CN113209913B - Preparation method of caramel-colored hydrogel - Google Patents
Preparation method of caramel-colored hydrogel Download PDFInfo
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- CN113209913B CN113209913B CN202110455174.7A CN202110455174A CN113209913B CN 113209913 B CN113209913 B CN 113209913B CN 202110455174 A CN202110455174 A CN 202110455174A CN 113209913 B CN113209913 B CN 113209913B
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- 239000000017 hydrogel Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 57
- 238000006243 chemical reaction Methods 0.000 claims abstract description 36
- 150000001720 carbohydrates Chemical class 0.000 claims abstract description 30
- 239000000940 FEMA 2235 Substances 0.000 claims abstract description 29
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000001816 cooling Methods 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 8
- 238000004321 preservation Methods 0.000 claims abstract description 8
- 239000002253 acid Substances 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 31
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 18
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- 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 10
- 229930006000 Sucrose Natural products 0.000 claims description 10
- 239000005720 sucrose Substances 0.000 claims description 10
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 8
- 238000004939 coking Methods 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 239000012295 chemical reaction liquid Substances 0.000 claims description 7
- 235000019534 high fructose corn syrup Nutrition 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- 150000005846 sugar alcohols Polymers 0.000 claims description 5
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 claims 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 claims description 4
- 229930195725 Mannitol Natural products 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- TVXBFESIOXBWNM-UHFFFAOYSA-N Xylitol Natural products OCCC(O)C(O)C(O)CCO TVXBFESIOXBWNM-UHFFFAOYSA-N 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 4
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 4
- 239000008103 glucose Substances 0.000 claims description 4
- 239000000594 mannitol Substances 0.000 claims description 4
- 235000010355 mannitol Nutrition 0.000 claims description 4
- HEBKCHPVOIAQTA-UHFFFAOYSA-N meso ribitol Natural products OCC(O)C(O)C(O)CO HEBKCHPVOIAQTA-UHFFFAOYSA-N 0.000 claims description 4
- 239000000811 xylitol Substances 0.000 claims description 4
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 claims description 4
- 235000010447 xylitol Nutrition 0.000 claims description 4
- 229960002675 xylitol Drugs 0.000 claims description 4
- 235000020357 syrup Nutrition 0.000 claims description 3
- 239000006188 syrup Substances 0.000 claims description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 239000002798 polar solvent Substances 0.000 abstract description 2
- MIDXCONKKJTLDX-UHFFFAOYSA-N 3,5-dimethylcyclopentane-1,2-dione Chemical compound CC1CC(C)C(=O)C1=O MIDXCONKKJTLDX-UHFFFAOYSA-N 0.000 abstract 1
- 235000013736 caramel Nutrition 0.000 abstract 1
- 235000013305 food Nutrition 0.000 description 5
- 238000004040 coloring Methods 0.000 description 4
- 235000012970 cakes Nutrition 0.000 description 2
- 235000019219 chocolate Nutrition 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 235000015110 jellies Nutrition 0.000 description 2
- 239000008274 jelly Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000010146 3D printing Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 235000013365 dairy product Nutrition 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000000576 food coloring agent Substances 0.000 description 1
- 235000011194 food seasoning agent Nutrition 0.000 description 1
- 235000021433 fructose syrup Nutrition 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 235000013555 soy sauce Nutrition 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 235000021419 vinegar Nutrition 0.000 description 1
- 239000000052 vinegar Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 235000014101 wine Nutrition 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0052—Preparation of gels
- B01J13/0065—Preparation of gels containing an organic phase
-
- 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
- A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
- A23L5/40—Colouring or decolouring of foods
- A23L5/42—Addition of dyes or pigments, e.g. in combination with optical brighteners
- A23L5/47—Addition of dyes or pigments, e.g. in combination with optical brighteners using synthetic organic dyes or pigments not covered by groups A23L5/43 - A23L5/46
- A23L5/48—Compounds of unspecified constitution characterised by the chemical process for their preparation
-
- 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
Abstract
The invention discloses a preparation method of caramel hydrogel, which comprises the following steps: firstly, adjusting the pH value of the glucide to 1.0-3.5 by using acid, heating to 100-120 ℃, and reacting for 1-5 hours to complete the dehydration reaction of the glucide; secondly, adding polyhydroxy alcohol into the solution obtained in the first step after the dehydration reaction of the saccharides at the temperature of 130-150 ℃, controlling the temperature of the reaction solution at 140-160 ℃, and reacting for 2.5-5 hours under the protection of nitrogen; thirdly, sequentially adding hot water and a sodium hydroxide solution into the reaction solution obtained after the heat preservation reaction in the second step, wherein the hot water and the sodium hydroxide solution respectively account for 10-30% and 4-6% of the dry weight of the saccharides; adjusting the baume degree to be 34-38 DEG Be, cooling the reaction material to room temperature to obtain the caramel-color hydrogel, wherein the prepared caramel-color hydrogel has low solubility in a polar solvent at normal temperature.
Description
Technical Field
The invention belongs to the technical field of caramel color production, and particularly relates to a preparation method of caramel color hydrogel.
Background
Caramel color is an edible pigment obtained from saccharides by caramelization or Maillard reaction. As an important food colorant, the colorant is widely used for toning or coloring various products such as soy sauce, vinegar, wine, beverage, baked food, compound seasoning and the like. With the increasing application requirements and application range of the industries and the emerging application requirements of new industries, the caramel color has higher requirements on the coloring performance and the coloring morphology. At present, the application forms of caramel color mainly comprise two forms of liquid and powder, and because the caramel color is a macromolecular pigment substance with strong hydrophilicity, the application requirements of the caramel color in a weak polar system are limited to a great extent, particularly, the caramel color powder has strong moisture absorption characteristics and has higher technical requirements on links of production, storage, transportation, application and the like.
The polymer hydrogel is a three-dimensional network structure between liquid and solid, has the performances of formability, film-forming property, cohesiveness and the like, is widely applied to the biological food and medicine industry, and provides good opportunity for the development of the coloring form of caramel color and the development of a new application field. In the caramel color reaction process, the graft modification treatment is carried out on the caramel color by adopting the polyhydric alcohol to form the caramel color hydrogel, thereby providing feasibility for expanding the application range of the caramel color. At present, no report is found on the preparation of caramel-colored hydrogel by polyol graft modification.
Disclosure of Invention
The invention aims to provide a preparation method of caramel-colored hydrogel, the solubility of the caramel-colored hydrogel prepared by the method in a polar solvent is very low at normal temperature, the problem of the application requirement of the caramel color in a weak polar system and a forming system is solved, the prepared caramel-colored hydrogel is suitable for application in food industries such as jelly, cakes, chocolate, dairy products and the like, and the application range of the caramel color is further expanded.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the first aspect of the present invention provides a method for preparing a caramel-colored hydrogel, comprising the steps of:
step one, dehydration reaction: adjusting the pH value of the saccharide to 1.0-3.5 (preferably 2.5-3.5) by using acid, heating to 100-120 ℃, and reacting for 1-5 hours to complete the dehydration reaction of the saccharide;
step two, coking and grafting reaction: adding polyhydric alcohol into the solution which is subjected to the dehydration reaction of the saccharide substances in the first step at the temperature of 130-150 ℃, controlling the temperature of the reaction solution to be 140-160 ℃, and reacting for 2.5-5 hours under the protection of nitrogen;
the mass of the polyhydroxy alcohol accounts for 5-30% of the dry weight of the saccharide;
step three, modulation and cooling: sequentially adding hot water and a sodium hydroxide solution (with the mass concentration of 30%) into the reaction liquid after the second-step heat preservation reaction is finished, wherein the hot water and the sodium hydroxide solution respectively account for 10-30% (preferably 12-22%) and 4-6% of the dry weight of the saccharides; adjusting the baume degree to be 34-38 DEG Be, and cooling the reaction material to room temperature to obtain the caramel-color hydrogel.
The saccharide is at least one selected from sucrose aqueous solution, glucose syrup, and high fructose syrup (F42 or F55).
The acid is at least one of sulfuric acid, phosphoric acid and citric acid.
The polyhydric alcohol is at least one selected from glycerol, n-butanol, xylitol and mannitol.
The sucrose aqueous solution is prepared by dissolving sucrose in water, and the mass concentration of the sucrose aqueous solution is 70-80%, preferably 73.3%.
The temperature of the hot water is 80-90 ℃, and is preferably 85 ℃.
The sodium hydroxide solution is prepared by dissolving sodium hydroxide in water.
The room temperature is 5-35 ℃.
Due to the adoption of the technical scheme, the invention has the following advantages and beneficial effects:
the preparation method of the caramel-color hydrogel provided by the invention is suitable for application in food industries such as jelly, cake, chocolate and the like by grafting and modifying the caramel color through the polyhydroxy alcohol in the stage of the caramel color coking and color conversion reaction, and solves the technical problem of application requirements of the existing caramel color in a weak polarity system and a forming system. Meanwhile, feasibility is provided for the application of non-food industries such as 3D printing, drug slow release, biosensors and the like, so that the application range of the caramel color is expanded to a great extent, and the comprehensive utilization value of the caramel color is improved.
Detailed Description
In order to more clearly illustrate the invention, the invention is further described below in connection with preferred embodiments. It is to be understood by persons skilled in the art that the following detailed description is illustrative and not restrictive, and is not to be taken as limiting the scope of the invention.
Example 1
A38 ℃ B.caramel-colored hydrogel was produced (The. B means the Baume value of the caramel color).
A preparation method of caramel-colored hydrogel comprises the following steps:
step one, dehydration reaction: adjusting the pH value of 100kg of high fructose corn syrup (F42, dry basis is 72.0%) to 2.5 by using sulfuric acid, heating to 100 ℃, and reacting for 5 hours to complete the dehydration reaction of saccharides;
step two, coking and grafting reaction: adding 7.2kg of glycerol into the solution after the dehydration reaction of the saccharide substances in the first step at the temperature of 130-136 ℃, controlling the temperature of the reaction solution to be 140-150 ℃, and reacting for 3 hours under the protection of nitrogen;
the mass of the glycerol accounts for 10% of the dry weight of the high fructose corn syrup;
step three, modulation and cooling: adding 15.84kg of hot water with the temperature of 85 ℃ and 2.88kg of sodium hydroxide solution (with the mass concentration of 30%) into the reaction liquid after the second heat preservation reaction is finished, wherein the hot water and the sodium hydroxide solution respectively account for 22% and 4% of the dry weight of the saccharides; adjusting the baume degree to 38 DEG Be, and cooling the reaction material to room temperature to obtain the caramel-colored hydrogel.
Example 2
Production of 34 ℃ Becaramel-colored hydrogels
A preparation method of caramel-colored hydrogel comprises the following steps:
step one, dehydration reaction: adjusting the pH value of 120kg of glucose syrup (dry basis is 72.0%) to 2.5 by using sulfuric acid, heating to 120 ℃, and reacting for 2 hours to complete the dehydration reaction of saccharides;
step two, coking and grafting reaction: adding 25.9kg of n-butanol into the solution for completing the dehydration reaction of the saccharide substances in the first step at the temperature of 135-145 ℃, controlling the temperature of the reaction solution to be 145-155 ℃, and reacting for 3 hours under the protection of nitrogen;
the mass of the n-butanol accounts for 30% of the dry weight of the glucose mother liquor;
step three, modulation and cooling: adding 12kg of hot water with the temperature of 85 ℃ and 4.32kg of sodium hydroxide solution (with the mass concentration of 30%) into the reaction liquid after the second heat preservation reaction is finished, wherein the hot water and the sodium hydroxide solution respectively account for 13.9% and 5% of the dry weight of the saccharides; adjusting the baume degree to 34 Be, and cooling the reaction material to room temperature to obtain the caramel-color hydrogel.
Example 3
Production of 35 ℃ Becaramel-colored hydrogels
A preparation method of caramel-colored hydrogel comprises the following steps:
step one, dehydration reaction: adjusting the pH value of 100kg of high fructose corn syrup (F55, dry basis is 72.0%) to 3 by using sulfuric acid, heating to 115 ℃, and reacting for 1.5 hours to complete the dehydration reaction of saccharides;
step two, coking and grafting reaction: under the condition that the temperature is 135-140 ℃, 14.4kg of xylitol is added into the solution which completes the dehydration reaction of the saccharide substances in the first step, the temperature of the reaction solution is controlled to be 140-150 ℃, and the reaction is carried out for 5 hours under the condition of nitrogen protection;
the mass of the xylitol accounts for 20% of the dry weight of the high fructose corn syrup;
step three, modulation and cooling: adding 14kg of hot water with the temperature of 85 ℃ and 4.32kg of sodium hydroxide solution (with the mass concentration of 30%) into the reaction liquid after the second heat preservation reaction is finished, wherein the hot water and the sodium hydroxide solution respectively account for 19.4% and 6% of the dry weight of the saccharides; adjusting the baume degree to 35 Be, and cooling the reaction material to room temperature to obtain the caramel-color hydrogel.
Example 4
Production of 36 ℃ Becaramel-coloured hydrogels
A preparation method of caramel-colored hydrogel comprises the following steps:
step one, dehydration reaction: adjusting the pH value of 100kg of high fructose corn syrup (F42, dry basis is 72.0%) to 3.5 by using sulfuric acid, heating to 120 ℃, and reacting for 1 hour to complete the dehydration reaction of saccharides;
step two, coking and grafting reaction: adding 3.6kg of mannitol into the solution which is subjected to the dehydration reaction of the saccharide substance in the first step at the temperature of 140-150 ℃, controlling the temperature of the reaction solution to 145-155 ℃, and reacting for 3 hours under the protection of nitrogen;
the mass of the mannitol accounts for 5% of the dry weight of the high fructose corn syrup;
step three, modulation and cooling: adding 15kg of hot water with the temperature of 85 ℃ and 4.32kg of sodium hydroxide solution (with the mass concentration of 30%) into the reaction liquid after the second heat preservation reaction is finished, wherein the hot water and the sodium hydroxide solution respectively account for 20.8% and 6% of the dry weight of the saccharides; adjusting the baume degree to 36 DEG Be, and cooling the reaction material to room temperature to obtain the caramel-colored hydrogel.
Example 5
Production of 35 ℃ Becaramel-colored hydrogels
A preparation method of caramel-colored hydrogel comprises the following steps:
step one, dehydration reaction: weighing 110kg of sucrose and 40kg of water, placing the sucrose and the water in a reaction kettle, stirring and dissolving, adjusting the pH value to 3 by using citric acid, heating to 105 ℃, and reacting for 5 hours to complete the dehydration reaction of the saccharides;
step two, coking and grafting reaction: adding 14.4kg of glycerol into the solution after the dehydration reaction of the saccharides is completed in the first step at the temperature of 145-150 ℃, controlling the temperature of the reaction solution to be 155-160 ℃, and reacting for 2.5 hours under the protection of nitrogen;
the mass of the glycerol accounts for 13% of the weight of the sucrose;
step three, modulation and cooling: adding 13.2kg of hot water with the temperature of 85 ℃ and 4.95kg of sodium hydroxide solution (the mass concentration is 30%) into the reaction liquid after the second heat preservation reaction is finished, wherein the hot water and the sodium hydroxide solution respectively account for 12% and 4.5% of the dry weight of the saccharides; adjusting the baume degree to 35 Be, and cooling the reaction material to room temperature to obtain the caramel-color hydrogel.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (8)
1. A preparation method of caramel-colored hydrogel is characterized by comprising the following steps:
step one, dehydration reaction: adjusting the pH value of the saccharide to 1.0-3.5 by using acid, heating to 100-120 ℃, and reacting for 1-5 hours to complete the dehydration reaction of the saccharide;
step two, coking and grafting reaction: adding polyhydric alcohol into the solution which is subjected to the dehydration reaction of the saccharide substances in the first step at the temperature of 130-150 ℃, controlling the temperature of the reaction solution to be 140-160 ℃, and reacting for 2.5-5 hours under the protection of nitrogen;
the mass of the polyhydroxy alcohol accounts for 5-30% of the dry weight of the saccharide;
thirdly, modulating and cooling: sequentially adding hot water and a sodium hydroxide solution into the reaction liquid after the second-step heat preservation reaction, wherein the hot water and the sodium hydroxide solution respectively account for 10-30% and 4-6% of the dry weight of the saccharides; adjusting the baume degree to be 34-38 DEG Be, and cooling the reaction material to room temperature to obtain the caramel-color hydrogel.
2. The method for producing a caramel-colored hydrogel according to claim 1, wherein the saccharide is at least one selected from the group consisting of an aqueous solution of sucrose, glucose syrup and glucose-fructose syrup.
3. The method of claim 1, wherein the acid is at least one selected from the group consisting of sulfuric acid, phosphoric acid, and citric acid.
4. The method for preparing a caramel-colored hydrogel according to claim 1, wherein the polyhydric alcohol is at least one selected from the group consisting of glycerol, n-butanol, xylitol and mannitol.
5. The method for preparing the caramel-colored hydrogel according to claim 2, wherein the sucrose solution is prepared by dissolving sucrose in water at a mass concentration of 70-80%.
6. The method for preparing caramel-colored hydrogel according to claim 1, wherein the temperature of the hot water is 80 to 90 ℃.
7. The method of claim 1, wherein the sodium hydroxide solution is present at a concentration of 30% by mass.
8. The method for preparing caramel-colored hydrogels according to claim 1, wherein the room temperature is 5-35 ℃.
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