# US 10,479,840 B2 · Resistant dextrin and method for preparing the same

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- Number: US 10,479,840 B2
- Document ID: US10479840B2
- Status: Granted
- Kind: B2
- Application number: 15/566,234
- Filed: 2017-01-17
- Published: 2018-04-05
- Granted: 2019-11-19
- Earliest claimed: 2016-01-27
- Assignees: Shandong Bailong Chuangyuan Bio-Tech Co., Ltd
- Applicants: Shandong Bailong Chuangyuan Bio-Tech Co., Ltd
- Inventors: Guangpeng Dou; Zhaobo Gan; Fanghua Li; Xianbao Shao; Tengteng Yang; Qian Du; Mingzhan Zhang; Xingjing Zhang
- Web page: https://patentgrep.com/patent/US10479840B2

## CPC

- C08B 30/18: Dextrin {, e.g. yellow canari, white dextrin, amylodextrin or maltodextrin; Methods of depolymerisation, e.g. by irradiation or mechanically}
- A23L 29/30: containing carbohydrate syrups; containing sugars; containing sugar alcohols, e.g. xylitol; containing starch hydrolysates, e.g. dextrin (products from apiculture A23L21/20; artificial sweetening agents A23L27/30)
- A23L 33/26: Polyol polyesters, e.g. sucrose polyesters; Synthetic sugar polymers, e.g. polydextrose
- B01D 15/1871: {placed in series}
- B01D 15/361: {Ion-exchange}
- C08B 31/006: {Crosslinking of derivatives of starch}
- A23V 2002/00: Food compositions, function of food ingredients or processes for food or foodstuffs
- C08B: POLYSACCHARIDES; DERIVATIVES THEREOF (polysaccharides containing less than six saccharide radicals attached to each other by glycosidic linkages C07H; fermentation or enzyme-using processes C12P19/00; sugar industry C13; production of cellulose D21)
- A23L: FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF (preservation thereof A23B)
- B01D: SEPARATION (separating solids from solids by wet methods B03B, B03D; by pneumatic jigs or tables B03B; by other dry methods B07; magnetic or electrostatic separation of solid materials from solid materials or fluids, separation by high-voltage electric fields B03C; centrifuges, vortex apparatus B04; presses per se for squeezing-out liquid from liquid-containing material B30B9/02; treatment of water C02F, e.g. softening by ion-exchange C02F1/42; {arrangements of air intake cleaners in gas turbine plants F02C7/05} ; arrangements or mounting of filters in air-conditioning, air-humidification or ventilation F24F13/28)
- A23V: INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION

## Abstract

A resistant dextrin and a method for preparing the same. In the resistant dextrin, 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%. The present invention further relates to a method for preparing the resistant dextrin. Since 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.

## Claims

### Claim 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 0.3% 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 2-4 h 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 140-200° C. and performing gelatinization reaction for 15-30 min 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 40-45 wt %, and preserving heat to perform acidic hydrolysis to 1-2 h at 80-100° C. to obtain hydrolysate; and
(4) performing discoloration, on exchange, concentration, purification and drying to the hydrolysate obtained in step (3) to obtain the resistant dextrin;
wherein the hydrochloric acid solution in step (1) and step (2) have a mass concentration of 0.12%;
the ion exchange is performed by using an ion exchange column to obtain ion exchange liquid with electric conductivity smaller than 100 μ/cm and light transmittance greater than or equal to 98%; and wherein the resistant dextrin has
a molar content of DP1 being smaller than or equal to 1%;
a molar content of DP2 being smaller than or equal to 4.5%;
a molar content of DP3 being 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 being greater than or equal to 85%.

### Claim 2 (depends on 1)

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 25-35 min, and then performing filtration to obtain a feed liquid with light transmittance greater than or equal to 95%.

### Claim 3 (depends on 1)

The method according to claim 1, characterized in that the ion exchange in step (4) comprises the following step:
regulating temperature of the feed liquid before entering an ion exchange column to 35-55° C. and pH of the feed liquid exiting the ion exchange column to 4.0-5.0 to obtain ion exchange liquid with electric conductivity smaller than 100 μs/cm and light transmittance greater than or equal to 98%.

### Claim 4 (depends on 1)

The method according to claim 1, characterized in that the concentration in step (4) is sextuple-effect concentration to solid substance mass content of 50-60%.

### Claim 5 (depends on 1)

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.

### Claim 6 (depends on 5)

The method according to claim 5, 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: operation pressure: 0.2-0.35 MPa, temperature: 50-70° C., water consumption ratio: 1:(1.2-1.5) and feed per hour: 1.2-1.5 m3.

### Claim 7 (depends on 1)

The method according to claim 1, characterized in that the secondary discoloration comprises adding activated carbon according to dry-base mass percent of 0.5-1.5%, preserving heat and stirring for 25-35 min and then performing filtration.

### Claim 8 (depends on 5)

The method according to claim 5, characterized in that the secondary ion exchange comprises the following step:
regulating temperature of the feed liquid before entering a column to 35-55° C. and pH of the feed liquid exiting the column to 4.0-5.0 to obtain secondary ion exchange liquid with electric conductivity smaller than 100 μs/cm and light transmittance greater than or equal to 98%.

### Claim 9 (depends on 5)

The method according to claim 5, characterized in that 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 100 μs/cm and light transmittance greater than or equal to 98%.

### Claim 10 (depends on 1)

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%.

### Claim 11 (depends on 1)

The method according to claim 1, wherein steps (1)-(4) are characterized in that:
(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 3 h 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 22 min 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 43 wt %, and preserving heat to perform acidic hydrolysis for 1.5 h at 91° 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.

### Claim 12

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 3 h 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 22 min 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 43 wt %, and preserving heat to perform acidic hydrolysis for 1.5 h 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 30 min, 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 100 μs/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;
wherein the hydrochloric acid solution in step (1) and step (2) have a mass concentration of 0.12%.