CN108103125B - Preparation process and application for industrially producing water-soluble dietary fiber - Google Patents
Preparation process and application for industrially producing water-soluble dietary fiber Download PDFInfo
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Abstract
The invention discloses a preparation process and application for industrially producing water-soluble dietary fiber. The process has simple reaction process and low reaction temperature, simultaneously adopts the glucose oxidase technology to directly oxidize the glucose in the enzymolysis process into the gluconic acid, utilizes a small amount of hydrogen peroxide generated by the glucose oxidase technology to carry out oxidation and decoloration on the materials, and the produced resistant dextrin has light color and low polymerization degree and is suitable for industrialized large-scale production.
Description
Technical Field
The invention belongs to the technical field of food production and processing, and relates to a preparation process and application of water-soluble dietary fiber in industrial production.
Background
The Food and Agriculture Organization (FAO) and the World Health Organization (WHO) of the united nations have commonly determined the definition of dietary fiber in 1985: the medium and novel low-viscosity water-soluble dietary fiber product can be measured by a known quantitative method, and the components of edible animals and plants which cannot be hydrolyzed by digestive enzymes inherent in human digestive organs are nutrient which maintains the health of human bodies and cannot be replaced by other substances, and is called as 'seventh nutrient' of human bodies besides six nutrients of secondary carbohydrates, fat, protein, vitamins, water and minerals. The resistant maltodextrin serving as a novel low-viscosity water-soluble dietary fiber is widely applied to the fields of beverages, baked foods, health-care products and the like, can improve the mouthfeel of products, reduce the calorific value of the products, improve the quality of the products, can regulate intestinal flora, inhibit the blood sugar concentration, reduce the serum lipid concentration, lose weight, absorb mineral elements in Zengjiang river and the like, and is a functional food raw material commonly used by modern functional foods and health-care products.
In patent CN201410671093, starch after acid treatment is used as a raw material, sea sand is used as a heat transfer medium, and a pyrolysis reaction is performed at a high temperature to obtain a crude product of pyrodextrin, and the crude product of pyrodextrin is refined to obtain a resistant dextrin product. The method has the advantages of low energy consumption, short time, high heat utilization rate, uniform starch heating, short reaction time, difficult carbonization of starch, simple process and low cost, but the technology has the defects of complex operation, great influence on equipment due to poor treatment and the need of sea sand separation before the saccharification process. In a method for producing indigestible dextrin containing isomerized sugar by Songu chemical industry Co., Ltd CN200580037471.9, digestible components in pyrodextrin containing indigestible components are converted into glucose, and then glucose isomerase is directly acted on the resulting indigestible dextrin containing glucose, thereby converting a part of glucose into fructose with an efficiency equal to or higher than that when the indigestible component is acted on a simple glucose solution, and thus indigestible dextrin containing isomerized sugar can be efficiently produced. CN201610700623 is a method for preparing resistant dextrin by adding acid into starch, vacuum dextrinizing at high temperature, adding water for acidolysis, and performing enzymolysis. The technical defect is that the acidolysis process is adopted, so that the generated resistant dextrin is easily hydrolyzed together with dextrin and starch which are not converted into the resistant dextrin, the yield of the resistant dextrin is low, and the problems of poor reaction uniformity, dark color and difficult decoloration of the industrialized resistant dextrin are not substantially solved. Therefore, it is desirable to provide a method suitable for the industrial production of resistant dextrins.
Disclosure of Invention
Aiming at the defects of the prior art, the inventor provides a method for industrially producing the resistant dextrin through long-term technical and practical exploration, the method is simple in reaction process and low in reaction temperature, glucose in the enzymolysis process is directly oxidized into gluconic acid by adopting a glucose oxidase technology, the material is oxidized and decolored by using a small amount of hydrogen peroxide generated by the glucose oxidase technology, and the produced resistant dextrin is light in color, low in polymerization degree and suitable for industrial large-scale production.
Specifically, the invention relates to the following technical scheme:
in a first aspect of the present invention, there is provided a method for industrially producing a resistant dextrin, the method comprising the steps of:
(1) adding acid into a starch raw material, carrying out high-temperature vacuum dextrinization reaction, adjusting the pH value of a reaction solution I to 5.5-6.5 after the reaction is finished, and adding a liquefying enzyme to carry out high-temperature reaction; after the reaction is finished, adjusting the pH value of the reaction liquid II to 4.2-4.8, adding saccharifying enzyme, glucose oxidase and catalase for saccharification reaction, and after the reaction is finished, performing high-temperature enzyme deactivation treatment to obtain a reaction liquid III, wherein the reaction liquid III contains resistant dextrin sugar liquid and gluconic acid;
(2) neutralizing the reaction liquid III prepared in the step (1) by alkali or alkaline oxide, decoloring by active carbon, and concentrating into 15-30% sugar liquid; the sugar solution contains resistant dextrin and gluconate;
(3) carrying out an ion exchange process on the sugar solution prepared in the step (2), wherein the ion exchange process is carried out in a series connection mode of strong acid cation exchange resin, weak base anion exchange resin and strong base anion exchange resin, the material subjected to the ion exchange process is concentrated and dried to prepare a finished product of resistant dextrin, the weak base anion exchange resin is eluted by ammonia water, and the finished product of gluconic acid is prepared by deaminizing, desalting, concentrating and crystallizing;
preferably, the starch raw material in the step (1) is selected from one or more of corn starch, wheat starch, cassava starch, potato starch or rice starch; further preferably, the starch raw material is corn starch;
preferably, the acid in step (1) is one or more of hydrochloric acid, sulfuric acid, methanesulfonic acid, citric acid, lactic acid and acetic acid, and further preferably, the acid is hydrochloric acid; the adding proportion of the acid is 0.02-5% of the mass of the starch raw material;
preferably, the specific conditions of the high-temperature vacuum dextrinization reaction in the step (1) are as follows: maintaining the vacuum degree at-0.35-0.8 Mpa, and keeping the temperature at 60-90 ℃ for 20-40 min; then heating to 140-180 ℃ and preserving the heat for 40-60 min;
preferably, in the step (1), NaOH aqueous solution with pH of 8.0-9.0 is adopted to adjust the reaction solution I to a solid content of 30-50% and pH of 5.5-6.5; the high-temperature reaction condition of the liquefying enzyme is that the liquefying enzyme reacts for 15-20 min at 105-110 ℃, the liquefying enzyme is high-temperature resistant liquefying enzyme, the enzyme activity is 1-20 ten thousand U/g, and the adding proportion is 0.02-1% of the mass of the reaction liquid I;
preferably, in the step (1), when the high-temperature reaction of the liquefying enzyme is finished and the temperature is reduced to 60 ℃, adding phosphoric acid to adjust the pH of the reaction solution II to 4.2-4.8, then adding saccharifying enzyme, glucose oxidase and catalase to carry out saccharification reaction, wherein the reaction temperature is 60 ℃ and the reaction time is 12-60 hours; the addition proportions of the saccharifying enzyme (the enzyme activity is 3-20 million U/g), the glucose oxidase (the enzyme activity is 1-10 million U/g) and the catalase (the enzyme activity is 10-80 million U/g) are respectively 0.03-0.5%, 0.02-1.5% and 0.02-1.5% of the reaction liquid II, and the mass ratio of the glucose oxidase to the catalase is further preferably 1: 1;
preferably, the temperature for inactivating the enzyme at the high temperature in the step (1) is 80 ℃, and the time is 30-40 min (preferably 30 min);
preferably, the alkali in the step (2) comprises sodium hydroxide, potassium hydroxide, zinc hydroxide and calcium oxide; the basic oxide comprises calcium oxide;
preferably, the ion exchange process in the step (3) is strong acid cation exchange resin-weak base anion exchange resin-strong acid cation exchange resin, and the strong base anion exchange resin is connected in series with the strong acid cation exchange resin, so that the pH of the resistant dextrin can be adjusted;
preferably, in the ion exchange process in the step (3), the flow rate of the sample introduction of the weak basic anion exchange resin is 0.3-1.5ml/min, the temperature is 25-50 ℃, and the pH is 1.0-2.0;
preferably, the strong acid cation exchange resin in the step (3) comprises a strong acid styrene-based cation exchange resin (001 × 7 resin), the weak base anion exchange resin comprises a D301 resin or a D318 resin, and the strong base anion exchange resin comprises a 201 × 7 resin, a D730 resin, a D750 resin, a D770 resin and a 732 resin;
preferably, the concentration and drying method in the step (3) adopts four-effect concentration and spray drying; more preferably, the specific conditions of the spray drying are that the air inlet temperature is 150-350 ℃, the air outlet temperature is 75-180 ℃, and the pressure is-80 to-500 Pa;
preferably, the ammonia water elution flow rate in the step (3) is 0.3-3.0ml/min, the eluted gluconic acid is deaminated and desalted by electrodialysis, and then the gluconic acid finished product is prepared by four-effect concentration and crystallization;
in a second aspect of the invention, the resistant dextrin and the gluconic acid prepared by the method are disclosed;
in a third aspect of the invention, the use of the above process for the preparation of resistant dextrins and gluconic acid is disclosed.
The invention has the beneficial effects that:
(1) according to the invention, the hydrolysis product glucose of the untransformed resistant dextrin in the starch is directly converted into gluconic acid, a small amount of hydrogen peroxide after enzymolysis is used for carrying out oxidation decoloration on the material, and then the material is decomposed by catalase through an integrated technology, so that the co-production of the high-purity resistant dextrin and the gluconic acid is realized;
(2) according to the invention, the glucose is converted into the gluconic acid technology, the separation of the glucose and the resistant dextrin can be realized through an ion exchange process, the high-purity resistant dextrin is prepared, the equipment investment cost is low, and the process technology is simple and feasible;
(3) the purification process of the strong acid cation exchange resin, the weak base anion exchange resin, the strong base anion exchange resin and the strong acid cation exchange resin is adopted, so that the separation and elution of the gluconic acid can be realized, the color of the resistant dextrin can be removed to the maximum extent, and the equipment investment and energy consumption of the conventional chromatographic separation or nanofiltration separation technology are avoided;
(4) the combination of the mixed acid and the drying process is realized by controlling the vacuum degree and the temperature of the acid adding and the feeding, the contact degree of the materials and oxygen is realized by controlling the vacuum degree in the reaction process, and the defects of slow heat radiation and heat transfer and the like caused by excessive vacuum are simultaneously controlled, so that the integration of the steps of acid adding, scorching, milk mixing, liquefying and the like in the whole process of preparing the resistant dextrin by starch in one reaction container is realized; thereby greatly reducing the equipment investment, being beneficial to reducing the production cost and being more suitable for the industrial production of the resistant dextrin and the gluconic acid.
Drawings
FIG. 1 is a process flow chart of the industrial synchronous production of resistant dextrin and gluconic acid.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present application. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
As introduced in the background art, the problems of beany flavor of soybean milk and stability of soybean milk powder are not fully considered in the preparation of soybean milk powder in the prior art;
in view of the above, in an exemplary embodiment of the present invention, there is provided a method for industrially producing resistant dextrin, the method comprising the steps of:
(1) adding acid into a starch raw material, carrying out high-temperature vacuum dextrinization reaction, adjusting the pH value of a reaction solution I to 5.5-6.5 after the reaction is finished, and adding a liquefying enzyme to carry out high-temperature reaction; after the reaction is finished, adjusting the pH value of the reaction liquid II to 4.0-4.8, adding saccharifying enzyme, glucose oxidase and catalase for saccharification reaction, and after the reaction is finished, performing high-temperature enzyme deactivation treatment to obtain a reaction liquid III, wherein the reaction liquid III contains resistant dextrin sugar liquid and gluconic acid;
(2) neutralizing the reaction liquid III prepared in the step (1) by alkali or alkaline oxide, decoloring by active carbon, and concentrating into 15-30% sugar liquid; the sugar solution contains resistant dextrin and gluconate;
(3) carrying out an ion exchange process on the sugar solution prepared in the step (2), wherein the ion exchange process is carried out in a series connection mode of strong acid cation exchange resin, weak base anion exchange resin and strong base anion exchange resin, the material subjected to the ion exchange process is concentrated and dried to prepare a finished product of resistant dextrin, the weak base anion exchange resin is eluted by ammonia water, and the finished product of gluconic acid is prepared by deaminizing, desalting, concentrating and crystallizing;
in still another exemplary embodiment of the present invention, the starch raw material in the step (1) is selected from one or more of corn starch, wheat starch, tapioca starch, potato starch or rice starch; further preferably, the starch raw material is corn starch;
in another exemplary embodiment of the present invention, the acid in step (1) is one or more of hydrochloric acid, sulfuric acid, methanesulfonic acid, citric acid, lactic acid, and acetic acid, and more preferably, the acid is hydrochloric acid; the adding proportion of the acid is 0.02-5% of the mass of the starch raw material;
in another exemplary embodiment of the present invention, the specific conditions of the high-temperature vacuum dextrinization reaction in step (1) are as follows: maintaining the vacuum degree at-0.35-0.8 Mpa, and keeping the temperature at 60-90 ℃ for 20-40 min; then heating to 140-180 ℃ and preserving the heat for 40-60 min;
in another exemplary embodiment of the invention, in the step (1), a NaOH aqueous solution with a pH of 8.0 to 9.0 is used to adjust the reaction solution I to a solid content of 30 to 50% and a pH of 5.5 to 6.5; the high-temperature reaction condition of the liquefying enzyme is that the liquefying enzyme reacts for 15-20 min at 105-110 ℃, and the adding proportion of the liquefying enzyme is 0.02-1% of the mass of the reaction liquid I;
in another exemplary embodiment of the invention, in the step (1), after the high-temperature reaction of the liquefying enzyme is finished and the temperature is reduced to 60 ℃, phosphoric acid is added to adjust the pH of the reaction solution II to 4.2-4.8, and then saccharifying enzyme, glucose oxidase and catalase are added to carry out saccharification reaction, wherein the reaction temperature is 60 ℃ and the reaction time is 12-60 hours; the addition proportions of the saccharifying enzyme, the glucose oxidase and the catalase are respectively 0.03-0.5%, 0.02-1.5% and 0.02-1.5% of the reaction liquid II; wherein, the saccharifying enzyme, the glucose oxidase and the catalase are added together or the saccharifying enzyme is added firstly for carrying out the saccharification reaction for a period of time and then the glucose oxidase and the peroxidase are added;
wherein, the liquefying enzyme is high temperature resistant liquefying enzyme, and the enzyme activity is 1-20 ten thousand U/g; the activity of the saccharifying enzyme is 3-20 million U/g, the activity of the glucose oxidase is 1-10 million U/g, and the activity of the catalase is 10-80 million U/g.
In another exemplary embodiment of the invention, the enzyme deactivation temperature in the step (1) is 80 ℃ and the time is 30-40 min (preferably 30 min);
in still another exemplary embodiment of the present invention, the alkali in the step (2) includes sodium hydroxide, potassium hydroxide, zinc hydroxide and calcium oxide; the basic oxide comprises calcium oxide;
in another exemplary embodiment of the present invention, in the step (3), the ion exchange process is a strong acid cation exchange resin-weak base anion exchange resin-strong acid cation exchange resin, and the strong acid cation exchange resin is connected in series after the strong base anion exchange resin, so as to facilitate the adjustment of the pH of the resistant dextrin;
in another exemplary embodiment of the invention, in the ion exchange step (3), the flow rate of the weak basic anion exchange resin is 0.3-1.5ml/min, the temperature is 25-50 ℃, and the pH is 1.0-2.0;
in still another exemplary embodiment of the present invention, the strong acid cation exchange resin in the step (3) includes a strong acid styrene-based cation exchange resin (001 × 7 resin), the weak base anion exchange resin includes a D301 resin or a D318 resin, and the strong base anion exchange resin includes a 201 × 7 resin, a D730 resin, a D750 resin, a D770 resin, and a 732 resin;
in another exemplary embodiment of the present invention, the concentration and drying in step (3) is performed by four-effect concentration, spray drying; more preferably, the specific conditions of the spray drying are that the air inlet temperature is 150-350 ℃, the air outlet temperature is 75-180 ℃, and the pressure is-80 to-500 Pa;
in another exemplary embodiment of the invention, the ammonia water elution flow rate in the step (3) is 0.3-3.0ml/min, and the eluted gluconic acid is deaminated and desalted by electrodialysis and then is subjected to four-effect concentration and crystallization to obtain a finished gluconic acid product;
in another exemplary embodiment of the present invention, there is provided resistant dextrin and gluconic acid prepared by the above method;
in a further exemplary embodiment of the present invention, there is provided the use of the above method for the preparation of resistant dextrins and gluconic acid.
The invention is further illustrated by the following examples, which are not to be construed as limiting the invention thereto.
Example 1
Controlling the vacuum degree of a 5t reaction kettle to be-0.085-0.1 MPa in advance, adjusting the temperature to 90 ℃, closing a negative pressure maintaining system, starting the maximum stirring speed to feed, feeding corn starch for 1t, adding 1% hydrochloric acid from a liquid adding port, controlling the vacuum degree in the whole process to be-0.05-0.08 MPa, continuously feeding starch for 2t, and 1% hydrochloric acid for 60kg, closing all feed ports when the negative pressure is lower than 0.05MPa, opening a negative pressure system to mix materials, closing a negative pressure valve when the feeding is always kept, and closing a material port when the negative pressure valve is opened. After all the materials are added, maintaining the temperature at-0.05 Mpa80 ℃, stirring for 20-40 min, then heating to 165 ℃ and maintaining for 60min, and maintaining the vacuum degree to-0.05-0.08 MPa in the whole process.
After the reaction is finished, adding NaOH aqueous solution with the pH of 8.0-9.0 through a liquid adding port, pulping until the pH is 6.5, continuously adding water to adjust the solid content to be 50%, adding 1% of liquefying enzyme, reacting at 105-110 ℃ for 15min, entering a saccharification tank, adding water to adjust the solid content to 35%, reducing the temperature to 60 ℃, adjusting the pH to 4.2-4.8 by adopting phosphoric acid, adding 0.3% of saccharifying enzyme, 0.02% of glucose oxidase and 0.02% of catalase, and saccharifying for 36h at 60 ℃. And (3) inactivating enzyme after the saccharification is finished, wherein the enzyme inactivation temperature is 80 ℃, and the time is 30 min. At this time, calcium oxide was added for neutralization, and activated carbon was used for decolorization. And concentrating the mixture of the decolorized resistant dextrin sugar solution and the calcium gluconate into 15-30% sugar solution, and directly entering an ion exchange process.
Wherein the liquefying enzyme is high-temperature resistant liquefying enzyme, and the enzyme activity is 1 ten thousand U/g; the activity of the saccharifying enzyme is 10 ten thousand U/g, the activity of the glucose oxidase is 10 ten thousand U/g and the activity of the catalase is 80 ten thousand U/g.
The ion exchange process is carried out by connecting strong acid cation exchange resin, weak base anion exchange resin, strong base anion exchange resin and strong acid cation exchange resin in series, and the ion-exchanged material is directly concentrated, sprayed and dried to obtain the resistant dextrin. Wherein the strong acid cation exchange resin is 001 × 7, the weak base anion exchange resin is D318, and the strong base anion exchange resin is 201 × 7. The pH value of the fed material of the weak base anion exchange resin is 1.0-2.0, the feeding temperature is 35 ℃, the flow rate is 0.3ml/min, after the feeding is finished, the weak base anion exchange resin is eluted by 2.0mol/L ammonia water so as to elute gluconate, and the elution flow rate is 0.3 ml/min; the discharge from the weak base anion exchange resin directly enters the strong base anion exchange resin to select 201X 7. Then the product is concentrated by four effects and is sprayed and dried to become a finished product of the resistant dextrin. Wherein the air inlet temperature of the spray drying is 160 ℃, the air outlet temperature is 110 ℃, and the pressure is-80 to-500 Pa. And carrying out deamination and desalination on the eluted gluconate by adopting electrodialysis, and then carrying out four-effect concentration and crystallization to obtain a finished product of the gluconate.
The content of resistant dextrin is detected by a second enzyme gravimetric method-liquid chromatography in GB/T22224-2008 'determination of dietary fiber in food gravimetric method and enzyme gravimetric method-liquid chromatography', wherein the content of the resistant dextrin is 83.47%.
Example 2
Controlling the vacuum degree of a 5t reaction kettle to reach-0.1 MPa in advance, adjusting the temperature to 80 ℃, closing a negative pressure maintaining system, starting the maximum stirring rotation speed to feed, feeding corn starch at 0.5t, adding 1% hydrochloric acid from a liquid adding port, controlling the vacuum degree in the whole process to be-0.05-0.08 MPa, continuously feeding starch at 2.5t and hydrochloric acid at 450kg, closing all feed ports when the negative pressure is lower than 0.05MPa, opening the negative pressure system to uniformly mix the materials, closing a negative pressure valve when the feeding is always kept, and closing a material port when the negative pressure valve is opened. After all the materials are added, the temperature is maintained at minus 0.05Mpa and 80 ℃ for stirring for 40min, then the temperature is raised to 155 ℃ and maintained for 50min, and the vacuum degree is maintained to be minus 0.05-0.08 MPa in the whole process.
After the reaction is finished, adding NaOH aqueous solution with the pH of 8.0-9.0 through a liquid adding port, regulating the pH to 5.5, continuously adding water to regulate the solid content to be 30%, adding 0.02% of liquefying enzyme, reacting at 105-110 ℃ for 15min, entering a saccharification tank, adding water to regulate the solid content to 35%, reducing the temperature to 60 ℃, adding 0.5% of saccharifying enzyme under the phosphoric acid condition with the pH of 4.2-4.8, saccharifying at 60 ℃ for 24h, adding 1.5% of glucose oxidase and 1.5% of catalase, and saccharifying at 60 ℃ for 36 h. And (3) inactivating enzyme after the saccharification is finished, wherein the enzyme inactivation temperature is 80 ℃, and the time is 30 min. At this time, calcium oxide was added for neutralization, and activated carbon was used for decolorization. The mixture of the decolorized resistant dextrin sugar liquid and the calcium gluconate is concentrated into 30 percent sugar liquid and directly enters an ion exchange process.
Wherein the liquefying enzyme is high-temperature resistant liquefying enzyme, and the enzyme activity is 20 ten thousand U/g; the activity of the saccharifying enzyme is 8 million U/g, the activity of the glucose oxidase is 4 million U/g, and the activity of the catalase is 40 million U/g.
The ion exchange process resin is carried out in a series connection mode of strong acid cation exchange resin, weak base anion exchange resin, strong base anion exchange resin and strong acid cation exchange resin, wherein the strong acid cation exchange resin is 001 multiplied by 7, the weak base anion exchange resin is D318, the feeding temperature is 50 ℃, the flow rate is 1.0ml/min, and the pH value is 1.0-2.0; the strong base anion exchange resin is selected from D770. Directly feeding the discharge of the weak base anion exchange resin into the strong base anion exchange resin selection D770. Then the resistant dextrin is obtained by four-effect concentration and spray drying, the air inlet temperature of the spray drying is 150 ℃, the air exhaust temperature is 75 ℃, and the pressure is-80 to-500 Pa. Eluting the gluconate by using 1.0mol/L ammonia water through the weak-base anion exchange resin at the elution flow rate of 1.0 ml/min; and carrying out deamination and desalination by adopting electrodialysis, and then obtaining a finished product of gluconic acid by four-effect concentration and crystallization.
The content of resistant dextrin is detected by a second enzyme gravimetric method-liquid chromatography in GB/T22224-2008 'determination of dietary fiber in food gravimetric method and enzyme gravimetric method-liquid chromatography', wherein the content of the resistant dextrin is 89.94%.
Example 3
Controlling the vacuum degree of a 5t reaction kettle to be-0.085-0.1 MPa in advance, adjusting the temperature to 90 ℃, closing a negative pressure maintaining system, starting the maximum stirring speed to feed, feeding corn starch for 1t, adding 2% hydrochloric acid from a liquid adding port, controlling the vacuum degree in the whole process to be-0.05-0.08 MPa, continuously feeding starch for 2t, and 300kg of 1% hydrochloric acid, closing all feed ports when the negative pressure is lower than 0.05MPa, opening the negative pressure system to uniformly mix materials, closing a negative pressure valve when the feeding is always kept, and closing a material port when the negative pressure valve is opened. After all the materials are added, maintaining the temperature at-0.05 Mpa80 ℃, stirring for 20-40 min, then heating to 165 ℃ and maintaining for 60min, and maintaining the vacuum degree to-0.05-0.08 MPa in the whole process.
After the reaction is finished, adding NaOH aqueous solution with the pH of 8.0-9.0 through a liquid adding port, pulping until the pH is 6.5, continuously adding water to adjust the solid content to be 50%, adding 0.2% of liquefying enzyme, reacting at 105-110 ℃ for 15min, feeding into a saccharification tank, adding water to adjust the solid content to 35%, lowering the temperature to 60 ℃, adjusting the pH to 4.2-4.8 by adopting phosphoric acid, adding 0.05% of saccharifying enzyme, 1.5% of glucose oxidase and 1.5% of catalase, and saccharifying at 60 ℃ for 36 h. And (3) inactivating enzyme after the saccharification is finished, wherein the enzyme inactivation temperature is 80 ℃, and the time is 30 min. At this time, calcium oxide was added for neutralization, and activated carbon was used for decolorization. And concentrating the mixture of the decolorized resistant dextrin sugar solution and the calcium gluconate into 15-30% sugar solution, and directly entering an ion exchange process.
Wherein the liquefying enzyme is high-temperature resistant liquefying enzyme, and the enzyme activity is 1-20 ten thousand U/g; the activity of the saccharifying enzyme is 20 ten thousand U/g, the activity of the glucose oxidase is 4 ten thousand U/g and the activity of the catalase is 40 ten thousand U/g.
The ion exchange process is carried out by connecting strong acid cation exchange resin, weak base anion exchange resin, strong base anion exchange resin and strong acid cation exchange resin in series, and the ion-exchanged material is directly concentrated, sprayed and dried to obtain the resistant dextrin. Wherein the strong acid cation exchange resin is 001 × 7, the weak base anion exchange resin is D318, and the strong base anion exchange resin is 201 × 7. The pH value of the fed material of the weak base anion exchange resin is 1.0-2.0, the feeding temperature is 35 ℃, the flow rate is 0.3ml/min, after the feeding is finished, the weak base anion exchange resin is eluted by 0.5mol/L ammonia water so as to elute gluconate, and the elution flow rate is 3.0 ml/min; the discharge from the weak base anion exchange resin directly enters the strong base anion exchange resin to select 201X 7. Then the product is concentrated by four effects and is sprayed and dried to become a finished product of the resistant dextrin. Wherein the air inlet temperature of the spray drying is 160 ℃, the air outlet temperature is 110 ℃, and the pressure is-80 to-500 Pa. And carrying out deamination and desalination on the eluted gluconate by adopting electrodialysis, and then carrying out four-effect concentration and crystallization to obtain a finished product of the gluconate.
The content of resistant dextrin is detected by a second enzyme gravimetric method-liquid chromatography in GB/T22224-2008 'determination of dietary fiber in food gravimetric method and enzyme gravimetric method-liquid chromatography', wherein the content of the resistant dextrin is 90.02%, but the color and luster of the product are obviously higher than those of the products in the examples 1 and 2.
Comparative example 1
Controlling the vacuum degree of a 5t reaction kettle to be-0.085-0.1 MPa in advance, adjusting the temperature to 90 ℃, closing a negative pressure maintaining system, starting the maximum stirring rotating speed to feed, feeding corn starch for 1t, adding 1% hydrochloric acid from a liquid adding port, controlling the vacuum degree of the whole process to be-0.05-0.08 MPa, continuously feeding starch for 2t and 60kg of hydrochloric acid, closing all feed ports when the negative pressure is lower than 0.05MPa, opening the negative pressure system to uniformly mix materials, closing a negative pressure valve when the feeding is always kept, and closing the material port when the negative pressure valve is opened. After all the materials are added, maintaining the temperature at-0.05 Mpa80 ℃, stirring for 20-40 min, then heating to 165 ℃ and maintaining for 60min, and maintaining the vacuum degree to-0.05-0.08 MPa in the whole process.
After the reaction is finished, adding NaOH aqueous solution with the pH value of 8.0-9.0 through a liquid adding port, and mixing to obtain slurry until the pH value is 6.5; at the moment, the solid content is 50 percent, 1 percent of liquefying enzyme is added, the reaction is carried out for 15min at the temperature of 105-. And (3) inactivating enzyme after the saccharification is finished, wherein the enzyme inactivation temperature is 80 ℃, and the time is 30 min. At this time, calcium oxide was added for neutralization, and activated carbon was used for decolorization. The sugar solution with 30 percent of the decolorized resistant dextrin sugar solution directly enters an ion exchange process.
Wherein the liquefying enzyme is high-temperature resistant liquefying enzyme, and the enzyme activity is 1-20 ten thousand U/g; the activity of the saccharifying enzyme is 10 ten thousand U/g. The ion exchange process is carried out by connecting strong acid cation exchange resin, strong base anion exchange resin and strong acid cation exchange resin in series, wherein the strong acid cation exchange resin is 001 × 7, and the strong base anion exchange resin is selected from 201 × 7. Then the concentration of the sugar liquid is concentrated to 50 to 60 percent through four-effect concentration; spray drying to obtain the final product. The air inlet temperature of spray drying is 150 ℃, the air outlet temperature is 75 ℃, and the pressure is-80 to-500 Pa.
The content of resistant dextrin is detected by a second enzyme gravimetric method-liquid chromatography in GB/T22224-2008 'determination of dietary fiber in food gravimetric method and enzyme gravimetric method-liquid chromatography', wherein the content of the resistant dextrin is 55.47%.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (6)
1. A method for industrially producing resistant dextrin, characterized in that the method comprises the following steps:
(1) adding acid into a starch raw material, carrying out high-temperature vacuum dextrinization reaction, adjusting the pH value of a reaction solution I to 5.5-6.5 after the reaction is finished, and adding a liquefying enzyme to carry out high-temperature reaction; after the reaction is finished, adjusting the pH value of the reaction liquid II to 4.2-4.8, adding saccharifying enzyme, glucose oxidase and catalase for saccharification reaction, and after the reaction is finished, performing high-temperature enzyme deactivation treatment to obtain a reaction liquid III, wherein the reaction liquid III contains resistant dextrin and gluconic acid solution;
(2) neutralizing the reaction liquid III prepared in the step (1) by alkali or alkaline oxide, decoloring by active carbon, and concentrating into 15-30% sugar liquid; the sugar solution contains resistant dextrin and gluconate;
(3) carrying out an ion exchange process on the sugar solution prepared in the step (2), wherein the ion exchange process is carried out in a series connection mode of strong acid cation exchange resin-weak base anion exchange resin-strong acid cation exchange resin, the material subjected to the ion exchange process is concentrated and dried to prepare a resistant dextrin finished product, the weak base anion exchange resin is eluted by ammonia water to realize the elution of gluconate, and the glucose finished product is prepared by deaminizing, desalting, concentrating and crystallizing;
the acid in the step (1) is hydrochloric acid; the adding proportion of the acid is 0.02-5% of the mass of the starch raw material;
the starch raw material in the step (1) is selected from one or more of corn starch, wheat starch, cassava starch, potato starch or rice starch;
the specific conditions of the high-temperature vacuum dextrinization reaction in the step (1) are as follows: maintaining the vacuum degree at-0.35-0.8 Mpa, and keeping the temperature at 60-90 ℃ for 20-40 min; then heating to 140-180 ℃ and preserving the heat for 40-60 min;
in the step (1), NaOH aqueous solution with the pH of 8.0-9.0 is adopted to adjust the reaction liquid I until the solid content is 30-50% and the pH is 5.5-6.5; the high-temperature reaction condition of the liquefying enzyme is that the liquefying enzyme reacts for 15-20 min at 105-110 ℃, and the adding proportion of the liquefying enzyme is 0.02-1% of the mass of the reaction liquid I;
after the high-temperature reaction of the liquefying enzyme is finished and the temperature is reduced to 60 ℃ in the step (1), adding phosphoric acid to adjust the pH value of the reaction solution IIto 4.2-4.8, then adding saccharifying enzyme, glucose oxidase and catalase to carry out saccharification reaction, wherein the reaction temperature is 60 ℃ and the reaction time is 12-60 hours; the addition proportions of the saccharifying enzyme, the glucose oxidase and the catalase are respectively 0.03-0.5%, 0.02-1.5% and 0.02-1.5% of the reaction liquid II;
wherein, the liquefying enzyme is high temperature resistant liquefying enzyme, and the enzyme activity is 1-20 ten thousand U/g; the activity of the saccharifying enzyme is 3-20 million U/g, the activity of the glucose oxidase is 1-10 million U/g, and the activity of the catalase is 10-80 million U/g;
the alkali in the step (2) is selected from sodium hydroxide, potassium hydroxide or zinc hydroxide; the alkaline oxide is selected from calcium oxide;
ammonia water is eluted at the flow rate of 0.3-3.0ml/min in the step (3), the eluted gluconic acid is deaminated and desalted by adopting electrodialysis, and then the gluconic acid finished product is prepared by four-effect concentration and crystallization;
the strong acid cation exchange resin in the step (3) is selected from a strong acid styrene cation exchange resin 001X 7 resin, the weak base anion exchange resin is selected from a D301 resin or a D318 resin, and the strong base anion exchange resin is selected from a 201X 7 resin, a D730 resin, a D750 resin or a D770 resin.
2. The method of claim 1, wherein said starch feedstock in step (1) is corn starch.
3. The method according to claim 1, wherein the enzyme deactivation at the high temperature in the step (1) is carried out at 80 ℃ for 30-40 min.
4. The method of claim 3, wherein the enzyme deactivation time at the high temperature in step (1) is 30 min.
5. The method according to claim 1, wherein the weak base anion exchange resin is fed in the ion exchange process of the step (3) at a flow rate of 0.3 to 1.5ml/min, a temperature of 25 to 50 ℃ and a pH of 1.0 to 2.0.
6. The method as claimed in claim 1, wherein the concentration and drying in step (3) are carried out by four-effect concentration, spray drying; the specific conditions of the spray drying are that the air inlet temperature is 150-350 ℃, the air exhaust temperature is 75-180 ℃, and the pressure is-80-500 Pa.
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