CN106318991A - Resistant dextrin and preparation method thereof - Google Patents
Resistant dextrin and preparation method thereof Download PDFInfo
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- CN106318991A CN106318991A CN201610700623.9A CN201610700623A CN106318991A CN 106318991 A CN106318991 A CN 106318991A CN 201610700623 A CN201610700623 A CN 201610700623A CN 106318991 A CN106318991 A CN 106318991A
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- 229920001353 Dextrin Polymers 0.000 title claims abstract description 90
- 239000004375 Dextrin Substances 0.000 title claims abstract description 86
- 235000019425 dextrin Nutrition 0.000 title claims abstract description 86
- 238000002360 preparation method Methods 0.000 title claims abstract description 51
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 48
- 230000000694 effects Effects 0.000 claims abstract description 44
- 239000007788 liquid Substances 0.000 claims abstract description 37
- 102000004190 Enzymes Human genes 0.000 claims abstract description 32
- 108090000790 Enzymes Proteins 0.000 claims abstract description 32
- 229940088598 enzyme Drugs 0.000 claims abstract description 32
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 229920002472 Starch Polymers 0.000 claims abstract description 18
- 235000019698 starch Nutrition 0.000 claims abstract description 18
- 239000008367 deionised water Substances 0.000 claims abstract description 17
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 17
- 239000008107 starch Substances 0.000 claims abstract description 17
- 102000004139 alpha-Amylases Human genes 0.000 claims abstract description 14
- 108090000637 alpha-Amylases Proteins 0.000 claims abstract description 14
- 229940024171 alpha-amylase Drugs 0.000 claims abstract description 14
- 238000001914 filtration Methods 0.000 claims abstract description 14
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000002253 acid Substances 0.000 claims abstract description 13
- 239000003456 ion exchange resin Substances 0.000 claims abstract description 13
- 229920003303 ion-exchange polymer Polymers 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000000746 purification Methods 0.000 claims abstract description 5
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 30
- 235000013325 dietary fiber Nutrition 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 21
- 239000000463 material Substances 0.000 claims description 20
- 239000000376 reactant Substances 0.000 claims description 20
- 238000005903 acid hydrolysis reaction Methods 0.000 claims description 13
- 239000000843 powder Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 238000007445 Chromatographic isolation Methods 0.000 claims description 11
- 238000010612 desalination reaction Methods 0.000 claims description 11
- 230000008569 process Effects 0.000 claims description 11
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 10
- 229910052791 calcium Inorganic materials 0.000 claims description 10
- 239000011575 calcium Substances 0.000 claims description 10
- 235000015165 citric acid Nutrition 0.000 claims description 10
- 238000001704 evaporation Methods 0.000 claims description 10
- 230000008020 evaporation Effects 0.000 claims description 10
- 238000009413 insulation Methods 0.000 claims description 10
- 239000011347 resin Substances 0.000 claims description 10
- 229920005989 resin Polymers 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 10
- 230000003068 static effect Effects 0.000 claims description 10
- 238000002834 transmittance Methods 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- -1 DE value is 5~20 Substances 0.000 claims description 3
- 235000011167 hydrochloric acid Nutrition 0.000 claims description 3
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 2
- 229930006000 Sucrose Natural products 0.000 claims description 2
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 2
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 238000011097 chromatography purification Methods 0.000 claims description 2
- 238000004042 decolorization Methods 0.000 claims description 2
- 235000007983 food acid Nutrition 0.000 claims description 2
- 239000001630 malic acid Substances 0.000 claims description 2
- 235000011090 malic acid Nutrition 0.000 claims description 2
- 235000011007 phosphoric acid Nutrition 0.000 claims description 2
- 229920001592 potato starch Polymers 0.000 claims description 2
- 238000001223 reverse osmosis Methods 0.000 claims description 2
- 229940100486 rice starch Drugs 0.000 claims description 2
- 239000005720 sucrose Substances 0.000 claims description 2
- 239000001117 sulphuric acid Substances 0.000 claims description 2
- 235000011149 sulphuric acid Nutrition 0.000 claims description 2
- 240000003183 Manihot esculenta Species 0.000 claims 1
- 235000016735 Manihot esculenta subsp esculenta Nutrition 0.000 claims 1
- 150000003839 salts Chemical class 0.000 claims 1
- 239000013049 sediment Substances 0.000 claims 1
- 210000000582 semen Anatomy 0.000 claims 1
- 238000000926 separation method Methods 0.000 claims 1
- 238000001228 spectrum Methods 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 7
- 239000012295 chemical reaction liquid Substances 0.000 abstract 2
- 229910052799 carbon Inorganic materials 0.000 abstract 1
- 238000013375 chromatographic separation Methods 0.000 abstract 1
- 238000011033 desalting Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 26
- 235000013305 food Nutrition 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 14
- 238000001514 detection method Methods 0.000 description 12
- 230000036541 health Effects 0.000 description 10
- 229920002261 Corn starch Polymers 0.000 description 9
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- 238000012360 testing method Methods 0.000 description 9
- 230000004044 response Effects 0.000 description 8
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- 238000006116 polymerization reaction Methods 0.000 description 5
- 239000012043 crude product Substances 0.000 description 4
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229920000881 Modified starch Polymers 0.000 description 2
- 239000004368 Modified starch Substances 0.000 description 2
- DLRVVLDZNNYCBX-UHFFFAOYSA-N Polydextrose Polymers OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(O)O1 DLRVVLDZNNYCBX-UHFFFAOYSA-N 0.000 description 2
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- 238000004519 manufacturing process Methods 0.000 description 2
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- 239000004576 sand Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- 208000017667 Chronic Disease Diseases 0.000 description 1
- 229920002245 Dextrose equivalent Polymers 0.000 description 1
- 208000031226 Hyperlipidaemia Diseases 0.000 description 1
- 206010020772 Hypertension Diseases 0.000 description 1
- 208000013016 Hypoglycemia Diseases 0.000 description 1
- 102000004877 Insulin Human genes 0.000 description 1
- 108090001061 Insulin Proteins 0.000 description 1
- 244000151018 Maranta arundinacea Species 0.000 description 1
- 235000010804 Maranta arundinacea Nutrition 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 229920001100 Polydextrose Polymers 0.000 description 1
- 235000012419 Thalia geniculata Nutrition 0.000 description 1
- 241000209140 Triticum Species 0.000 description 1
- 235000021307 Triticum Nutrition 0.000 description 1
- 239000003377 acid catalyst Substances 0.000 description 1
- 235000008452 baby food Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 235000014633 carbohydrates Nutrition 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000002354 daily effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 208000002925 dental caries Diseases 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
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- 238000002651 drug therapy Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 235000013350 formula milk Nutrition 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000003345 hyperglycaemic effect Effects 0.000 description 1
- 230000002218 hypoglycaemic effect Effects 0.000 description 1
- 229940125396 insulin Drugs 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 235000012054 meals Nutrition 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 230000035764 nutrition Effects 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 239000001259 polydextrose Substances 0.000 description 1
- 235000013856 polydextrose Nutrition 0.000 description 1
- 229940035035 polydextrose Drugs 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000003716 rejuvenation Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
- 239000006188 syrup Substances 0.000 description 1
- 235000020357 syrup Nutrition 0.000 description 1
- 230000026676 system process Effects 0.000 description 1
- 238000002560 therapeutic procedure Methods 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/04—Polysaccharides, i.e. compounds containing more than five saccharide radicals attached to each other by glycosidic bonds
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
- A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
- A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
- A23L3/3463—Organic compounds; Microorganisms; Enzymes
- A23L3/3562—Sugars; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/14—Preparation of compounds containing saccharide radicals produced by the action of a carbohydrase (EC 3.2.x), e.g. by alpha-amylase, e.g. by cellulase, hemicellulase
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/18—Preparation of compounds containing saccharide radicals produced by the action of a glycosyl transferase, e.g. alpha-, beta- or gamma-cyclodextrins
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
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- Wood Science & Technology (AREA)
- Health & Medical Sciences (AREA)
- Microbiology (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Biotechnology (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Nutrition Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The invention relates to resistant dextrin and a preparation method thereof. The DE value of the resistant dextrin is 5 to 20; the water activity is less than or equal to 0.85, and the average molecular weight is 1000 to 2500. The preparation method of the resistant dextrin comprises the following steps: (1) adding acid into a starch raw material, performing high-temperature vacuum dextrinization reaction, then adding deionized water, performing acidolysis to prepare an acidolysis solution, then adding an enzymic preparation proportionally, and performing reaction to prepare reaction liquid; (2) decoloring the reaction liquid through active carbon, filtering with a plate frame, desalting macroporous ion exchange resin, then performing chromatographic separation purification, performing conventional concentration to obtain resistant dextrin concentrated liquid, and drying to obtain the resistant dextrin. By means of effectively controlling the temperature and the time of acidolysis and optimally adjusting the proportion of alpha-amylase and trans-glycosides enzyme which are added, the resistant dextrin with low water activity is finally prepared.
Description
Technical field
The present invention relates to a kind of resistant dextrin and preparation method thereof, belong to food additive production technical field.
Background technology
Along with the raising of people's living standard, a lot of people occur in that hyperlipidemia, hypertension, hyperglycemic symptoms, are commonly called as " three
High ", and have the trend of increasingly rejuvenation.World Health Organization (WHO) the most clearly proposes, and the first line of defence of anti-angiocardiopathy is just
It is to reduce " three high " and control " three high ".In the crowd of these three-hypers, except situation more serious need coordinate in addition to Drug therapy,
Majority of populations can be nursed one's health by modes such as diet dietetic therapies, it is to avoid side effects of pharmaceutical drugs.
Dietary fiber is a kind of water-insoluble and water-soluble fibre two can not to be divided into big by the carbohydrate of human consumption
Class.Country, in the middle of " 12 " planning, advocates the application of development dietary fiber, the potential danger that compatriots are caused by containment chronic disease
Evil, the dietary cellulose daily intaking amount that international linked groups is recommended is: cancer society of U.S. proposed standard for for each person every day 30～
40 grams, Food Science committee of European Economic Community proposed standard is 30 grams for each person every day.Chinese Soclety of Nutrition is recommended: human body every day
Dietary fiber intake is 25-35 gram.
Resistant dextrin is a kind of Low Caloric Polydextrose, fine with the low molecule aqueous soluble dietary that native starch is prepared for raw material
Dimension, relative to other diet fiber products, resistant dextrin has good acid, heat stability, and high digestion toleration, hypoglycemia refers to
Number, low insulin index, heat is low, prevents the excellent characteristics such as dental caries.
Chinese patent literature CN 104403009 A (application number 201410671093.0) discloses a kind of resistant dextrin
Preparation method, comprises the following steps: with acid treated starch as raw material, and employing sea sand is heat transfer medium, in hot conditions
Under carry out pyrolytic reaction, it is thus achieved that pyrodextrin crude product, pyrodextrin crude product obtains resistant dextrin product through refinement treatment again.
It is comprehensive that Chinese patent literature CN103725732A (application number 201310743226.6) discloses a kind of wheat C starch
The method of resistant dextrin is prepared in utilization, comprises the following steps: (1) starches as raw material with wheaten starch C starch, after adjusting pH with hydrochloric acid,
Seal acidifying；(2) it is dried after centrifugal for acidified starch slurry；(3) Pintsch process in roller heating stove；(4) it is cooled to room
Temperature, adds appropriate distilled water, is modulated into the emulsion of finite concentration scope；(5) double enzymes work in coordination with method liquefying-saccharifying synchronize carry out；
(6) add activated carbon decolorizing and sucking filtration obtains sample liquid；(7) feed liquid being carried out precipitate with ethanol, centrifugal, supernatant distilled spirit reclaims circulation profit
With, precipitation carries out pneumatic conveying drying, obtains the resistant dextrin that content is 85%-90%, and product yield is 80%-90%.
Chinese patent literature CN105542019A (application number 201610055348.X) disclose a kind of resistant dextrin and
Preparation method.Described resistant dextrin, molar content≤1% of DP1, molar content≤4.5% of DP2, DP3 rubs
That percentage composition≤7.0%, average degree of polymerization is 6～12, pH value 3.0～6.0, dietary fiber molar content >=85%.
The invention still further relates to the preparation method of above-mentioned resistant dextrin.Dextrinization reaction, with starch as raw material, is divided into two by the present invention first
In the individual stage, it is effectively guaranteed that the degree of polymerization of polyreaction, reduce the generation of side reaction simultaneously, greatly reduce purification subsequent treatment
Difficulty.
Resistant dextrin product moisture activity prepared by above-mentioned preparation method is higher, it is impossible to meet at food, health product extensive
Application, the most high-end food and field of health care products.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, it is provided that a kind of have the low resistant dextrin of water activity and preparation side thereof
Method.The resistant dextrin prepared through the present invention has that water activity is low, is difficult to deliquescence, good mouthfeel and mobility, it is simple at food
The most high-end food of product, health product and field of health care products are extensively applied.
The present inventor conducts in-depth research for the manufacture method with the resistant dextrin of low water activity, finds
With starch as raw material, add acid catalyst, in reactor, carry out the reaction of high temperature dextrinization, be subsequently adding deionized water and carry out acid
During solution prepares resistant dextrin, the temperature and time of the acidolysis that adds water is the key preparing low moisture activity resistant dextrin.
Term explanation
DP refers to the degree of polymerization (Degree of Polymerization), is the index weighing polymer molecule size, with
On the basis of repetitive glucose, i.e. the meansigma methods of contained repetitive glucose number on polymer macromolecule chain.
DE value i.e. Dextrose Equivalent, is reducing sugar (with the glucose meter) percentage ratio that accounts for syrup dry.
Water activity refers to the state that in food, moisture exists, i.e. moisture and food combination degree (free degree).Moisture
Activity value is the highest, and combination degree is the lowest；Water activity value is the lowest, and combination degree is the highest.Water activity determines that the food storage phase
One key factor of limit.As control growth of microorganism an important indicator, by reduce water activity can more added with
The control shelf life of power.
In order to realize the present invention, the present invention adopts the following technical scheme that
A kind of resistant dextrin, it is characterised in that described resistant dextrin, DE value is 5～20, water activity≤0.85, flat
Average molecular weight is 1000～2500.
According to currently preferred, the mean molecule quantity of described resistant dextrin is 1500～2000.
According to currently preferred, dietary fiber molar content >=85% of described resistant dextrin；Further preferably
, dietary fiber molar content >=90% of described resistant dextrin.
According to currently preferred, the pH value of described resistant dextrin is 3.5～6.5.
According to currently preferred, the sugariness of described resistant dextrin is the 0.2～0.35 of sucrose.
The preparation method of above-mentioned resistant dextrin, comprises the steps:
(1) adding acid in starch material, high-temperature vacuum dextrinization is reacted, is subsequently adding deionized water, is 55 in temperature
～acidolysis 10～40min under conditions of 75 DEG C, prepare acid hydrolysis solution, the ratio of 0.001%～0.005% the most by mass percentage
Add enzyme preparation, under the conditions of 40～50 DEG C, react 30～120min, prepare reactant liquor；
In described enzyme preparation, ratio alive is 1.2:1～20:1 to α-amylase with the enzyme of transglucosidase；
(2) reactant liquor step (1) prepared is through activated carbon decolorizing, plate-and-frame filtration, macroporous ion exchange resin desalination, so
After carry out chromatographic purification, Conventional concentration obtains resistant dextrin concentrated solution, then drying, prepare resistant dextrin.
According to currently preferred, the starch material in described step (1) is selected from: corn starch, wheaten starch, para arrowroot
One of powder, potato starch or rice starch；
According to currently preferred, in described step (1) acid adding proportion is starch material quality 0.01～
0.05%.
According to currently preferred, the acid in described step (1) is food acids；It is further preferred that described acid is selected from
One or more combination in citric acid, malic acid, hydrochloric acid, phosphoric acid, sulphuric acid.
According to currently preferred, in described step (1) temperature of high-temperature vacuum dextrinization reaction be 120～180 DEG C, true
Reciprocal of duty cycle is-0.09～-0.1MPa, and the time is 20～60min.
According to currently preferred, the deionized water in described step (1) is RO reverse osmosis water, and conductance is less than 50 μ S/cm；
The addition of deionized water is 20～50% for being adjusted to solid content.
According to currently preferred, the DE value of described acid hydrolysis solution is 15～50.
According to currently preferred, the decolorization condition in described step (2) for adjust pH value to 4.5～5.5, by percent mass
Activated carbon is added than the ratio of 0.5～1%, 85～90 DEG C of static insulations 40～60min, then stirring 20～30min.
According to currently preferred, the plate-and-frame filtration condition in described step (2) is: filter pressure 0.25～0.35Mpa,
Discharge 5.0～6.0t/h.
According to currently preferred, the macroporous ion exchange resin desalination in described step (2) uses continuous ionic exchange
System processes feed liquid, feed liquid light transmittance >=98% after handing over.Feed liquid after process is as clear as crystal, free from extraneous odour.
According to currently preferred, the chromatographic isolation in described step (2) uses calcium type chromatographic isolation resin, after purification
Feed liquid DE value 5～20.
According to currently preferred, the concentration condition in described step (2) is for using six effect plate evaporation concentration systems dense
It is reduced to the 60～70% of material liquid volume.
According to currently preferred, in described step (2) being dried for use drying tower be dried, baking temperature be 110～
120 DEG C, dried powder product moisture content≤5%.
Beneficial effect
The present invention by efficiently controlling the temperature and time of acidolysis, and to add α-amylase and the ratio of transglucosidase
Optimize and revise final prepared low moisture activity resistant dextrin.Owing to the resistant dextrin of low moisture activity can efficiently control shelf
Phase, the resistant dextrin that therefore present invention prepares can be widely used in food, the most high-end food of health product and health product neck
Territory.
Detailed description of the invention
Below in conjunction with embodiment, technical scheme is described further, but institute of the present invention protection domain is not limited to
This.
The detection method of water activity:
Use Aqualab water activity detector to detect, ready resistant dextrin is added directly into moisture and lives
Property detector specimen cup puts into groove room.For ensureing test normal operation, before putting into, remove bowl cover.Shutting groove lid, handlebar stem moves on to
Reading state.So meeting closed cell room, starts reading.After about 5 minutes, water activity value can show on the lcd screen.
The detection method of dietary fiber:
According to GB/T 22224-2008 " the mensuration enzymatic gravimetric method of dietary fiber and enzymatic gravimetric method-liquid chromatograph in food
Method " in the second method enzymatic gravimetric method-liquid chromatography detect.
The detection method of anti-moisture absorption:
The method specified according to GB 5009.3-2010 " mensuration of moisture in national food safety standard food " is carried out.
The detection method of dissolubility:
According in GB 5413.29-2010 " deliquescent mensuration in national food safety standard infant food and milk "
The mensuration of the second method dissolubility detects.
Embodiment 1
The preparation method of resistant dextrin, comprises the steps:
(1) in corn starch, add the citric acid of its quality 0.01%, 130 DEG C, under-0.09MPa pressure condition anti-
Carry out high temperature dextrinization reaction 20min in answering still, be subsequently adding deionized water and adjust solid content to carry out acidolysis, acidolysis temperature to 20%
Being 55 DEG C, the response time is 10min, and sampling detection acid hydrolysis solution DE is 15；
0.001% adds enzyme preparation the most by mass percentage, the enzyme of α-amylase and transglucosidase ratio alive in enzyme preparation
For 1.2:1, react 30min, prepare reactant liquor；
(2) step (1) preparing reactant liquor adjusts pH value to 4.5, and the ratio of 0.5% adds activated carbon by mass percentage,
At 85 DEG C of static insulation 40min, then stir 20min；Through plate-and-frame filtration, filter pressure 0.25Mpa, discharge 5.0t/h；Greatly
Ion exchange resin desalination, uses continuous ionic exchange system to process feed liquid, feed liquid light transmittance 98% after handing over；Then carry out
Calcium type chromatographic isolation resin separating-purifying, uses six effect plate evaporation concentration systems to be concentrated into the 60% of material liquid volume；Again through dry
Dry tower is dried, temperature 110 DEG C, dried powder product moisture content 4.5%；Prepare resistant dextrin.
The water activity of gained resistant dextrin is 0.845 after testing, and dietary fiber content is 91%, and mean molecule quantity is
1000, DE values 10.
Embodiment 2
The preparation method of resistant dextrin, comprises the steps:
(1) in corn starch, add the citric acid of its quality 0.02%, 150 DEG C, under-0.095MPa pressure condition anti-
Carry out high temperature dextrinization reaction 40min in answering still, be subsequently adding deionized water and adjust solid content to carry out acidolysis, acidolysis temperature to 35%
Being 60 DEG C, the response time is 20min, and sampling detection acid hydrolysis solution DE is 17；
0.003% ratio adds enzyme preparation the most by mass percentage, and in enzyme preparation, α-amylase is lived with the enzyme of transglucosidase
Ratio is 5:1, reacts 40min, prepares reactant liquor；
(2) step (1) preparing reactant liquor adjusts pH value to 4.8, and the ratio of 0.7% adds activated carbon by mass percentage,
At 87 DEG C of static insulation 50min, then stir 25min；Through plate-and-frame filtration, filter pressure 0.30Mpa, discharge 5.5t/h；Greatly
Ion exchange resin desalination, uses continuous ionic exchange system to process feed liquid, feed liquid light transmittance 99% after handing over；Then carry out
Calcium type chromatographic isolation resin separating-purifying, uses six effect plate evaporation concentration systems to be concentrated into the 65% of material liquid volume；Again through dry
Dry tower is dried, temperature 115 DEG C, dried powder product moisture content 4.5%；Prepare resistant dextrin.
The water activity of gained resistant dextrin is 0.84 after testing, and dietary fiber content is 90%, and mean molecule quantity is
2000, DE values 15.
Embodiment 3
The preparation method of resistant dextrin, comprises the steps:
(1) in corn starch, add the citric acid of its quality 0.03%, 160 DEG C, react under-0.1MPa pressure condition
Carrying out high temperature dextrinization reaction 50min in still, be subsequently adding deionized water and adjust solid content to carry out acidolysis to 40%, acidolysis temperature is
65 DEG C, the response time is 25min, and sampling detection acid hydrolysis solution DE is 18；
0.004% adds enzyme preparation the most by mass percentage, the enzyme of α-amylase and transglucosidase ratio alive in enzyme preparation
For 10:1, react 50min, prepare reactant liquor；
(2) step (1) preparing reactant liquor adjusts pH value to 4.9, and the ratio of 0.8% adds activated carbon by mass percentage,
At 88 DEG C of static insulation 50min, then stir 26min；Through plate-and-frame filtration, filter pressure 0.30Mpa, discharge 5.6t/h；Greatly
Ion exchange resin desalination, uses continuous ionic exchange system to process feed liquid, feed liquid light transmittance 99% after handing over；Then carry out
Calcium type chromatographic isolation resin separating-purifying, uses six effect plate evaporation concentration systems to be concentrated into the 66% of material liquid volume；Again through dry
Dry tower is dried, temperature 115 DEG C, dried powder product moisture content 4.5%；Prepare resistant dextrin.
The water activity of gained resistant dextrin is 0.825 after testing, and dietary fiber content is 92%, and mean molecule quantity is
1800, DE values 13.
Embodiment 4
The preparation method of resistant dextrin, comprises the steps:
(1) in corn starch, add the citric acid of its quality 0.04%, 170 DEG C, react under-0.1MPa pressure condition
Carrying out high temperature dextrinization reaction 60min in still, be subsequently adding deionized water and adjust solid content to carry out acidolysis to 50%, acidolysis temperature is
110 DEG C, the response time is 20min, and sampling detection acid hydrolysis solution DE is 20；
0.005% adds enzyme preparation the most by mass percentage, the enzyme of α-amylase and transglucosidase ratio alive in enzyme preparation
For 15:1, react 80min, prepare reactant liquor；
(2) step (1) preparing reactant liquor adjusts pH value to 5.5, and the ratio of 1% adds activated carbon by mass percentage,
90 DEG C of static insulation 60min, then stir 30min；Through plate-and-frame filtration, filter pressure 0.35Mpa, discharge 6.0t/h；Macropore
Ion exchange resin desalination, uses continuous ionic exchange system to process feed liquid, feed liquid light transmittance 99% after handing over；Then calcium is carried out
Type chromatographic isolation resin separating-purifying, uses six effect plate evaporation concentration systems to be concentrated into the 70% of material liquid volume；Drying again
Tower is dried, temperature 120 DEG C, dried powder product moisture content 4.0%；Prepare resistant dextrin.
The water activity of gained resistant dextrin is 0.835 after testing, and dietary fiber content is 90%, and mean molecule quantity is
2200, DE values 18.
Comparative example 1
The preparation method of resistant dextrin, comprises the steps:
(1) in corn starch, add the citric acid of its quality 0.01%, 130 DEG C, under-0.09MPa pressure condition anti-
Carry out high temperature dextrinization reaction 20min in answering still, be subsequently adding deionized water and adjust solid content to carry out acidolysis, acidolysis temperature to 20%
Being 35 DEG C, the response time is 5min, and sampling detection acid hydrolysis solution DE is 35；
0.001% ratio adds enzyme preparation the most by mass percentage, and in enzyme preparation, α-amylase is lived with the enzyme of transglucosidase
Ratio is 1.2:1, reacts 30min, prepares reactant liquor；
(2) step (1) preparing reactant liquor adjusts pH value to 4.5, and the ratio of 0.5% adds activated carbon by mass percentage,
At 85 DEG C of static insulation 40min, then stir 20min；Through plate-and-frame filtration, filter pressure 0.25Mpa, discharge 5.0t/h；Greatly
Ion exchange resin desalination, uses continuous ionic exchange system to process feed liquid, feed liquid light transmittance 98% after handing over；Then carry out
Calcium type chromatographic isolation resin separating-purifying, uses six effect plate evaporation concentration systems to be concentrated into the 60% of material liquid volume；Again through dry
Dry tower is dried, temperature 110 DEG C, dried powder product moisture content 4.5%；Prepare resistant dextrin.
The water activity of gained resistant dextrin is 0.86 after testing, and dietary fiber content is 75%, and mean molecule quantity is
300, DE values 30.
Comparative example 2
The preparation method of resistant dextrin, comprises the steps:
(1) in corn starch, add the citric acid of its quality 0.02%, 150 DEG C, under-0.095MPa pressure condition anti-
Carry out high temperature dextrinization reaction 40min in answering still, be subsequently adding deionized water and adjust solid content to carry out acidolysis, acidolysis temperature to 35%
Being 120 DEG C, the response time is 60min, and sampling detection acid hydrolysis solution DE is 55；
0.003% adds enzyme preparation the most by mass percentage, the enzyme of α-amylase and transglucosidase ratio alive in enzyme preparation
For 5:1, react 40min, prepare reactant liquor；
(2) step (1) preparing reactant liquor adjusts pH value to 4.8, and the ratio of 0.7% adds activated carbon by mass percentage,
At 87 DEG C of static insulation 50min, then stir 25min；Through plate-and-frame filtration, filter pressure 0.30Mpa, discharge 5.5t/h；Greatly
Ion exchange resin desalination, uses continuous ionic exchange system to process feed liquid, feed liquid light transmittance 99% after handing over；Then carry out
Calcium type chromatographic isolation resin separating-purifying, uses six effect plate evaporation concentration systems to be concentrated into the 65% of material liquid volume；Again through dry
Dry tower is dried, temperature 115 DEG C, dried powder product moisture content 4.5%；Prepare resistant dextrin.
The water activity of gained resistant dextrin is 0.88 after testing, and dietary fiber content is 60%, and mean molecule quantity is
200, DE values 50.
Comparative example 3
The preparation method of resistant dextrin, comprises the steps:
(1) in corn starch, add the citric acid of its quality 0.03%, 160 DEG C, react under-0.1MPa pressure condition
Carrying out high temperature dextrinization reaction 60min in still, be subsequently adding deionized water and adjust solid content to carry out acidolysis to 50%, acidolysis temperature is
65 DEG C, the response time is 25min, and sampling detection acid hydrolysis solution DE is 30；
0.005% ratio adds enzyme preparation the most by mass percentage, and in enzyme preparation, α-amylase is lived with the enzyme of transglucosidase
Ratio is 0.4:1, reacts 30min, prepares reactant liquor；
(2) step (1) preparing reactant liquor adjusts pH value to 4.9, and the ratio of 0.8% adds activated carbon by mass percentage,
At 88 DEG C of static insulation 50min, then stir 26min；Through plate-and-frame filtration, filter pressure 0.30Mpa, discharge 5.6t/h；Greatly
Ion exchange resin desalination, uses continuous ionic exchange system to process feed liquid, feed liquid light transmittance 99% after handing over；Then carry out
Calcium type chromatographic isolation resin separating-purifying, uses six effect plate evaporation concentration systems to be concentrated into the 66% of material liquid volume；Again through dry
Dry tower is dried, temperature 115 DEG C, dried powder product moisture content 4.5%；Prepare resistant dextrin.
The water activity of gained resistant dextrin is 0.90 after testing, and dietary fiber content is 65%, and mean molecule quantity is
400, DE values 25.
Comparative example 4
The preparation method of resistant dextrin, comprises the steps:
(1) in corn starch, add the citric acid of its quality 0.04%, 170 DEG C, react under-0.1MPa pressure condition
Carrying out high temperature dextrinization reaction 60min in still, be subsequently adding deionized water and adjust solid content to carry out acidolysis to 50%, acidolysis temperature is
110 DEG C, the response time is 20min, and sampling detection acid hydrolysis solution DE is 60；
0.005% adds enzyme preparation the most by mass percentage, the enzyme of α-amylase and transglucosidase ratio alive in enzyme preparation
For 30:1, react 80min, prepare reactant liquor；
(2) step (1) preparing reactant liquor adjusts pH value to 5.5, and the ratio of 1% adds activated carbon by mass percentage,
90 DEG C of static insulation 60min, then stir 30min；Through plate-and-frame filtration, filter pressure 0.35Mpa, discharge 6.0t/h；Macropore
Ion exchange resin desalination, uses continuous ionic exchange system to process feed liquid, feed liquid light transmittance 99% after handing over；Then calcium is carried out
Type chromatographic isolation resin separating-purifying, uses six effect plate evaporation concentration systems to be concentrated into the 70% of material liquid volume；Drying again
Tower is dried, temperature 120 DEG C, dried powder product moisture content 4.0%；Prepare resistant dextrin.
The water activity of gained resistant dextrin is 0.90 after testing, and dietary fiber content is 55%, and mean molecule quantity is
180, DE values 55.
By above example 1～4 and the water activity of resistant dextrin that obtains of comparative example 1～4 and dietary fiber content
Evaluation result collects and table 1.
The water activity of table 1 embodiment and comparative example gained resistant dextrin and the evaluation table of dietary fiber content
From above comparing result, when the temperature meeting acidolysis is 55～75 DEG C simultaneously, the time 10～40min, add
When adding the condition that ratio is 1.2:1～20:1 of α-amylase and transglucosidase, can obtain that water activity is low and dietary fiber contains
Measure high resistant dextrin, if the temperature only meeting acidolysis is 55～75 DEG C, the time 10～40min, or add α-amylase
During with the condition that ratio is 1.2:1～20:1 of transglucosidase, it is impossible to obtain same resistant dextrin.
Comparative example 5
Chinese patent literature CN 104403009 A (application number 201410671093.0) discloses a kind of resistant dextrin
Preparation method, comprises the following steps: with acid treated starch as raw material, and employing sea sand is heat transfer medium, in hot conditions
Under carry out pyrolytic reaction, it is thus achieved that pyrodextrin crude product, pyrodextrin crude product obtains resistant dextrin product through refinement treatment again.
Comparative example 6
Chinese patent literature CN105542019A (application number 201610055348.X) disclose a kind of resistant dextrin and
Preparation method.Described resistant dextrin, molar content≤1% of DP1, molar content≤4.5% of DP2, DP3 rubs
That percentage composition≤7.0%, average degree of polymerization is 6～12, pH value 3.0～6.0, dietary fiber molar content >=85%.
Its preparation method comprises the steps:
(1) ratio of 0.1%～0.5% adds acid solution in starch by mass percentage, stirs, and prepares reaction
Material；
(2) reaction material that step (1) prepares is warming up to 80 DEG C～120 DEG C, reacts 2～4h under normal pressure, prepare initial action
Material, then adds acid solution in the ratio of initial action material mass percent 1%～10% and stirs, be warming up to 140～200
DEG C, under condition of normal pressure, gelatinizing reaction 15～30min, prepare dextrin coarse fodder；
(3) adding deionized water in the dextrin coarse fodder that step (2) prepares, regulation sugar concentration is 40～45wt%, in temperature
Degree is incubated acidic hydrolysis 1～2 hours under the conditions of being 80～100 DEG C, prepares hydrolyzed solution；
(4) hydrolyzed solution step (3) prepared is through decolouring, from friendships, concentrations, purification, dry, prepared resistant dextrin.
Experimental example
Comparative example 5, comparative example 6 are analyzed as shown in table 2 with embodiment 3 product:
Table 2
| Project | Comparative example 5 | Comparative example 6 | Embodiment 3 |
| Mean molecule quantity | 3000-4000 | 2500-3500 | 1000-2500 |
| Water activity | 0.88 | 0.86 | 0.825 |
| Dietary fiber content | 82% | 85% | 92% |
| Anti-moisture absorption | 60% | 70% | 85% |
| Dissolubility | 70 | 90 | 100 |
From above contrast it can be seen that embodiment 3 resistant dextrin product is bright in water activity, anti-moisture absorption, dissolubility
Aobvious be better than comparative example 5 and comparative example 6 resistant dextrin product, have low moisture activity and agent of low hygroscopicity feature, meals simultaneously
Fiber content is the highest, can be widely used in food, the most high-end food of health product and field of health care products so that it is shelf life prolongs
Long.
Claims (10)
1. a resistant dextrin, it is characterised in that described resistant dextrin, DE value is 5～20, water activity≤0.85, averagely
Molecular weight is 1000～2500.
2. resistant dextrin as claimed in claim 1, it is characterised in that the mean molecule quantity of described resistant dextrin be 1500～
2000；
Preferably, dietary fiber molar content >=85% of described resistant dextrin；It is further preferred that described resistant dextrin
Dietary fiber molar content >=90%；
Preferably, the pH value of described resistant dextrin is 3.5～6.5；
Preferably, the sugariness of described resistant dextrin is the 0.2～0.35 of sucrose.
3. the preparation method of resistant dextrin described in claim 1, it is characterised in that comprise the steps:
(1) adding acid in starch material, high-temperature vacuum dextrinization is reacted, is subsequently adding deionized water, is 55～75 in temperature
Acidolysis 10～40min under conditions of DEG C, prepare acid hydrolysis solution, and the ratio of 0.001%～0.005% adds the most by mass percentage
Enzyme preparation, reacts 30～120min under the conditions of 40～50 DEG C, prepares reactant liquor；
In described enzyme preparation, ratio alive is 1.2:1～20:1 to α-amylase with the enzyme of transglucosidase；
(2) reactant liquor step (1) prepared is through activated carbon decolorizing, plate-and-frame filtration, macroporous ion exchange resin desalination, then enters
Row chromatographic purification, Conventional concentration obtains resistant dextrin concentrated solution, then drying, prepares resistant dextrin.
4. preparation method as claimed in claim 3, it is characterised in that the starch material in described step (1) is selected from: Semen Maydis forms sediment
One of powder, wheaten starch, tapioca, potato starch or rice starch；
Preferably, adding proportion is starch material quality 0.01～0.05% of the acid in described step (1).
Preferably, the acid in described step (1) is food acids；It is further preferred that described acid selected from citric acid, malic acid,
One or more combination in hydrochloric acid, phosphoric acid, sulphuric acid；
Preferably, in described step (1) temperature of high-temperature vacuum dextrinization reaction be 120～180 DEG C, vacuum for-0.09～-
0.1MPa, the time is 20～60min；
Preferably, the deionized water in described step (1) is RO reverse osmosis water, and conductance is less than 50 μ S/cm；The interpolation of deionized water
Amount is 20～50% for being adjusted to solid content；
According to currently preferred, the DE value of the acid hydrolysis solution in described step (1) is 15～50.
5. preparation method as claimed in claim 3, it is characterised in that the decolorization condition in described step (2) is for adjusting pH value extremely
4.5～5.5, by mass percentage 0.5～1% ratio add activated carbon, 85～90 DEG C of static insulations 40～60min, so
Rear stirring 20～30min.
6. preparation method as claimed in claim 3, it is characterised in that the plate-and-frame filtration condition in described step (2) is: filter
Pressure 0.25～0.35Mpa, discharge 5.0～6.0t/h.
7. preparation method as claimed in claim 3, it is characterised in that the macroporous ion exchange resin in described step (2) takes off
Salt uses continuous ionic exchange system to process feed liquid, feed liquid light transmittance >=98% after handing over.
8. preparation method as claimed in claim 3, it is characterised in that the chromatographic isolation in described step (2) uses calcium type color
Spectrum separation resin, the feed liquid DE value 5～20 after purification.
9. preparation method as claimed in claim 3, it is characterised in that the concentration condition in described step (2) is for using six effects
Plate evaporation concentration systems is concentrated into the 60～70% of material liquid volume.
10. preparation method as claimed in claim 3, it is characterised in that being dried as using drying tower to do in described step (2)
Dry, baking temperature is 110～120 DEG C, dried powder product moisture content≤5%.
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| CN110042134A (en) * | 2019-03-22 | 2019-07-23 | 广州华汇生物实业有限公司 | The preparation method of resistant dextrin |
| CN110295208B (en) * | 2019-06-28 | 2023-04-18 | 山东省食品发酵工业研究设计院 | Method for improving resistance and yield of resistant dextrin |
| CN110295208A (en) * | 2019-06-28 | 2019-10-01 | 山东省食品发酵工业研究设计院 | A method of promoting resistant dextrin resistance and yield |
| CN111455002A (en) * | 2020-04-14 | 2020-07-28 | 曲阜贝斯迪生物医药有限公司 | Preparation method of resistant dextrin |
| CN114262387A (en) * | 2021-12-29 | 2022-04-01 | 山东百龙创园生物科技股份有限公司 | Preparation method of resistant dextrin |
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