RESISTANT DEXTRIN AND MANUFACTURING METHOD FOR IT

Description

Field of the Invention

[0001] The present invention relates to a method for preparing a resistant dextrin, and belongs to the technical field of food additive production.Background of the Invention

[0002] With the improvement of the level of people's life, many people suffer from hyperlipidemia, hypertension and hyperglycemia symptoms, which are commonly known as "Triple H" and have a trend of increasingly attacking younger peoples. WHO (World Health Organization) ever clearly pointed out that a first defense line for preventing and treating cardiovascular diseases is to decrease "Triple H" and control "Triple H". Among people who suffer from "Triple H", except seriously ill people who need to be treated under the cooperation of drugs, the health of most people may be conditioned by means such as dietary therapy such that side effects of drugs can be avoided.

[0003] Dietary fibers are a kind of carbohydrates which cannot be digested by human bodies, including two major types, i.e., non-water-soluble fibers and water-soluble fibers. In the "Twelfth Five-Year Plan" of China, it is advocated to develop application of dietary fibers, so as to restrain potential hazards caused to people. Daily intakes of dietary fibers which are recommended by relevant international organizations are as follows: a standard recommended by American Cancer Society is 30-40g / person / day, a standard recommended by European Scientific Committee on Food is 30g / person / day, and a standard recommended by Chinese Nutrition Society is 25-35g / person / day.

[0004] Resistant dextrin is a kind of low-calorie glucan. As compared with other dietary fiber products, resistant dextrin in low-molecule water-soluble dietary fibers prepared by using natural starch as a raw material has excellent features such as of good acidic and thermal stability, high digestion tolerance, low glycemic index, low insulin index, low calorie and tooth decay prevention.

[0005] Yin Yueling et al. 2012 discloses the research progress and market status of resistant dextrin.

[0006] CN105542019A discloses a resistant dextrin with a molar content of DP1 smaller than or equal to 1%, a molar content of DP2 smaller than or equal to 4.5%, a molar content of DP3 smaller than or equal to 7.0%, an average degree of polymerization of 6-12, a pH value of 3.0-6.0, and a molar content of dietary fibers is larger than or equal to 85%, as well as a preparation method thereof wherein starch serves as the raw material, and a dextrinization reaction is divided into two stages.

[0007] A Fibersol-2 Brochure dated 2005 describes a digestion resistant maltodextrin that is colorless and transparent in solution, highly soluble, stable, low-viscosity, low-hygroscopicity, low in sweetness and has water-binding as well as body- and texture-improving characteristics.

[0008] US2015025037A1 discloses hyper-branched maltodextrins having a dextrose equivalent between 8 and 15, a molecular weight of 1,700-3,000 daltons, a 1,6-glucoside bond content of 30-45%, and a soluble indigestible fiber content between 75% and 100%.

[0009] WO2014 / 145276A1 discloses a carbohydrate composition having lower digestibility and lower sugar compared to traditional nutritive sweeteners, methods of preparing said carbohydrate compositions as well as food products comprising them.

[0010] US5430141 discloses a method for preparing a low-caloric dextrin using a pyrodextrin prepared by heating a starch to which mineral acid is added.

[0011] US5364652 discloses an indigestible dextrin prepared by heat-treating potato starch with addition of hydrochloric acid to obtain a pyrodextrin, hydrolyzing the pyrodextrin with α-amylase and glucoamylase and removing at least one-half of glucose formed from the resulting hydrolysate. The resulting product is decolorized and deionized.

[0012] JP2005263867 discloses a roasted dextrin with a dietary fiber content of equal to or greater than 55% and a whiteness equal to or greater than 60% obtained through heat treatment of starch at 130-170°C in the presence of an acid and subsequent cooling to equal to or less than 120°C within 30 min.

[0013] US2013 / 030167A1 discloses a method for producing a resistant dextrin from starch hydrolysates by mixing starch hydrolysate, dextrose and an acid catalyst and reacting the mixture at 130-180°C under mild vacuum.

[0014] US2009 / 0196975A1 discloses a water-soluble carrier comprising pullulan and maltodextrin having a dextrose equivalent of 4 to 40, and a weight ratio of maltodextrin to pullulan greater than 3.

[0015] GB / T 5009.88-2008 is a Chinese Standard that specifies the determination method of total, soluble and insoluble dietary fiber in foods and the determination method of insoluble dietary fiber in plant foods.

[0016] The Dietary Fiber Measurement Product Guide Megazyme dated October 2016 describes different measurement methods of dietary fiber and their accuracy in measuring the resistant starch content.

[0017] JPH09278802A discloses an aging-resistant starch obtained by heat-treating a starch with fructose or a saccharide mainly comprising fructose in the presence of an acid under dry conditions. Chinese patent literature CN104403009A (Application No. 201410671093.0) discloses a method for preparing resistant dextrin, comprising the following steps: performing pyrolytic reaction under a high-temperature condition by using starch after acidic treatment as a raw material and adopting sea sand as a heat transfer medium to obtain a pyrodextrin crude product, and then performing refining treatment to the pyrodextrin crude product to obtain a resistant dextrin product.

[0018] Chinese patent literature CN103725732A (Application No. 201310743226.6) discloses a method for preparing resistant dextrin by comprehensively utilizing C-type wheat starch, comprising the following steps: using C-type wheat starch paste as a raw material, regulating pH by using hydrochloric acid and then performing acidification in a closed environment; (2) centrifuging the acidified starch paste and then performing drying; (3) performing high-temperature pyrolysis in a roller heating furnace; (4) cooling to room temperature, adding a proper amount of distilled water and preparing emulsion liquid within a certain concentration range; (5) synchronously performing liquefaction and saccharification by adopting a two-enzymes synergy method; (6) adding activated carbon for discoloration and performing suction filtration to obtain sample liquid; and (7) performing alcohol precipitation and centrifugation to the feed liquid, distilling supernatant, recycling alcohol and performing air flow drying to precipitate to obtain resistant dextrin with a content of 85-90%, wherein the product yield is 80-90%.

[0019] The above-mentioned preparation methods still have the disadvantages such as of great product bitterness, deliquescence and poor flowability, cannot be widely applied to food and healthcare products, especially the field of high-grade food and healthcare products.Summary of the Invention

[0020] Aiming at the defects of the prior art, the present invention provides a method for preparing a resistant dextrin. The resistant dextrin prepared by the present invention is not deliquescent, has good taste and flowability and can be widely applied to food and healthcare products, especially the field of high-grade food and healthcare products.Description of terms

[0021] DP refers to Degree of Polymerization, is an index for measuring the magnitude of a polymer molecule and uses a number of repeated units as a datum, i.e., is an average value of number of repeated units contained in a polymer macromolecule chain.

[0022] DP1 refers to a macromolecule with a degree of polymerization which is 1, DP2 refers to a macromolecule with a degree of polymerization which is 2 and DP3 refers to a macromolecule with a degree of polymerization which is 3.

[0023] In order to implement the present invention, the present invention adopts the following technical solution: A method for preparing a resistant dextrin comprises the following steps: (1) adding hydrochloric acid solution into starch according to mass percent of 0.1-0.5% and uniformly stirring the mixture to obtain a reaction material; (2) increasing temperature of the reaction material obtained in step (1) to 80-120°C, performing reaction for 2-4h at normal pressure to obtain an initial reaction material, then adding hydrochloric acid solution according tomass percent of 1-10% relative to the initial reaction material, uniformly stirring the mixture, increasing temperature to 140-200°C and performing gelatinization reaction for 15-30min at normal pressure to obtain a dextrin crude material; (3) adding deionized water into the dextrin crude material obtained in step (2), regulating sugar concentration to 40-45wt%, and preserving heat to perform acidic hydrolysis for 1-2h at 80-100°C to obtain hydrolysate; and (4) performing discoloration, ion exchange, concentration, purification and drying to the hydrolysate obtained in step (3) to obtain the resistant dextrin; wherein the mass concentration of the hydrochloric acid in step (1) and step (2) is 0.08-0.12%; wherein the resistant dextrin is characterized in that molar content of DP1 is smaller than or equal to 1%, molar content of DP2 is smaller than or equal to 4.5%, molar content of DP3 is smaller than or equal to 7.0%, an average degree of polymerization is 6-12, a pH value is 3.0-6.0 and molar content of dietary fibers is greater than or equal to 85%.

[0024] According to the present invention, preferably, the discoloration in step (4) comprises the following step: adding activated carbon according to dry-base mass percent of 0.5-1.5%, preserving heat and stirring for 25-35min, and then performing filtration to obtain feed liquid with light transmittance greater than or equal to 95%.

[0025] According to the present invention, preferably, the ion exchange in step (4) comprises the following step: regulating temperature of feed liquid before entering a column to 35-55°C and pH of feed liquid exiting the column to 4.0-5.0 to obtain ion exchange liquid with electric conductivity smaller than 100µs / cm and light transmittance greater than or equal to 98%; and according to the present invention, preferably, the concentration in step (4) is sextuple-effect concentration to solid substance mass content of 50-60%.

[0026] According to the present invention, preferably, the purification in step (4) comprises chromatographic purification, secondary discoloration, secondary ion exchange and secondary concentration.

[0027] According to the present invention, more preferably, the chromatographic purification comprises regulating pH to 6.0-7.0 and then performing chromatographic purification through a chromatographic separation system, wherein operating conditions for chromatographic separation are as follows: operating pressure: 0.2-0.35MPa, temperature: 50-70°C, water consumption ratio: 1:(1.2-1.5) and feed per hour: 1.2-1.5m 3< .

[0028] According to the present invention, more preferably, the secondary discoloration comprises adding activated carbon according to dry-base mass percent of 0.5-1.5%, preserving heat and stirring for 25-35min and then performing filtration.

[0029] According to the present invention, more preferably, the secondary ion exchange comprises the following step: regulating temperature of feed liquid before entering a column to 35-55°C and pH of feed liquid exiting the column to 4.0-5.0 to obtain secondary ion exchange liquid with electric conductivity smaller than 100µs / cm and light transmittance greater than or equal to 98%; and according to the present invention, more preferably, the secondary concentration is sextuple-effect concentration to solid substance mass content of 50-60%, pH of 4.0-5.0%, electric conductivity smaller than 100µs / cm and light transmittance greater than or equal to 98%.

[0030] According to the present invention, preferably, the drying in step (4) is belt vacuum drying to water mass content smaller than or equal to 6%.

[0031] A method for preparing a resistant dextrin consisting of the following steps: (1) adding hydrochloric acid solution into starch according to mass percent of 0.3% and uniformly stirring the mixture to obtain a reaction material; (2) increasing temperature of the reaction material obtained in step (1) to 100°C, performing reaction for 3h at normal pressure to obtain an initial reaction material, then adding hydrochloric acid solution according to mass percent of 6% relative to the initial reaction material, uniformly stirring the mixture, increasing temperature to 160°C and performing gelatinization reaction for 22min at normal pressure to obtain a dextrin crude material; (3) adding deionized water into the dextrin crude material obtained in step (2), regulating sugar concentration to 43wt%, and preserving heat to perform acidic hydrolysis for 1.5h at 91°C to obtain hydrolysate; and (4) adding activated carbon into the hydrolysate obtained in step (3) according to dry-base mass percent of 1.0%, preserving heat and stirring for 30min, and then performing filtration to obtain feed liquid with light transmittance of 96%; then regulating temperature of feed liquid before entering a column to 45°C and pH of feed liquid exiting the column to 4.5 to obtain ion exchange liquid with electric conductivity smaller than 100µs / cm and light transmittance greater than or equal to 98%; then performing sextuple-effect concentration to solid substance mass content of 55%; and performing chromatographic purification, secondary discoloration, secondary ion exchange, secondary concentration and belt vacuum drying to water mass content of 5% to obtain the resistant dextrin; the chromatographic purification comprises regulating pH to 6.5 and then performing chromatographic purification through a chromatographic separation system, wherein operating conditions for chromatographic separation are as follows: operating pressure: 0.3MPa, temperature: 60°C, water consumption ratio: 1:1.3 and feed per hour: 1.4m 3< ; the secondary discoloration comprises adding activated carbon according to dry-base mass percent of 1%, preserving heat and stirring for 30min and then performing filtration; the secondary ion exchange comprises the following step: regulating temperature of feed liquid before entering a column to 50°C and pH of feed liquid exiting the column to 4.5 to obtain secondary ion exchange liquid with electric conductivity of 85µs / cm and light transmittance of 99%; the secondary concentration is sextuple-effect concentration to solid substance mass content of 60%, pH of 4.5, electric conductivity of 90µs / cm and light transmittance of 99%; and the mass concentration of the hydrochloric acid in step (1) and step (2) is 0.12%; wherein the resistant dextrin is characterized in that molar content of DP1 is 0.5%, molar content of DP2 is 4.1%, molar content of DP3 is 6.0%, average degree of polymerization is 9, pH value is 3.5 and molar content of dietary fibers is 86%.

[0032] The above-mentioned raw materials are commercially available products in the field. Unless otherwise specially stated, process steps can be all performed according to common operations in the field.Beneficial Effects

[0033] 1. The present invention uses starch as the raw material and divides dextrinization reaction into two stages for the first time, the degree of polymerization of the polymerization reaction is reliably guaranteed, the number of caused side reactions is decreased at the same time and the difficulty in subsequent purification treatment is greatly decreased. 2. The present invention adopts enzyme-free catalytic reaction, i.e., no biological enzyme needs to be added in the entire reaction process, natural hydrolysis is realized in the hydrolysis process by using the acidic environment which exists per se, and by adopting enzyme-free catalytic reaction, on one hand, the reaction process is simplified, and on the other hand, the production cost is greatly reduced and the difficulty in subsequent purification treatment is decreased. 3. The present invention overcomes the disadvantages such as of much side reaction in the original process, great product bitterness, deliquescence and poor flowability, the molar content of DP1 of the prepared resistant dextrin is smaller than or equal to 1%, the molar content of DP2 of the prepared resistant dextrin is smaller than or equal to 4.5%, the molar content of DP3 of the prepared resistant dextrin is smaller than or equal to 7.0%, the average degree of polymerization is 6-12, the pH value is 3.0-6.0 and the molar content of dietary fibers is greater than or equal to 85%, such that the product has good taste and flowability and can be widely applied to food and healthcare products, especially the field of high-grade food and healthcare products. Description of the Embodiments

[0034] The technical solution of the present invention will be further described below in combination with the embodiments. However, the protection scope of the present invention is not limited thereto.

[0035] In the embodiments, the starch was purchased from Shandong Fuyang Biotechnology Co., Ltd.; the malic acid was purchased from Nanjing Guohai Bioengineering Co., Ltd; and the citric acid was purchased from TTCA Co., Ltd. Example 1

[0036] A method for preparing a resistant dextrin comprises the following steps: (1) adding malic acid solution into starch according to mass percent of 0.2% and uniformly stirring the mixture to obtain a reaction material; (2) increasing temperature of the reaction material obtained in step (1) to 85°C, performing reaction for 2.5h at normal pressure to obtain an initial reaction material, then adding malic acid solution according to mass percent of 2% relative to the initial reaction material, uniformly stirring the mixture, increasing temperature to 160°C and performing gelatinization reaction for 20min at normal pressure to obtain a dextrin crude material; (3) adding deionized water into the dextrin crude material obtained in step (2), regulating sugar concentration to 41wt%, and preserving heat to perform acidic hydrolysis for 1.2h at 85°C to obtain hydrolysate; and (4) adding activated carbon into the hydrolysate obtained in step (3) according to dry-base mass percent of 0.7%, preserving heat and stirring for 30min, and then performing filtration to obtain feed liquid with light transmittance of 96%; then regulating temperature of feed liquid before entering a column to 41°C and pH of feed liquid exiting the column to 4.2 to obtain ion exchange liquid with electric conductivity of 80µs / cm and light transmittance of 99%; then performing sextuple-effect concentration to solid substance mass content of 52%; and performing chromatographic purification, secondary discoloration, secondary ion exchange, secondary concentration and belt vacuum drying to water mass content of 5% to obtain the resistant dextrin.

[0037] The chromatographic purification comprises regulating pH to 6.5 and then performing chromatographic purification through a chromatographic separation system, wherein operating conditions for chromatographic separation are as follows: operating pressure: 0.2MPa, temperature: 50-70°C, water consumption ratio: 1:1.2 and feed per hour: 1.2m 3< ; the secondary discoloration comprises adding activated carbon according to dry-base mass percent of 0.6%, preserving heat and stirring for 30min and then performing filtration; the secondary ion exchange comprises the following step: regulating temperature of feed liquid before entering a column to 39°C and pH of feed liquid exiting the column to 4.2 to obtain secondary ion exchange liquid with electric conductivity of 90µs / cm and light transmittance of 99%; the secondary concentration is sextuple-effect concentration to solid substance mass content of 55%, pH of 4.5, electric conductivity smaller than 80µs / cm and light transmittance greater than or equal to 99%; and mass concentration of acid in step (1) and step (2) is 0.1%.

[0038] As tested, in the prepared resistant dextrin, the molar content of DP1 is 0.3%, the molar content of DP2 is 4.1%, the molar content of DP3 is 6.0%, the average degree of polymerization is 7, the pH value is 5.0 and the molar content of dietary fibers is 88%.Example 2

[0039] A method for preparing a resistant dextrin comprises the following steps: (1) adding citric acid solution into starch according to mass percent of 0.1% and uniformly stirring the mixture to obtain a reaction material; (2) increasing temperature of the reaction material obtained in step (1) to 80°C, performing reaction for 2h at normal pressure to obtain an initial reaction material, then adding citric acid solution according to mass percent of 2% relative to the initial reaction material, uniformly stirring the mixture, increasing temperature to 150°C and performing gelatinization reaction for 17min at normal pressure to obtain a dextrin crude material; (3) adding deionized water into the dextrin crude material obtained in step (2), regulating sugar concentration to 42wt%, and preserving heat to perform acidic hydrolysis for 1.5h at 85°C to obtain hydrolysate; and (4) adding activated carbon into the hydrolysate obtained in step (3) according to dry-base mass percent of 0.7%, preserving heat and stirring for 30min, and then performing filtration to obtain feed liquid with light transmittance of 96%; then regulating temperature of feed liquid before entering a column to 40°C and pH of feed liquid exiting the column to 4.5 to obtain ion exchange liquid with electric conductivity of 90µs / cm and light transmittance of 98%; then performing sextuple-effect concentration to solid substance mass content of 55%; and performing chromatographic purification, secondary discoloration, secondary ion exchange, secondary concentration and belt vacuum drying to water mass content of 5% to obtain the resistant dextrin.

[0040] The chromatographic purification comprises regulating pH to 6.5 and then performing chromatographic purification through a chromatographic separation system, wherein operating conditions for chromatographic separation are as follows: operating pressure: 0.35MPa, temperature: 70°C, water consumption ratio: 1:1.5 and feed per hour: 1.5m 3< ; the secondary discoloration comprises adding activated carbon according to dry-base mass percent of 0.7%, preserving heat and stirring for 30min and then performing filtration; the secondary ion exchange comprises the following step: regulating temperature of feed liquid before entering a column to 40°C and pH of feed liquid exiting the column to 4.5 to obtain secondary ion exchange liquid with electric conductivity of 80µs / cm and light transmittance of 99%; the secondary concentration is sextuple-effect concentration to solid substance mass content of 58%, pH of 4.5, electric conductivity of 90µs / cm and light transmittance of 99%; and according to the present invention, preferably, mass concentration of acid in step (1) and step (2) is 0.08%.

[0041] As tested, in the prepared resistant dextrin, the molar content of DP1 is 0.2%, the molar content of DP2 is 4.3%, the molar content of DP3 is 6.5%, the average degree of polymerization is 7, the pH value is 4.0 and the molar content of dietary fibers is 90%.Example 3

[0042] A method for preparing a resistant dextrin comprises the following steps: (1) adding hydrochloric acid solution into starch according to mass percent of 0.3% and uniformly stirring the mixture to obtain a reaction material; (2) increasing temperature of the reaction material obtained in step (1) to 100°C, performing reaction for 3h at normal pressure to obtain an initial reaction material, then adding hydrochloric acid solution according to mass percent of 6% relative to the initial reaction material, uniformly stirring the mixture, increasing temperature to 160°C and performing gelatinization reaction for 22min at normal pressure to obtain a dextrin crude material; (3) adding deionized water into the dextrin crude material obtained in step (2), regulating sugar concentration to 43wt%, and preserving heat to perform acidic hydrolysis for 1.5h at 91°C to obtain hydrolysate; and (4) adding activated carbon into the hydrolysate obtained in step (3) according to dry-base mass percent of 1.0%, preserving heat and stirring for 30min, and then performing filtration to obtain feed liquid with light transmittance of 96%; then regulating temperature of feed liquid before entering a column to 45°C and pH of feed liquid exiting the column to 4.5 to obtain ion exchange liquid with electric conductivity smaller than 100µs / cm and light transmittance greater than or equal to 98%; then performing sextuple-effect concentration to solid substance mass content of 55%; and performing chromatographic purification, secondary discoloration, secondary ion exchange, secondary concentration and belt vacuum drying to water mass content of 5% to obtain the resistant dextrin.

[0043] The chromatographic purification comprises regulating pH to 6.5 and then performing chromatographic purification through a chromatographic separation system, wherein operating conditions for chromatographic separation are as follows: operating pressure: 0.3MPa, temperature: 60°C, water consumption ratio: 1:1.3 and feed per hour: 1.4m 3< ; the secondary discoloration comprises adding activated carbon according to dry-base mass percent of 1%, preserving heat and stirring for 30min and then performing filtration; the secondary ion exchange comprises the following step: regulating temperature of feed liquid before entering a column to 50°C and pH of feed liquid exiting the column to 4.5 to obtain secondary ion exchange liquid with electric conductivity of 85µs / cm and light transmittance of 99%; the secondary concentration is sextuple-effect concentration to solid substance mass content of 60%, pH of 4.5, electric conductivity of 90µs / cm and light transmittance of 99%; and mass concentration of acid in step (1) and step (2) is 0.12%.

[0044] As tested, in the prepared resistant dextrin, the molar content of DP1 is 0.5%, the molar content of DP2 is 4.1%, the molar content of DP3 is 6.0%, the average degree of polymerization is 9, the pH value is 3.5 and the molar content of dietary fibers is 86%.Example 4

[0045] A method for preparing a resistant dextrin comprises the following steps: (1) adding mixed solution of citric acid and malic acid at volume ratio of 1:1 into starch according to mass percent of 0.5% and uniformly stirring the mixture to obtain a reaction material; (2) increasing temperature of the reaction material obtained in step (1) to 120°C, performing reaction for 2h at normal pressure to obtain an initial reaction material, then adding mixed solution of citric acid and malic acid at volume ratio of 1:1 according to mass percent of 10% relative to the initial reaction material, uniformly stirring the mixture, increasing temperature to 200°C and performing gelatinization reaction for 30min at normal pressure to obtain a dextrin crude material; (3) adding deionized water into the dextrin crude material obtained in step (2), regulating sugar concentration to 45wt%, and preserving heat to perform acidic hydrolysis for 2h at 100°C to obtain hydrolysate; and (4) adding activated carbon into the hydrolysate obtained in step (3) according to dry-base mass percent of 1.5%, preserving heat and stirring for 35min, and then performing filtration to obtain feed liquid with light transmittance of 95%; then regulating temperature of feed liquid before entering a column to 55°C and pH of feed liquid exiting the column to 5.0 to obtain ion exchange liquid with electric conductivity of 95µs / cm and light transmittance of 98%; then performing sextuple-effect concentration to solid substance mass content of 60%; and performing chromatographic purification, secondary discoloration, secondary ion exchange, secondary concentration and belt vacuum drying to water mass content of 6% to obtain the resistant dextrin.

[0046] The chromatographic purification comprises regulating pH to 7.0 and then performing chromatographic purification through a chromatographic separation system, wherein operating conditions for chromatographic separation are as follows: operating pressure: 0.25MPa, temperature: 65°C, water consumption ratio: 1:1.4 and feed per hour: 1.3m 3< ; the secondary discoloration comprises adding activated carbon according to dry-base mass percent of 1.5%, preserving heat and stirring for 35min and then performing filtration; the secondary ion exchange comprises the following step: regulating temperature of feed liquid before entering a column to 55°C and pH of feed liquid exiting the column to 5.0 to obtain secondary ion exchange liquid with electric conductivity of 95µs / cm and light transmittance of 99%; the secondary concentration is sextuple-effect concentration to solid substance mass content of 56%, pH of 5.0, electric conductivity of 95µs / cm and light transmittance of 99%; and mass concentration of acid in step (1) and step (2) is 0.09%.

[0047] As tested, in the prepared resistant dextrin, the molar content of DP1 is 0.5%, the molar content of DP2 is 4.1%, the molar content of DP3 is 6.0%, the average degree of polymerization is 11, the pH value is 5.0 and the molar content of dietary fibers is 91%.Example 5

[0048] A method for preparing a resistant dextrin comprises the following steps: (1) adding phosphoricacid solution into starch according to mass percent of 0.1% and uniformly stirring the mixture to obtain a reaction material; (2) increasing temperature of the reaction material obtained in step (1) to 80°C, performing reaction for 2h at normal pressure to obtain an initial reaction material, then adding phosphoricacid solution according to mass percent of 1% relative to the initial reaction material, uniformly stirring the mixture, increasing temperature to 140°C and performing gelatinization reaction for 15min at normal pressure to obtain a dextrin crude material; (3) adding deionized water into the dextrin crude material obtained in step (2), regulating sugar concentration to 40wt%, and preserving heat to perform acidic hydrolysis for 1h at 80°C to obtain hydrolysate; and (4) adding activated carbon into the hydrolysate obtained in step (3) according to dry-base mass percent of 0.5%, preserving heat and stirring for 25min, and then performing filtration to obtain feed liquid with light transmittance of 96%; then regulating temperature of feed liquid before entering a column to 35°C and pH of feed liquid exiting the column to 4.0 to obtain ion exchange liquid with electric conductivity of 80µs / cm and light transmittance of 99%; then performing sextuple-effect concentration to solid substance mass content of 50%; and performing chromatographic purification, secondary discoloration, secondary ion exchange, secondary concentration and belt vacuum drying to water mass content of 6% to obtain the resistant dextrin.

[0049] The chromatographic purification comprises regulating pH to 6.0 and then performing chromatographic purification through a chromatographic separation system, wherein operating conditions for chromatographic separation are as follows: operating pressure: 0.25MPa, temperature: 55°C, water consumption ratio: 1:1.25 and feed per hour: 1.25m 3< ; the secondary discoloration comprises adding activated carbon according to dry-base mass percent of 0.5%, preserving heat and stirring for 25min and then performing filtration; the secondary ion exchange comprises the following step: regulating temperature of feed liquid before entering a column to 35°C and pH of feed liquid exiting the column to 4.0 to obtain secondary ion exchange liquid with electric conductivity of 80µs / cm and light transmittance of 99%; the secondary concentration is sextuple-effect concentration to solid substance mass content of 53%, pH of 4.0, electric conductivity of 80µs / cm and light transmittance of 99%; and mass concentration of acid in step (1) and step (2) is 0.11%.

[0050] As tested, in the prepared resistant dextrin, the molar content of DP1 is 1%, the molar content of DP2 is 4.5%, the molar content of DP3 is 7.0%, the average degree of polymerization is 6, the pH value is 3.5 and the content of dietary fibers is 89%.Comparative Example 1

[0051] A traditional process for preparing a resistant dextrin comprises the following steps: adding 0.05-0.5wt% of hydrochloric acid solution into starch, performing uniform mixing, filtration, pre-drying, crushing by using a crusher, screening by using a 20-mesh to 60-mesh sieve, uniformly mixing edible oil with the pre-dried starch, then adding the mixture into a reaction container, increasing temperature to 150-250°C to perform acid-hot reaction for 10-120min, obtaining an indigestible dextrin crude product after reaction and performing refining treatment to the indigestible dextrin crude product to obtain an indigestible dextrin product.

[0052] Mass concentration of the hydrochloric acid is 0.1%.

[0053] Temperature for the pre-drying is 80-110°C and the pre-drying is performed till water content is less than 5wt%.

[0054] The edible oil is edible soybean oil.

[0055] Weight of the added edible oil is 10-20% of weight of the starch.Comparative Example 2

[0056] A method for preparing a resistant dextrin comprises the following steps: (1) adding hydrochloric acid solution into starch according to mass percent of 6.3%, uniformly stirring the mixture, increasing temperature to 160°C, and performing gelatinization reaction for 3h and 22min at normal pressure to obtain a dextrin crude material; and uniformly stirring the dextrin crude material to obtain a reaction material; (2) adding deionized water into the dextrin crude material obtained in step (1), regulating sugar concentration to 43wt%, and preserving heat to perform acidic hydrolysis for 1.5h at 91°C to obtain hydrolysate; and (3) adding activated carbon into the hydrolysate obtained in step (2) according to dry-base mass percent of 1.0%, preserving heat and stirring for 30min, and then performing filtration to obtain feed liquid with light transmittance of 96%; then regulating temperature of feed liquid before entering a column to 45°C and pH of feed liquid exiting the column to 4.5 to obtain ion exchange liquid with electric conductivity smaller than 100µs / cm and light transmittance greater than or equal to 98%; then performing sextuple-effect concentration to solid substance mass content of 55%; and performing chromatographic purification, secondary discoloration, secondary ion exchange, secondary concentration and belt vacuum drying to water mass content of 5% to obtain the resistant dextrin.

[0057] The chromatographic purification comprises regulating pH to 6.5 and then performing chromatographic purification through a chromatographic separation system, wherein operating conditions for chromatographic separation are as follows: operating pressure: 0.25MPa, temperature: 55°C, water consumption ratio: 1:1.25 and feed per hour: 1.25m 3< ; the secondary discoloration comprises adding activated carbon according to dry-base mass percent of 1%, preserving heat and stirring for 30min and then performing filtration; the secondary ion exchange comprises the following step: regulating temperature of feed liquid before entering a column to 50°C and pH of feed liquid exiting the column to 4.5 to obtain secondary ion exchange liquid with electric conductivity of 85µs / cm and light transmittance of 99%; the secondary concentration is sextuple-effect concentration to solid substance mass content of 55%, pH of 4.5, electric conductivity of 90µs / cm and light transmittance of 99%; and mass concentration of acid in step (1) and step (2) is 0.1%.

[0058] As tested, in the prepared resistant dextrin, the molar content of DP1 is 2.5%, the molar content of DP2 is 8.1%, the molar content of DP3 is 12.0%, the average degree of polymerization is 15, the pH value is 3.5 and the molar content of dietary fibers is 62%.Application Example 1 After the products prepared in comparative example 1 and comparative example 2 and the product prepared in Example 3 were tested, product indexes were compared as follow:

[0059] Content of dietary fibers was tested according to the national standard Determination of Dietary Fibers in Food (GB / T 5009.88-2008). Table 1DP1DP2DP3Average degree of polymerizationContent of dietary fibersComparative example13.2%8.5%15.0%2158%Comparative example22.5%8.1%12%1562%Example 30.5%4.1%6.0%986%

[0060] From the above-mentioned comparison, it can be seen that the content of DP1-DP3 in the resistant dextrin prepared in Example 3 is much lower than the content of DP1-DP3 in the comparative examples, the average degree of polymerization is low, it indicates that the reaction is more complete, the separation quantity distribution is more uniform, the content of dietary fibers is higher at the same time and the product performance advantage is obvious.The applicability of the products prepared in comparative example 1 and comparative example 2 and the applicability of the product prepared in Example 3 were compared as follow:

[0061] The resistant dextrin product in Example embodiment 3 and the products prepared in comparative example 1 and comparative example 2 were compared, the product flowability was evaluated by adopting an angle-of-repose index, and the angle of repose refers to an included angle between a sloping side of the most slope stack formed by powder or particles and a horizontal plane, and the flowability is usually represented by using angle of repose, the smaller the angle of repose is, the better the flowability is, and otherwise, the flowability is poorer.

[0062] Hygroscopicity (moisture absorption rate) was calculated by adopting the following formula:

[0063] Test results are shown in Table 2: Table 2Product tasteFlowability (angle of repose)SolubilityHygroscopicity (moisture absorption rate)Example 3No bitterness22°Immediately soluble in water, short dissolution time, no insoluble substance31%Comparative example 1Bitterness66°Not easily soluble, longer dissolution time, no insoluble substance65%Comparative example 2Bitterness62°Not easily soluble, longer dissolution time, no insoluble substance72%

[0064] From the above-mentioned data, it can be seen that, for comparative example 1 and comparative example 2, since DP1, DP2 and DP3 do not respectively satisfy the requirements that the molar content of DP1 is smaller than or equal to 1%, the molar content of DP2 is smaller than or equal to 4.5% and the molar content of DP3 is smaller than or equal to 7.0%, and the average degree of polymerization does not satisfy the requirement of 6-12, the taste, flowability, solubility, hygroscopicity and the like are obviously poorer than that of the product prepared in Example 3.Comparative Example 3

[0065] A resistant dextrin was prepared according to a method recorded in embodiment 1 of Chinese patent literature CN104403009A (Application No.: 201410671093.0). As detected, in the prepared resistant dextrin, the molar content of DP1 is 3.0%, the molar content of DP2 is 7.5%, the molar content of DP3 is14.0%, the average degree of polymerization is 20, the pH value is 4.2 and the molar content of dietary fibers is 84.6%.Application Example 2 After the product prepared in comparative example 3 and the products prepared in Example 1 and Example2 were tested, product indexes were compared as follow:

[0066] Content of dietary fibers was tested according to the national standard Determination of Dietary Fibers in Food (GB / T 5009.88-2008). Table 1DP1DP2DP3Average degree of polymerizationContent of dietary fibersComparative example 33.0%7.5%14.0%2084.6%Example 10.3%4.1%6%788%Example 20.2%4.3%6.5%790%

[0067] From the above-mentioned comparison, it can be seen that the content of DP1-DP3 in the resistant dextrin prepared in Example 1 and Example 2 is much lower than the content of DP1-DP3 in the comparative example 3, the average degree of polymerization is low, which indicates that the reaction is more complete, the separation quantity distribution is more uniform, the content of dietary fibers is higher at the same time and the product performance advantage is obvious.The applicability of the product prepared in comparative example 3 and the applicability of the products prepared in Example1 and Example3 were compared as follow:

[0068] The resistant dextrin products in Example 1 and Example 2 and the product prepared in comparative example 3 were compared, the product flowability was evaluated by adopting an angle-of-repose index, and the angle of repose refers to an included angle between a sloping side of the most slope stack formed by powder or particles and a horizontal plane, and the flowability is usually represented by using angle of repose, the smaller the angle of repose is, the better the flowability is, and otherwise, the flowability is poorer.

[0069] Hygroscopicity (moisture absorption rate) was calculated by adopting the following formula:

[0070] Test results are shown in Table 2: Table 2Product tasteFlowability (angle of repose)SolubilityHygroscopicity (moisture absorption rate)Example 1No bitterness22°Immediately soluble in water, short dissolution time, no insoluble substance31%Example 2No bitterness22°Immediately soluble in water, short dissolution time, no insoluble substance30%Comparative example 3Bitterness60°Not easily soluble, longer dissolution time, no insoluble substance75%

[0071] From the above-mentioned data, it can be seen that, for comparative example 3, since DP1, DP2 and DP3 do not respectively satisfy the requirements that the molar content of DP1 is smaller than or equal to 1%, the molar content of DP2 is smaller than or equal to 4.5% and the molar content of DP3 is smaller than or equal to 7.0%, and the average degree of polymerization does not satisfy the requirement of 6-12, the taste, flowability, solubility, hygroscopicity and the like are obviously poorer than those of the products prepared in Example 1 and Example 2.

Claims

1. A method for preparing a resistant dextrin, characterized in that the method comprises the following steps: (1) adding hydrochloric acid solution into starch according to mass percent of 0.1-0.5% and uniformly stirring the mixture to obtain a reaction material; (2) increasing temperature of the reaction material obtained in step (1) to 80-120°C, performing reaction for 2-4h at normal pressure to obtain an initial reaction material, then adding hydrochloric acid solution according to mass percent of 1-10% relative to the initial reaction material, uniformly stirring the mixture, increasing temperature to 140-200°C and performing gelatinization reaction for 15-30min at normal pressure to obtain a dextrin crude material; (3) adding deionized water into the dextrin crude material obtained in step (2), regulating sugar concentration to 40-45wt%, and preserving heat to perform acidic hydrolysis for 1-2h at 80-100°C to obtain hydrolysate; and (4) performing discoloration, ion exchange, concentration, purification and drying to the hydrolysate obtained in step (3) to obtain the resistant dextrin; wherein the mass concentration of the hydrochloric acid in step (1) and step (2) is 0.08-0.12% wherein the resistant dextrin is characterized in that molar content of DP1 is smaller than or equal to 1%, molar content of DP2 is smaller than or equal to 4.5%, molar content of DP3 is smaller than or equal to 7.0%, an average degree of polymerization is 6-12, a pH value is 3.0-6.0 and molar content of dietary fibers is greater than or equal to 85%.

2. The method according to claim 1, characterized in that the discoloration in step (4) comprises the following step: adding activated carbon according to dry-base mass percent of 0.5-1.5%, preserving heat and stirring for 25-35min, and then performing filtration to obtain feed liquid with light transmittance greater than or equal to 95%.

3. The method according to claim 1, characterized in that the ion exchange in step (4) comprises the following step: regulating temperature of feed liquid before entering a column to 35-55°C and pH of feed liquid exiting the column to 4.0-5.0 to obtain ion exchange liquid with electric conductivity smaller than 100µs / cm and light transmittance greater than or equal to 98%; and preferably, the concentration in step (4) is sextuple-effect concentration to solid substance mass content of 50-60%.

4. The method according to claim 1, characterized in that the purification in step (4) comprises chromatographic purification, secondary discoloration, secondary ion exchange and secondary concentration.

5. The method according to claim 4, characterized in that the chromatographic purification comprises regulating pH to 6.0-7.0 and then performing chromatographic purification through a chromatographic separation system, wherein operating conditions for chromatographic separation are as follows: operating pressure: 0.2-0.35MPa, temperature: 50-70°C, water consumption ratio: 1:(1.2-1.5) and feed per hour:1.2-1.5m3; and preferably, the secondary discoloration comprises adding activated carbon according to dry-base mass percent of 0.5-1.5%, preserving heat and stirring for 25-35min and then performing filtration.

6. The method according to claim 4, characterized in that the secondary ion exchange comprises the following step: regulating temperature of feed liquid before entering a column to 35-55°C and pH of feed liquid exiting the column to 4.0-5.0 to obtain secondary ion exchange liquid with electric conductivity smaller than 100µs / cm and light transmittance greater than or equal to 98%; and preferably, the secondary concentration is sextuple-effect concentration to solid substance mass content of 50-60%, pH of 4.0-5.0, electric conductivity smaller than 100µs / cm and light transmittance greater than or equal to 98%.

7. The method according to claim 1, characterized in that the drying in step (4) is belt vacuum drying to water mass content smaller than or equal to 6%.

8. A method for preparing a resistant dextrin, consisting of the following steps: (1) adding hydrochloric acid solution into starch according to mass percent of 0.3% and uniformly stirring the mixture to obtain a reaction material; (2) increasing temperature of the reaction material obtained in step (1) to 100°C, performing reaction for 3h at normal pressure to obtain an initial reaction material, then adding hydrochloric acid solution according to mass percent of 6% relative to the initial reaction material, uniformly stirring the mixture, increasing temperature to 160°C and performing gelatinization reaction for 22min at normal pressure to obtain a dextrin crude material; (3) adding deionized water into the dextrin crude material obtained in step (2), regulating sugar concentration to 43wt%, and preserving heat to perform acidic hydrolysis for 1.5h at 91°C to obtain hydrolysate; and (4) adding activated carbon into the hydrolysate obtained in step (3) according to dry-base mass percent of 1.0%, preserving heat and stirring for 30min, and then performing filtration to obtain feed liquid with light transmittance of 96%; then regulating temperature of feed liquid before entering a column to 45°C and pH of feed liquid exiting the column to 4.5 to obtain ion exchange liquid with electric conductivity smaller than 100µs / cm and light transmittance greater than or equal to 98%; then performing sextuple-effect concentration to solid substance mass content of 55%; and performing chromatographic purification, secondary discoloration, secondary ion exchange, secondary concentration and belt vacuum drying to water mass content of 5% to obtain the resistant dextrin; the chromatographic purification comprises regulating pH to 6.5 and then performing chromatographic purification through a chromatographic separation system, wherein operating conditions for chromatographic separation are as follows: operating pressure: 0.3MPa, temperature: 60°C, water consumption ratio: 1:1.3 and feed per hour: 1.4m3; the secondary discoloration comprises adding activated carbon according to dry-base mass percent of 1%, preserving heat and stirring for 30min and then performing filtration; the secondary ion exchange comprises the following step: regulating temperature of feed liquid before entering a column to 50°C and pH of feed liquid exiting the column to 4.5 to obtain secondary ion exchange liquid with electric conductivity of 85µs / cm and light transmittance of 99%; the secondary concentration is sextuple-effect concentration to solid substance mass content of 60%, pH of 4.5, electric conductivity of 90µs / cm and light transmittance of 99%; and the mass concentration of the hydrochloric acid in step (1) and step (2) is 0.12%; wherein the resistant dextrin is characterized in that molar content of DP1 is 0.5%, molar content of DP2 is 4.1%, molar content of DP3 is 6.0%, average degree of polymerization is 9, pH value is 3.5 and molar content of dietary fibers is 86%.