CN114231577A - Porous etherified potato starch and preparation method and application thereof - Google Patents
Porous etherified potato starch and preparation method and application thereof Download PDFInfo
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- 229920001592 potato starch Polymers 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 229920002472 Starch Polymers 0.000 claims abstract description 122
- 235000019698 starch Nutrition 0.000 claims abstract description 122
- 239000008107 starch Substances 0.000 claims abstract description 121
- 235000013336 milk Nutrition 0.000 claims abstract description 51
- 239000008267 milk Substances 0.000 claims abstract description 51
- 210000004080 milk Anatomy 0.000 claims abstract description 51
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 51
- 238000002156 mixing Methods 0.000 claims abstract description 27
- 239000007853 buffer solution Substances 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- 238000001035 drying Methods 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims abstract description 19
- 238000005406 washing Methods 0.000 claims abstract description 19
- 238000006266 etherification reaction Methods 0.000 claims abstract description 16
- 239000003513 alkali Substances 0.000 claims abstract description 14
- 238000001179 sorption measurement Methods 0.000 claims abstract description 13
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims abstract description 11
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims abstract description 9
- 235000013305 food Nutrition 0.000 claims abstract description 9
- 229910052938 sodium sulfate Inorganic materials 0.000 claims abstract description 9
- 235000011152 sodium sulphate Nutrition 0.000 claims abstract description 9
- 239000003814 drug Substances 0.000 claims abstract description 8
- 239000004382 Amylase Substances 0.000 claims abstract description 7
- 102000013142 Amylases Human genes 0.000 claims abstract description 7
- 108010065511 Amylases Proteins 0.000 claims abstract description 7
- 235000019418 amylase Nutrition 0.000 claims abstract description 7
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 18
- 102000004190 Enzymes Human genes 0.000 claims description 17
- 108090000790 Enzymes Proteins 0.000 claims description 17
- 239000000243 solution Substances 0.000 claims description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 13
- 239000012141 concentrate Substances 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 9
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 9
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 9
- 244000061456 Solanum tuberosum Species 0.000 claims description 8
- 235000002595 Solanum tuberosum Nutrition 0.000 claims description 8
- 229960000583 acetic acid Drugs 0.000 claims description 7
- 239000012362 glacial acetic acid Substances 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 6
- 239000002131 composite material Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 abstract description 14
- 150000001875 compounds Chemical class 0.000 abstract description 11
- 239000011148 porous material Substances 0.000 abstract description 6
- 239000002245 particle Substances 0.000 abstract description 5
- 239000008187 granular material Substances 0.000 abstract description 3
- 239000007788 liquid Substances 0.000 abstract 1
- 229940088598 enzyme Drugs 0.000 description 16
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 7
- 102000004139 alpha-Amylases Human genes 0.000 description 6
- 108090000637 alpha-Amylases Proteins 0.000 description 6
- 229940024171 alpha-amylase Drugs 0.000 description 6
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 5
- 229940040526 anhydrous sodium acetate Drugs 0.000 description 5
- 230000018044 dehydration Effects 0.000 description 5
- 238000006297 dehydration reaction Methods 0.000 description 5
- 229920000881 Modified starch Polymers 0.000 description 4
- 239000004368 Modified starch Substances 0.000 description 4
- 238000007385 chemical modification Methods 0.000 description 4
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 3
- 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
- 102000004157 Hydrolases Human genes 0.000 description 3
- 108090000604 Hydrolases Proteins 0.000 description 3
- 239000008103 glucose Substances 0.000 description 3
- 229920002521 macromolecule Polymers 0.000 description 3
- 235000019426 modified starch Nutrition 0.000 description 3
- 238000006467 substitution reaction Methods 0.000 description 3
- 230000009144 enzymatic modification Effects 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 125000002791 glucosyl group Chemical group C1([C@H](O)[C@@H](O)[C@H](O)[C@H](O1)CO)* 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 229920000856 Amylose Polymers 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- 240000008415 Lactuca sativa Species 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- DKVNPHBNOWQYFE-UHFFFAOYSA-N carbamodithioic acid Chemical compound NC(S)=S DKVNPHBNOWQYFE-UHFFFAOYSA-N 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 210000003850 cellular structure Anatomy 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 239000012990 dithiocarbamate Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002255 enzymatic effect Effects 0.000 description 1
- 230000007071 enzymatic hydrolysis Effects 0.000 description 1
- 238000006047 enzymatic hydrolysis reaction Methods 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- -1 hydroxypropyl Chemical group 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 235000012045 salad Nutrition 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- 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
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/30—Foods or foodstuffs containing additives; Preparation or treatment thereof containing carbohydrate syrups; containing sugars; containing sugar alcohols, e.g. xylitol; containing starch hydrolysates, e.g. dextrin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
- A61K47/36—Polysaccharides; Derivatives thereof, e.g. gums, starch, alginate, dextrin, hyaluronic acid, chitosan, inulin, agar or pectin
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- C08B31/00—Preparation of derivatives of starch
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- 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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- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/20—Preparation of compounds containing saccharide radicals produced by the action of an exo-1,4 alpha-glucosidase, e.g. dextrose
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- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
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Abstract
The invention discloses porous etherified potato starch and a preparation method and application thereof, and the specific preparation method comprises the steps of preparing starch milk by using a buffer solution with the pH value of 3.0-4.0, adding compound amylase for enzymolysis, centrifugally drying enzymolysis liquid to obtain porous potato starch, adding water for size mixing, adding 10-15% of sodium sulfate to inhibit expansion of starch granules, heating to 38-45 ℃, adding alkali to adjust the pH value to 10-13, then adding propylene oxide for etherification reaction, washing, concentrating and centrifugally drying after the reaction is finished to obtain the porous etherified potato starch. The prepared porous etherified potato starch has complete particle structure, obviously raised pore opening rate and pore diameter, greatly raised oil absorption and water absorption, capacity of being suitable for adsorption and embedding of various macromolecular matters in complicated conditions, and capacity of being used as one kind of lipophilic porous adsorption carrier for food, medicine and other fields.
Description
Technical Field
The invention belongs to the technical field of food and medicine, and particularly relates to porous etherified potato starch and a preparation method and application thereof.
Background
In the seventh and eighty years of the last century, students found that porous starch granules exist in animal excrement and alcohol fermentation residues, and the more clear definition of porous starch was firstly provided by Changgu Xinhong in Japan in 1998-enzymes with hydrolytic activity to raw starch degrade various starches at a temperature lower than the gelatinization temperature to obtain hydrolysates which are called porous starch. Porous starch is a novel enzyme-modified starch with a porous cellular structure. The surface of the porous starch is fully distributed with small holes with the diameter of about 1 mu m, the small holes go deep from the surface to the center, and the volume of the holes accounts for about 50 percent of the volume of the particles. Compared with natural starch, the porous starch has large specific pore volume and specific surface area and good water and oil absorption characteristics, but the water and oil absorption capacity, particularly the oil absorption capacity of the porous starch still cannot meet the requirements. In addition, the existing porous starch has the defects of low aperture ratio and small aperture, and cannot realize the adsorption and embedding of macromolecular substances.
Etherified starch is a chemically modified starch, which is prepared from native starch by chemical modification. The native starch is prepared by taking water as a medium and carrying out etherification reaction with propylene oxide, ethylene oxide and the like under an alkaline condition. At present, modified starch is mostly limited to single enzymatic modification or chemical modification, the problem of low lipophilicity generally exists in the enzymatic modified porous starch, and the lipophilicity rate is lower than 60%; the chemically modified etherified starch has no porous structure and relatively poor adsorption and embedding performance. Chinese patent discloses a preparation method of dithiocarbamate modified porous starch, potato starch is subjected to enzymatic hydrolysis to prepare porous starch, then the porous starch is subjected to crosslinking and etherification to prepare etherified porous starch, and then the modified starch prepared by polyamine and grafted carbon disulfide has the advantages of increased specific surface area, strong adsorption property and high adsorption selectivity. But the oil absorption is not good, so that the oil-absorbing porous adsorbent is difficult to be widely applied to the fields of food, medicine and the like as a lipophilic porous adsorption carrier.
Disclosure of Invention
Aiming at the problems that the porous starch in the prior art is low in oleophylic rate, low in opening rate and small in pore size and cannot adsorb and embed macromolecular substances, the invention provides porous etherified potato starch and a preparation method and application thereof. The porous etherified potato starch has high porosity, large specific surface area, obviously raised lipophilicity and hydrophilicity, and raised adsorption affinity.
The invention is realized by the following technical scheme:
a porous etherified potato starch is prepared by the following steps:
(1) preparing a buffer solution with the pH of 3.0-4.0, preparing starch milk according to a proportion, and heating to 45-55 ℃; adding 10-15 ml/Kg (absolutely dry starch) of composite amylase into starch milk, reacting for 12-20 h at 50-54 ℃, cooling to 35-45 ℃ after the reaction is finished, adding sodium bicarbonate to adjust pH to terminate the reaction, and then carrying out cyclone washing and concentration for 3-7 times to obtain porous starch refined milk;
(2) centrifugally drying the porous starch concentrate prepared in the step (1) until the water content is less than or equal to 8wt%, and preparing the porous potato starch;
(3) adding water into the potato porous starch prepared in the step (2) for size mixing, adding sodium sulfate accounting for 10-15% of the porous starch in absolute dry basis weight, uniformly stirring, heating to 38-45 ℃, then adding alkali liquor, adjusting the pH value to 10-13, adding epoxy propane accounting for 5-7% of the porous starch in absolute dry basis, carrying out etherification reaction for 14-24 hours, adding acid to adjust the pH value to 6.2-6.8 after the reaction is finished, terminating the reaction, washing and concentrating to obtain porous etherified refined starch milk;
(4) and (4) centrifugally drying the porous etherified refined starch milk prepared in the step (3) until the water content is less than or equal to 8wt%, thereby obtaining the porous etherified potato starch.
Further, the buffer solution in the step (1) is a sodium acetate-glacial acetic acid buffer solution with the pH value of 3.6, and the mass ratio of the absolutely dry potato starch to the buffer solution is 1: 1 to 1.5.
Further, the mass ratio of the composite amylase in the step (1) is 2-5: 1 of an alpha-amylase and a saccharifying enzyme;
further, the saccharifying enzyme is glucohydrolase.
Further, in the step (2), the mass ratio of the porous starch absolute dry basis to the water is 1: 1.2 to 1.8;
further, the alkali liquor in the step (3) is dilute alkali liquor with the mass concentration of 3%, and the acid is hydrochloric acid with the mass concentration of 5%.
The preparation method of the porous etherified potato starch comprises the following steps:
(1) preparing a buffer solution with the pH of 3.0-4.0, preparing starch milk according to a proportion, and heating to 45-55 ℃; adding 10-15 ml/Kg (absolutely dry starch) of composite amylase into starch milk, reacting for 12-20 h at 50-54 ℃, cooling to 35-45 ℃ after the reaction is finished, adding sodium bicarbonate to adjust pH to terminate the reaction, and then carrying out cyclone washing and concentration for 3-7 times to obtain porous starch refined milk;
(2) centrifugally drying the porous starch concentrate prepared in the step (1) until the water content is less than or equal to 8wt%, and preparing the porous potato starch;
(3) adding water into the potato porous starch prepared in the step (2) for size mixing, adding sodium sulfate accounting for 10-15% of the mass of the porous starch in the absolute dry basis for inhibiting the expansion of starch granules, uniformly stirring, heating to 38-45 ℃, then adding alkali liquor, adjusting the pH value to 10-13, adding propylene oxide accounting for 5-7% of the porous starch in the absolute dry basis, carrying out etherification reaction for 14-24 hours, adding acid to adjust the pH value to 6.2-6.8 after the reaction is finished, stopping the reaction, washing and concentrating to obtain porous etherified refined starch milk;
(4) and (4) centrifugally drying the porous etherified refined starch milk prepared in the step (3) until the water content is less than or equal to 8wt%, thereby obtaining the porous etherified potato starch.
According to the invention, the porous etherified potato starch is applied to the food or medicine field, and the porous etherified potato starch is applied to the food or medicine field as a lipophilic porous adsorption carrier.
According to the invention, an enzymatic modification method and a chemical modification method are combined, potato starch with larger starch particle size is selected, directional cutting and punching are carried out through a complex enzyme preparation, and an etherifying group is connected to a free porous starch glucose unit through chemical modification to obtain the porous etherified potato starch. The porous etherified starch prepared by the invention not only has a cellular porous structure, but also keeps the integrity of the granular structure of the potato starch; and part of the hydroxyl groups of the glucose units of the starch are replaced by etherification. The porous etherified potato starch has high porosity, great specific surface area, obviously raised lipophilicity and hydrophilicity, and raised adsorption affinity, and may be used as one kind of lipophilic porous adsorption carrier widely applied in food, medicine and other fields.
Advantageous effects
The porous etherified potato starch prepared by the method has a complete particle structure, the aperture ratio is more than or equal to 80%, the pore diameter is more than or equal to 1.5 mu m, the etherification substitution degree reaches MS more than or equal to 0.14, the oil absorption rate is more than or equal to 100%, the water absorption rate is more than or equal to 130%, the aperture ratio and the pore diameter are obviously improved, the oil absorption and water absorption are greatly improved, the porous etherified potato starch can adapt to various macromolecular substances, and the porous etherified potato starch can be adsorbed and embedded under complex working conditions and is widely applied to the fields of food, medicine and the like as a lipophilic porous adsorption carrier.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and the described embodiments are only a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The mean particle size of the potato starch described in the following examples was 35 μm, with an amylose content of 22%.
Example 1
(1) A buffer solution of ph3.6 (1.52 g of anhydrous sodium acetate, 13.89 g of glacial acetic acid dissolved in 1L of pure water to prepare a buffer solution) was prepared, according to the mass ratio of potato starch: buffer solution = 1: 1.25, blending the starch milk, uniformly stirring, and heating to 50 ℃ for later use; mixing alpha-amylase with a mass ratio of 3: 1: uniformly mixing glucose hydrolase to prepare a compound enzyme solution, adding the compound enzyme solution into starch milk according to 11.5ml/Kg (absolute dry starch), keeping the temperature of the starch milk at 50-54 ℃ for reaction for 14 hours, cooling to 40 ℃ after the reaction is finished, adding sodium bicarbonate to adjust the pH value to 6.0, and then carrying out cyclone washing and concentration for 4 times to prepare porous starch refined milk;
(2) centrifugally dewatering the porous starch concentrate prepared in the step (1) until the moisture content is less than or equal to 36%, and then drying until the moisture content is less than or equal to 8% to prepare the porous potato starch;
(3) according to the absolute dry basis of the potato porous starch: water = 1: 1.3, adding water to mix the slurry, adding sodium sulfate accounting for 15% of the porous starch absolute dry basis, stirring and mixing uniformly, heating to 42 ℃, adding 3% dilute alkali solution, adjusting the pH to 11.5, adding 5% epoxypropane accounting for 5% of the porous starch absolute dry basis, carrying out etherification reaction for 16 hours, then adding 5% hydrochloric acid, adjusting the pH to 6.2, washing and concentrating to obtain porous etherified refined starch milk;
(4) and (3) carrying out centrifugal dehydration on the porous etherified refined starch milk prepared in the step (3) until the water content is less than or equal to 38%, and then drying until the water content is less than or equal to 8% to obtain the porous etherified potato starch.
Example 2
(1) A buffer solution of ph3.6 (1.52 g of anhydrous sodium acetate, 13.89 g of glacial acetic acid dissolved in 1L of pure water to prepare a buffer solution) was prepared, according to the mass ratio of potato starch: buffer solution = 1: 1.25, blending the starch milk, uniformly stirring, and heating to 50 ℃ for later use; mixing alpha-amylase with a mass ratio of 3: 1: uniformly mixing glucose hydrolase to prepare a compound enzyme solution, adding the compound enzyme solution into starch milk according to 13.0ml/Kg (absolute dry starch), keeping the temperature of the starch milk at 50-54 ℃ for reacting for 16 hours, cooling to 40 ℃ after the reaction is finished, adding sodium bicarbonate to adjust the pH value to 6.0, and then carrying out cyclone washing and concentration for 5 times to prepare porous starch refined milk;
(2) centrifugally dewatering the porous starch concentrate prepared in the step (1) until the moisture content is less than or equal to 36%, and then drying until the moisture content is less than or equal to 8% to prepare the porous potato starch;
(3) according to the absolute dry basis of the potato porous starch: water = 1: 1.3, adding water to adjust the mass ratio, adding sodium sulfate accounting for 15% of the porous starch absolute dry basis, stirring and mixing uniformly, heating to 42 ℃, adding 3% dilute alkali solution, adjusting the pH to 11.5, adding 6% epoxypropane accounting for the porous starch absolute dry basis, carrying out etherification reaction for 18 hours, then adding 5% hydrochloric acid, adjusting the pH to 6.2, washing and concentrating to obtain porous etherified refined starch milk;
(4) and (3) carrying out centrifugal dehydration on the porous etherified refined starch milk prepared in the step (3) until the water content is less than or equal to 38%, and then drying until the water content is less than or equal to 8% to obtain the porous etherified potato starch.
Example 3
(1) A buffer solution of ph3.6 (1.52 g of anhydrous sodium acetate, 13.89 g of glacial acetic acid dissolved in 1L of pure water to prepare a buffer solution) was prepared, according to the mass ratio of potato starch: buffer solution = 1: 1.25, blending the starch milk, uniformly stirring, and heating to 50 ℃ for later use; mixing alpha-amylase with a mass ratio of 3: 1: uniformly mixing glucose hydrolase to prepare a compound enzyme solution, adding the compound enzyme solution into starch milk according to the volume of 14.5ml/Kg (absolute dry starch), keeping the temperature of the starch milk at 50-54 ℃ for reacting for 18 hours, cooling to 40 ℃ after the reaction is finished, adding sodium bicarbonate to adjust the pH value to 6.0, and then carrying out cyclone washing and concentration for 6 times to prepare porous starch refined milk;
(2) centrifugally dewatering the porous starch concentrate prepared in the step (1) until the moisture content is less than or equal to 36%, and then drying until the moisture content is less than or equal to 8% to prepare the porous potato starch;
(3) according to the absolute dry basis of the potato porous starch: water = 1: 1.3, adding water to mix the slurry, adding sodium sulfate accounting for 15% of the porous starch absolute dry basis, stirring and mixing uniformly, heating to 42 ℃, adding 3% dilute alkali solution, adjusting the pH to 11.5, adding 7% epoxypropane accounting for the porous starch absolute dry basis, carrying out etherification reaction for 20 hours, then adding 5% hydrochloric acid, adjusting the pH to 6.2, washing and concentrating to obtain porous etherified refined starch milk;
(4) and (3) carrying out centrifugal dehydration on the porous etherified refined starch milk prepared in the step (3) until the water content is less than or equal to 38%, and then drying until the water content is less than or equal to 8% to obtain the porous etherified potato starch.
Comparative example 1
(1) A buffer solution of ph3.6 was prepared (1.52 g anhydrous sodium acetate, 13.89 g glacial acetic acid dissolved in 1L pure water to prepare a buffer solution) according to potato starch oven dried: buffer solution = 1: 1.25, blending starch milk, stirring uniformly, and heating to 50 ℃ for later use; mixing alpha-amylase: saccharifying enzyme = 3:1, uniformly mixing to prepare a compound enzyme solution, adding the compound enzyme solution into starch milk according to 13ml/Kg (absolute dry starch), keeping the temperature of the starch milk at 50-54 ℃ for reacting for 16 hours, cooling to 40 ℃ after the reaction is finished, adding sodium bicarbonate to adjust the pH value to 6.0, and then carrying out cyclone washing and concentration for 5 times to prepare porous starch refined milk;
(2) and (2) centrifugally dewatering the porous starch concentrate prepared in the step (1) until the moisture content is less than or equal to 36%, and then drying until the moisture content is less than or equal to 8% to prepare the porous potato starch.
Comparative example 2
(1) According to the absolute dry basis of the potato starch: water = 1: 1.3, adding water for size mixing, adding sodium sulfate accounting for 15% of the absolute dry basis of the potato starch, stirring and mixing uniformly, heating to 42 ℃, adding 3% dilute alkali solution, adjusting the pH to 11.5, adding 7% epoxypropane accounting for the absolute dry basis of the potato starch, carrying out etherification reaction for 18 hours, then adding 5% hydrochloric acid, adjusting the pH to 6.2, washing and concentrating to obtain etherified refined starch milk;
(2) and (3) carrying out centrifugal dehydration on the etherified refined starch milk prepared in the step (2) until the water content is less than or equal to 38%, and then drying until the water content is less than or equal to 8% to obtain the potato etherified starch.
Comparative example 3
(1) A buffer solution of ph3.6 was prepared (1.52 g anhydrous sodium acetate, 13.89 g glacial acetic acid dissolved in 1L pure water to prepare a buffer solution) according to potato starch oven dried: buffer solution = 1: 1.25, blending starch milk, stirring uniformly, and heating to 50 ℃ for later use; mixing alpha-amylase: saccharifying enzyme = 3:1, uniformly mixing to prepare a compound enzyme solution, adding the compound enzyme solution into starch milk according to 13ml/Kg (absolute dry starch), keeping the temperature of the starch milk at 50-54 ℃ for reacting for 16 hours, cooling to 40 ℃ after the reaction is finished, adding sodium bicarbonate to adjust the pH value to 6.0, and then carrying out cyclone washing and concentration for 5 times to prepare porous starch refined milk;
(2) centrifugally dewatering the porous starch concentrate prepared in the step (1) until the moisture content is less than or equal to 36%, and then drying until the moisture content is less than or equal to 8% to prepare the porous potato starch;
(3) according to the porous starch absolute dry basis: water = 1: 1.3, adding water for size mixing, heating to 42 ℃, adding 3% of dilute alkali liquor, adjusting the pH to 11.5, adding 7% of propylene oxide of porous starch absolute dry basis, carrying out etherification reaction for 18 hours, then adding 5% of hydrochloric acid, adjusting the pH to 6.2, washing and concentrating to obtain porous etherified refined starch milk;
(4) and (3) carrying out centrifugal dehydration on the porous etherified refined starch milk prepared in the step (3) until the water content is less than or equal to 38%, and then drying until the water content is less than or equal to 8% to obtain the porous etherified potato starch.
Performance testing
And (3) measuring gelatinization temperature: the moisture contents of examples 1 to 3 and comparative examples 1 to 3 were measured, and a Brabender viscograph-E viscometer was selected according to the absolute concentration of 5%, and the measurement range was 700cmg, the temperature increase and decrease rate was 1.5 ℃/min, the initial temperature was 50 ℃, the minimum temperature was 30 ℃, the viscosity curve was measured, and the value of the gelatinization temperature T (. degree. C.) was observed.
And (3) water absorption and oil absorption determination: 10.0G (absolute dry) of the final product prepared in examples 1 to 3 and comparative examples 1 to 3 was accurately weighed in a 250ml beaker, 50ml of distilled water or salad oil was added and mixed in a water bath at 40 ℃ for 30min, and the mixture was filtered by a constant weight G4 sand core funnel until no water or oil was dropped, and the water absorption and oil absorption rate were calculated by weighing.
And (3) determining the etherification substitution degree: the hydroxypropyl contents WH (%) of examples 1 to 3 and comparative examples 1 to 3 were measured, and the etherification substitution degree MS, MS = 2.84 WH/(100-WH), was calculated by the method described in appendix A.4 of GB 29930.
TABLE 1 final product Performance test results for examples 1-3 and comparative examples 1-3
Claims (9)
1. A porous etherified potato starch is prepared by the following method:
(1) preparing a buffer solution with the pH of 3.0-4.0, preparing starch milk according to a proportion, and heating to 45-55 ℃; adding the composite amylase into starch milk according to the amount of 10-15 ml/Kg of absolutely dry starch, reacting for 12-20 hours at 50-54 ℃, cooling to 35-45 ℃ after the reaction is finished, adding sodium bicarbonate to adjust the pH value to terminate the reaction, and then carrying out cyclone washing and concentration for 3-7 times to obtain porous starch refined milk;
(2) centrifugally drying the porous starch concentrate prepared in the step (1) until the water content is less than or equal to 8wt%, and preparing the porous potato starch;
(3) adding water into the potato porous starch prepared in the step (2) for size mixing, adding sodium sulfate accounting for 10-15% of the porous starch in absolute dry basis weight, uniformly stirring, heating to 38-45 ℃, then adding alkali liquor, adjusting the pH value to 10-13, adding epoxy propane accounting for 5-7% of the porous starch in absolute dry basis, carrying out etherification reaction for 14-24 hours, adding acid to adjust the pH value to 6.2-6.8 after the reaction is finished, terminating the reaction, washing and concentrating to obtain porous etherified refined starch milk;
(4) and (4) centrifugally drying the porous etherified refined starch milk prepared in the step (3) until the water content is less than or equal to 8wt%, thereby obtaining the porous etherified potato starch.
2. The porous etherified potato starch of claim 1, wherein the buffer solution in step (1) is a sodium acetate-glacial acetic acid buffer solution having a pH of 3.6, and the mass ratio of the absolutely dry potato starch to the buffer solution is 1: 1 to 1.5.
3. The porous etherified potato starch as claimed in claim 1, wherein the composite amylase in the step (1) is prepared by mixing 2-5: 1 and a saccharifying enzyme.
4. Porous etherified potato starch as claimed in claim 3, wherein said saccharifying enzyme is glucohydrolase.
5. The porous etherified potato starch of claim 1 wherein in step (2), the mass ratio of the porous starch to water is 1: 1.2 to 1.8.
6. The porous etherified potato starch of claim 1, wherein the alkali solution in the step (3) is a dilute alkali solution having a mass concentration of 3%, and the acid is hydrochloric acid having a mass concentration of 5%.
7. A preparation method of porous etherified potato starch as set forth in any one of claims 1 to 6, comprising the steps of:
(1) preparing a buffer solution with the pH of 3.0-4.0, preparing starch milk according to a proportion, and heating to 45-55 ℃; adding the composite amylase into starch milk according to the amount of 10-15 ml/Kg of absolutely dry starch, reacting for 12-20 hours at 50-54 ℃, cooling to 35-45 ℃ after the reaction is finished, adding sodium bicarbonate to adjust the pH value to terminate the reaction, and then carrying out cyclone washing and concentration for 3-7 times to obtain porous starch refined milk;
(2) centrifugally drying the porous starch concentrate prepared in the step (1) until the water content is less than or equal to 8wt%, and preparing the porous potato starch;
(3) adding water into the potato porous starch prepared in the step (2) for size mixing, adding sodium sulfate accounting for 10-15% of the porous starch in absolute dry basis weight, uniformly stirring, heating to 38-45 ℃, then adding alkali liquor, adjusting the pH value to 10-13, adding epoxy propane accounting for 5-7% of the porous starch in absolute dry basis, carrying out etherification reaction for 14-24 hours, adding acid to adjust the pH value to 6.2-6.8 after the reaction is finished, terminating the reaction, washing and concentrating to obtain porous etherified refined starch milk;
(4) and (4) centrifugally drying the porous etherified refined starch milk prepared in the step (3) until the water content is less than or equal to 8wt%, thereby obtaining the porous etherified potato starch.
8. The application of the porous etherified potato starch as set forth in any one of claims 1-6 in the fields of food or medicine.
9. The use of claim 8, wherein said porous etherified potato starch is used as a lipophilic porous adsorption carrier in the food or pharmaceutical field.
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