5mol/l respectively with absolute ethyl alcohol and acetone; Centrifugation once more; Discard precipitation; Supernatant is transferred to neutrality with the HCl solution of 1mol/l and the NaOH solution of 0.5mol/l; 4 times of volume fractions of adding concentrate are 95% ethanol alcohol precipitation 1h after concentrating; Suction filtration, filter residue get SDF with absolute ethyl alcohol, washing with acetone respectively;
4) decolouring: adopt H
2O
2IDF is decoloured H
2O
2Mass fraction is 8%～12%, regulates H
2O
2PH be 8～12,50 ℃～70 ℃ of bleaching temperatures, bleaching time is 1.5h～3.5h; Adopt ethanol that SDF is decoloured, the volume fraction of ethanol is 40%～60%, uses ammoniacal liquor to regulate ethanol pH and 6～11 carries out pure ammonia process decolouring;
5) remove lignin: the IDF that gets after 1g decolours adds 13ml distilled water, 0.1ml glacial acetic acid, 0.12ml clorox; Shake up, seal, place 50 ℃～80 ℃ water bath with thermostatic control ultrasonic Treatment 10min～20min; Filter, filter residue the same terms is handled 1～4 time down;
6) modification: using volume fraction is that 30%～50% ethanolic solution preparation mass fraction is alkali-ethanolic solution of 5%～13%, and the IDF that the SDF after the step 4) decolouring and step 5) are removed lignin places alkali-ethanolic solution to react 1.5h～2.5h at 35 ℃～55 ℃ dietary fiber is alkalized;
Using volume fraction is that 25%～45% ethanolic solution preparation mass concentration is 10%～20% chloroacetic acid solution, and the dietary fiber after will alkalizing then places chloroacetic acid solution at 50 ℃～70 ℃ etherificate 1.5h～3.0h;
7) dietary fiber after the etherificate is adopted vacuum freeze drying, pulverize sweet buckwheat dietary fibers.
2. method for extracting sweet buckwheat dietary fibers according to claim 1 is characterized in that: the centrifugal rotational speed of the centrifugation of said step 3) is: 2500～4000r/min.
3. method for extracting sweet buckwheat dietary fibers according to claim 1 is characterized in that: the vacuum pressure of said step 7) vacuum freeze drying is 60.0～70.0Pa, and thickness of feed layer is 1cm, below the precooling temperature-45 ℃.
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| CN102640905B (en) * | 2012-05-02 | 2013-05-08 | 浙江万里学院 | Method for extracting water-insoluble dietary fiber of osmunda cinnamomea |
| CN103431389B (en) * | 2013-08-27 | 2015-10-28 | 陕西科技大学 | A kind of method extracting buckwheat flavone and dietary fiber from buckwheat shell continuously |
| CN103738910B (en) * | 2013-09-26 | 2015-08-19 | 中国农业科学院作物科学研究所 | A kind of processing method of buckwheat shell purification and decoloration |
| CN105077287A (en) * | 2014-05-06 | 2015-11-25 | 阿拉善盟万铭生物制品有限公司 | Cynomorium songaricum dietary fiber powder, preparation method and applications thereof |
| CN104068357B (en) * | 2014-06-19 | 2016-04-06 | 中国农业大学 | A kind of preparation method of capsicum dietary fiber |
| CN104304573A (en) * | 2014-10-20 | 2015-01-28 | 陈安均 | Instant tartary buckwheat tea and preparation method thereof |
| CN105341952B (en) * | 2015-11-26 | 2017-12-12 | 中国农业大学 | A kind of method of soluble dietary fiber in extrusion assistance enzymolysis extraction rice bran |
| CN105795482A (en) * | 2016-03-29 | 2016-07-27 | 上海交通大学 | Water extraction method of highland barley dietary fibers by optimized by response surface method |
| CN110536610B (en) * | 2017-03-28 | 2023-02-17 | 马克斯·迪茨 | Disintegration/separation and decomposition method of plant shell material and ingredients to obtain and produce plant ingredients and plant-based fiber products |
| CN107397231A (en) * | 2017-08-23 | 2017-11-28 | 佛山市三水区嘉信农业技术研究院（普通合伙） | A kind of extracting method of sunflower seed shell insoluble diedairy fiber |
| CN108926003A (en) * | 2018-06-15 | 2018-12-04 | 河南工业大学 | A kind of preparation method of wheat bran insoluble diedairy fiber fat substitute |
| CN115137079A (en) * | 2022-07-08 | 2022-10-04 | 南开大学 | Buckwheat extract with function of regulating intestinal flora |
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