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CN-121991255-A - High-purity low-density resistant dextrin and preparation method thereof

CN121991255ACN 121991255 ACN121991255 ACN 121991255ACN-121991255-A

Abstract

The invention belongs to the technical field of functional foods, and in particular relates to high-purity low-density resistant dextrin and a preparation method thereof, wherein the preparation method comprises the steps of mixing corn starch with water, regulating the pH value, performing high-temperature reaction to obtain a dextrinization product, and performing enzymolysis to obtain an enzymolysis solution; and adding trimethoxybenzoyl resistant dextrin derivative and resistant dextrin-1- (2-oxo-pyrrolidine) carbamate modified compound in a specific proportion into the enzymolysis liquid in turn for reaction, concentrating the mixture obtained by the reaction, precipitating with ethanol, decoloring, purifying and drying. According to the method, specific functional groups are introduced into the resistant dextrin molecular chain through covalent modification, so that the digestion resistance, prebiotic activity and drug loading capacity of the product are obviously improved, and the obtained product is high in purity and low in density, and is suitable for the fields of foods and medicines.

Inventors

  • DING YI

Assignees

  • 曲阜贝斯迪生物医药有限公司

Dates

Publication Date
20260508
Application Date
20260209

Claims (10)

  1. 1. The preparation method of the high-purity low-density resistant dextrin is characterized by comprising the following steps of: S1, mixing 80-120 parts of corn starch and 400-600 parts of deionized water in parts by weight, stirring to obtain starch milk, regulating the pH of the starch milk to 2.4-2.6, placing the starch milk in a high-pressure reaction kettle, reacting at 135-145 ℃ to obtain a reaction mixture, cooling the reaction mixture to 60-70 ℃, adding 1-2 parts of medium-temperature alpha-amylase, carrying out enzymolysis at 60-70 ℃, then heating to 115-125 ℃ to inactivate enzyme to obtain an enzymolysis solution, transferring the enzymolysis solution to the reaction kettle, sequentially adding 3-8 parts of 3,4, 5-trimethoxybenzoyl resistant dextrin derivative and 2-6 parts of resistant dextrin-1- (2-oxo-pyrrolidine) carbamate at 84-86 ℃ and reacting under stirring to obtain a mixture; S2, concentrating the mixture, adding ethanol for precipitation, standing, centrifugally collecting precipitate, dispersing the precipitate in water, decolorizing with active carbon at 68-72 ℃, filtering to obtain filtrate, purifying the filtrate to obtain purified liquid, and drying the purified liquid.
  2. 2. The method for preparing high-purity low-density resistant dextrin according to claim 1, characterized in that in step S1, the enzymolysis time is 30-40min at 60-70 ℃.
  3. 3. The method for preparing high purity low density resistant dextrin according to claim 1, characterized in that in step S2, the time for decolorizing with activated carbon at 68-72 ℃ is 30-40min.
  4. 4. The method for preparing high purity low density resistant dextrin according to claim 1, characterized in that the method for preparing 3,4, 5-trimethoxybenzoyl resistant dextrin derivative comprises: Adding 40-60 parts of 3,4, 5-trimethoxybenzoic acid and 180-220 parts of anhydrous methylene dichloride into a three-neck flask under the protection of dry nitrogen, cooling to 0-5 ℃, dropwise adding 24-26 parts of thionyl chloride under stirring, heating to 38-42 ℃ for reflux reaction after the dropwise addition is finished, and distilling under reduced pressure at 38-42 ℃ after the reaction is finished to obtain 3,4, 5-trimethoxybenzoyl chloride; Dissolving 8-12 parts of 3,4, 5-trimethoxybenzoyl chloride in 100-150 parts of anhydrous dichloromethane to obtain an organic phase solution of acyl chloride, dissolving 4-6 parts of resistant dextrin in 200-300 parts of aqueous solution containing 2-5 parts of sodium hydroxide, cooling to 0-5 ℃, adding 0.5-2 parts of tetrabutylammonium bromide to obtain an aqueous phase solution of resistant dextrin, dropwise adding the organic phase solution of acyl chloride into the aqueous phase solution of resistant dextrin under stirring to react at 0-10 ℃, standing for separating after the reaction is finished, regulating the pH of the aqueous phase to be neutral, adding ethanol for precipitation, filtering to obtain a solid product, washing the solid product with deionized water and ethanol in sequence, and vacuum drying at 48-52 ℃.
  5. 5. The process for producing a high purity low density resistant dextrin according to claim 4, wherein in step A1, the reflux reaction is carried out for 3 to 5 hours at a temperature of 38 to 42 ℃.
  6. 6. The process for preparing high purity, low density resistant dextrins according to claim 4, characterized in that in step A2 the reaction time is 2-4 hours at 0-10 ℃.
  7. 7. The method for preparing high purity low density resistant dextrin according to claim 1, characterized in that the method for preparing resistant dextrin-1- (2-oxopyrrolidine) carbamate comprises: Adding 18-22 parts by weight of 2-pyrrolidone into 140-160 parts by weight of anhydrous toluene, stirring and cooling with ice water bath, introducing dry hydrogen chloride gas to obtain 2-pyrrolidone hydrochloride suspension, dropwise adding 16-20 parts by weight of triphosgene into 48-52 parts by weight of anhydrous toluene solution under stirring at 0-5 ℃, heating to 60-80 ℃ for reaction, and cooling to room temperature to obtain an organic phase solution containing isocyanate intermediates; And B2, dispersing 6-10 parts of resistant dextrin in a mixed solvent consisting of 100-150 parts of anhydrous dimethyl sulfoxide containing 0.5-2 parts of triethylamine and 100-150 parts of anhydrous N, N-dimethylformamide, stirring at 50-60 ℃ to obtain a dispersion liquid, dropwise adding an organic phase solution containing an isocyanate intermediate into the dispersion liquid under the condition of 0-10 ℃ and continuous stirring, continuing to react at 25-40 ℃ after the dropwise adding to obtain a reaction mixture, pouring the reaction mixture into diethyl ether for precipitation, centrifugally collecting the precipitate, washing the precipitate with the anhydrous diethyl ether to obtain a crude product, redissolving the crude product in deionized water, filling into a dialysis bag for dialysis to obtain a dialysate, and freeze-drying the dialysate.
  8. 8. The method for producing high purity low density resistant dextrin according to claim 7, characterized in that in step B1, the reaction time for heating to 60-80 ℃ is 2-4 hours.
  9. 9. The process for preparing high purity low density resistant dextrin according to claim 7, characterized in that in step B2, stirring is performed for a period of 2-4 hours at 50-60 ℃.
  10. 10. High purity low density resistant dextrin, characterized in that the high purity low density resistant dextrin is prepared according to the method for preparing high purity low density resistant dextrin according to any of claims 1-9.

Description

High-purity low-density resistant dextrin and preparation method thereof Technical Field The invention belongs to the technical field of functional foods, and particularly relates to high-purity low-density resistant dextrin and a preparation method thereof. Background The resistant dextrin is used as a water-soluble dietary fiber and plays an increasingly important role in the fields of functional foods and medical auxiliary materials. The starch is prepared by acid thermal processing, partial hydrolysis and repolymerization, and the glycosidic bond structure in the molecule can resist the decomposition of digestive enzymes of human small intestine, so that the starch completely enters the large intestine and is selectively fermented and utilized by intestinal microbiota. This property imparts a number of recognized physiological benefits thereto, including, but not limited to, regulating postprandial glycemic response, improving lipid metabolism, promoting proliferation of intestinal beneficial flora, enhancing mineral absorption, and the like. Therefore, resistant dextrins are widely used in low glycemic index foods, prebiotic products, weight management formulas, and health foods that require improved bowel movement, as key functional ingredients connecting daily diet and health management. Although the resistant dextrin has a plurality of advantages, the existing products and technologies still face a plurality of remarkable limitations, and the full play of the efficacy and the expansion of the application range are restricted. Firstly, from the purity point of view, the resistant dextrin produced by the conventional process often contains a certain proportion of digestible sugar, the existence of the impurities weakens the stability of the blood sugar and the core value of the pure dietary fiber, and the preparation of the high-purity product usually depends on complicated chromatographic separation and other technologies, so that the production cost is high, and the large-scale industrial production is difficult to realize. Secondly, the functionality of traditional resistant dextrins is relatively single, and mainly depends on the inherent physical anti-digestion properties, but there is a lack of effective means in targeted enhancement of specific biological activities, such as promotion of growth-promoting ability of specific probiotics, imparting antioxidant or anti-inflammatory auxiliary functions, and improving loading and controlled release properties of active ingredients when used as drug carriers. Finally, conventional reagents such as citric acid, acetic anhydride or octenyl succinic anhydride are mostly adopted in the common chemical modification method, and although the physical and chemical properties of dextrin can be changed to a certain extent, the introduced groups are not novel enough and can not meet the dual severe requirements of the food and medicine fields on safety and functionality. In order to break through the technical bottleneck, the industry is required to develop an innovative strategy for synchronously realizing the improvement of the purity and the diversification of the functions of the resistant dextrin product on the premise of not depending on an expensive purification process. The present invention is the innovative search in this context. The core idea is to design and synthesize two functional compounds which have brand new and safe structures and are suitable for the fields of foods and medicines, and accurately introduce the functional compounds into the molecular skeleton of the resistant dextrin by using the functional compounds as key modifiers through an efficient covalent modification process. This strategy is not only expected to further enhance the anti-digestion properties of the product by the introduced steric hindrance and hydrophobic interactions, but is more focused on imparting potential targeted prebiotic activity, mucosal affinity, and enhanced drug binding capacity to the final product by the specific functional groups grafted. The complete preparation scheme provided by the invention forms a system solution from the synthesis of two special modifiers to the integration and application of the special modifiers in the formation process of the resistant dextrin, and aims to finally obtain a novel resistant dextrin product with high purity, low density and compounding functions, thereby meeting the increasing demands of modern functional foods and high-end drug delivery systems on high-performance auxiliary materials. Disclosure of Invention Aiming at the defects of the prior art, the invention aims to provide high-purity low-density resistant dextrin and a preparation method thereof. In a first aspect of the present invention, there is provided a process for the preparation of high purity low density resistant dextrins, comprising the steps of: S1, mixing 80-120 parts of corn starch and 400-600 parts of deionized water in parts by weight, sti