CN113930086A - Preparation method for improving color and stability of calcium carbonate edible lake - Google Patents
Preparation method for improving color and stability of calcium carbonate edible lake Download PDFInfo
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- CN113930086A CN113930086A CN202111208947.8A CN202111208947A CN113930086A CN 113930086 A CN113930086 A CN 113930086A CN 202111208947 A CN202111208947 A CN 202111208947A CN 113930086 A CN113930086 A CN 113930086A
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- calcium carbonate
- carbonate
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 title claims abstract description 141
- 229910000019 calcium carbonate Inorganic materials 0.000 title claims abstract description 70
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 92
- 239000000049 pigment Substances 0.000 claims abstract description 53
- 239000000243 solution Substances 0.000 claims abstract description 44
- 239000011259 mixed solution Substances 0.000 claims abstract description 39
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000002156 mixing Methods 0.000 claims abstract description 26
- 239000002244 precipitate Substances 0.000 claims abstract description 26
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 14
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims abstract description 12
- 159000000007 calcium salts Chemical class 0.000 claims abstract description 10
- 125000000129 anionic group Chemical group 0.000 claims abstract description 6
- 239000007864 aqueous solution Substances 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000000227 grinding Methods 0.000 claims abstract description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical group [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 60
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 14
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 12
- 239000001110 calcium chloride Substances 0.000 claims description 12
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 12
- 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 11
- 239000011734 sodium Substances 0.000 claims description 11
- 229910052708 sodium Inorganic materials 0.000 claims description 11
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 6
- 125000000542 sulfonic acid group Chemical group 0.000 claims description 4
- JMEVHYCNAPFOAB-UHFFFAOYSA-L 2-(3-hydroxy-5-sulfonato-1H-indol-2-yl)-3-oxoindole-5-sulfonate Chemical compound [O-]c1c([nH]c2ccc(cc12)S([O-])(=O)=O)C1=[NH+]c2ccc(cc2C1=O)S([O-])(=O)=O JMEVHYCNAPFOAB-UHFFFAOYSA-L 0.000 claims description 3
- SGHZXLIDFTYFHQ-UHFFFAOYSA-L Brilliant Blue Chemical compound [Na+].[Na+].C=1C=C(C(=C2C=CC(C=C2)=[N+](CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C=2C(=CC=CC=2)S([O-])(=O)=O)C=CC=1N(CC)CC1=CC=CC(S([O-])(=O)=O)=C1 SGHZXLIDFTYFHQ-UHFFFAOYSA-L 0.000 claims description 3
- 235000005979 Citrus limon Nutrition 0.000 claims description 3
- 244000131522 Citrus pyriformis Species 0.000 claims description 3
- NKWPZUCBCARRDP-UHFFFAOYSA-L calcium bicarbonate Chemical compound [Ca+2].OC([O-])=O.OC([O-])=O NKWPZUCBCARRDP-UHFFFAOYSA-L 0.000 claims description 3
- 229910000020 calcium bicarbonate Inorganic materials 0.000 claims description 3
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 3
- 235000009328 Amaranthus caudatus Nutrition 0.000 claims description 2
- 240000001592 Amaranthus caudatus Species 0.000 claims description 2
- 235000012741 allura red AC Nutrition 0.000 claims description 2
- 239000004191 allura red AC Substances 0.000 claims description 2
- 235000012735 amaranth Nutrition 0.000 claims description 2
- 239000004178 amaranth Substances 0.000 claims description 2
- 235000012730 carminic acid Nutrition 0.000 claims description 2
- DGQLVPJVXFOQEV-JNVSTXMASA-N carminic acid Chemical compound OC1=C2C(=O)C=3C(C)=C(C(O)=O)C(O)=CC=3C(=O)C2=C(O)C(O)=C1[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O DGQLVPJVXFOQEV-JNVSTXMASA-N 0.000 claims description 2
- CEZCCHQBSQPRMU-UHFFFAOYSA-L chembl174821 Chemical compound [Na+].[Na+].COC1=CC(S([O-])(=O)=O)=C(C)C=C1N=NC1=C(O)C=CC2=CC(S([O-])(=O)=O)=CC=C12 CEZCCHQBSQPRMU-UHFFFAOYSA-L 0.000 claims description 2
- IINNWAYUJNWZRM-UHFFFAOYSA-L erythrosin B Chemical compound [Na+].[Na+].[O-]C(=O)C1=CC=CC=C1C1=C2C=C(I)C(=O)C(I)=C2OC2=C(I)C([O-])=C(I)C=C21 IINNWAYUJNWZRM-UHFFFAOYSA-L 0.000 claims description 2
- 235000012732 erythrosine Nutrition 0.000 claims description 2
- 239000004174 erythrosine Substances 0.000 claims description 2
- 229940011411 erythrosine Drugs 0.000 claims description 2
- 150000005323 carbonate salts Chemical class 0.000 claims 1
- 235000013373 food additive Nutrition 0.000 abstract description 3
- 239000002778 food additive Substances 0.000 abstract description 3
- 239000013049 sediment Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 22
- 235000019441 ethanol Nutrition 0.000 description 22
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 20
- 238000003756 stirring Methods 0.000 description 20
- 238000001179 sorption measurement Methods 0.000 description 18
- 235000000177 Indigofera tinctoria Nutrition 0.000 description 11
- 229940097275 indigo Drugs 0.000 description 11
- COHYTHOBJLSHDF-UHFFFAOYSA-N indigo powder Natural products N1C2=CC=CC=C2C(=O)C1=C1C(=O)C2=CC=CC=C2N1 COHYTHOBJLSHDF-UHFFFAOYSA-N 0.000 description 11
- 239000002253 acid Substances 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 6
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 230000008859 change Effects 0.000 description 4
- 235000013305 food Nutrition 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000003463 adsorbent Substances 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 208000024827 Alzheimer disease Diseases 0.000 description 1
- 239000000120 Artificial Saliva Substances 0.000 description 1
- 206010006187 Breast cancer Diseases 0.000 description 1
- 208000026310 Breast neoplasm Diseases 0.000 description 1
- 206010039966 Senile dementia Diseases 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 229940069428 antacid Drugs 0.000 description 1
- 239000003159 antacid agent Substances 0.000 description 1
- 230000001458 anti-acid effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 229940069978 calcium supplement Drugs 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 235000010855 food raising agent Nutrition 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 210000005036 nerve Anatomy 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B63/00—Lakes
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention relates to the technical field of food additives, and provides a preparation method for improving the color and stability of an edible calcium carbonate lake, which comprises the following steps: s1, dissolving carbonate in water to prepare a carbonate aqueous solution; s2, adding water-soluble anionic pigment into the carbonated aqueous solution obtained in the S1 to obtain a mixed solution; s3, adding ethanol into the S2 mixed solution, fully mixing, and adjusting the pH value to 9-11; s4, dissolving the calcium salt in water, adding ethanol, mixing uniformly, mixing with the solution obtained in S3, performing ultrasonic treatment for 1-10 minutes, and centrifuging to collect calcium carbonate precipitate adsorbed with pigment; s5, drying and grinding the calcium carbonate sediment absorbed with the pigment obtained in the step S4 to obtain the edible calcium carbonate-based lake. By adopting the technical scheme, the color and the stability of the edible calcium carbonate lake are obviously improved.
Description
Technical Field
The invention relates to the technical field of food additives, in particular to a preparation method for improving the color and stability of calcium carbonate edible lake.
Background
The lake is a water-insoluble pigment product prepared by adsorbing a water-soluble pigment on a water-insoluble substrate, separating the substrate adsorbed with the pigment and drying. When the pigments, matrix and other agents used are food grade, the resulting lake is an edible lake. In the preparation of edible lakes, aluminum hydroxide is the traditional adsorbent matrix and is most widely used. Numerous studies have shown that excessive aluminum intake may lead to senile dementia, increase the incidence of breast cancer, and may affect the development of bone and nerves in the newborn, making aluminum hydroxide-based lakes questionable in terms of safety. At present, the search for safe and reliable adsorption matrix to replace aluminum hydroxide for preparing color lake is an urgent target to be achieved in the food pigment industry. Current research indicates that the use of calcium carbonate instead of aluminum hydroxide is a very promising solution.
Calcium carbonate is a common food additive, has wide application, and can be used as a calcium supplement, a coloring agent, a leavening agent, an antacid and the like. Calcium carbonate microparticles have a significant surface charge and flexible surface modifiability and can be used as adsorbents. Research shows that calcium carbonate has good adsorbability to various water-soluble anionic food pigments and the capability of preparing lakes.
The invention patent "a preparation method of edible lake based on calcium carbonate" (application number 201910512968.5) discloses a novel preparation technology of lake based on calcium carbonate: firstly, adding pigment into a carbonate solution to form a mixed solution, then adjusting the pH value, adding calcium salt, and then carrying out ultrasonic treatment, centrifugation, drying and grinding to prepare the edible calcium carbonate lake. Researches find that the adsorption between the calcium carbonate and the pigment is electrostatic adsorption or takes the electrostatic adsorption as a main driving force. However, unlike aluminum hydroxide, the application and theoretical research of using calcium carbonate as an adsorbent is relatively poor, and the color and stability of calcium carbonate lake have room for further improvement, which has certain limitations in application, especially the insufficient adsorption stability limits the application in high-moisture food.
Disclosure of Invention
The invention provides a preparation method for improving the color and stability of an edible calcium carbonate lake, and solves the problems that the color and stability of the calcium carbonate lake in the prior art need to be improved and the application is limited.
The technical scheme of the invention is as follows:
a preparation method for improving the color and the stability of calcium carbonate edible color lake comprises the following steps:
s1, dissolving carbonate in water to prepare a carbonate aqueous solution;
s2, adding water-soluble anionic pigment into the carbonated aqueous solution obtained in the S1 to obtain a mixed solution;
s3, adding ethanol into the S2 mixed solution, fully mixing, and adjusting the pH value to 9-11;
s4, dissolving the calcium salt in water, adding ethanol, mixing uniformly, mixing with the solution obtained in S3, carrying out ultrasonic treatment for 1-10 minutes, and centrifuging to collect the calcium carbonate precipitate adsorbed with the pigment.
As a further technical proposal, the step S4 is followed by S5, and the calcium carbonate precipitate obtained in S4 is dried and ground to obtain the calcium carbonate-based edible color lake.
As a further technical solution, in the step S1, the carbonate is sodium carbonate or potassium carbonate.
As a further technical scheme, in the step S1, the carbonate solution has a mass concentration of 0.9% to 1.2%.
In a further aspect, in step S2, the water-soluble anionic dye is a sulfonic acid group-containing dye or a carboxyl group-containing dye.
According to a further technical scheme, the pigment containing sulfonic acid groups comprises one or more of sodium indigo disulfonate, brilliant blue, lemon yellow, sunset yellow, amaranth, new red, carmine and allura red, and the pigment containing carboxyl groups is erythrosine.
As a further technical scheme, in the step S3, ethanol accounts for 9% -11% of the total volume of the solution obtained after the ethanol is mixed with the S2 solution.
As a further technical solution, in the step S4, the calcium salt is a water-soluble calcium salt selected from calcium chloride or calcium bicarbonate.
As a further technical scheme, in the step S4, the molar ratio of the calcium salt to the carbonate is 1: 1.
As a further technical scheme, in the step S4, the ultrasonic frequency is 25-100 kHz.
The invention has the beneficial effects that:
1. the invention is based on CaCO3On the basis of the technology of producing novel color lake for matrix, ethanol is added in the preparation process of color lake to further improve the color of color lake. Compared with the prior art without ethanol, the indigo lake prepared by the new process has higher blue color value and brighter color.
2. The invention increases the use of ethanol in the preparation technology of the color lake, and compared with the prior method, the method realizes the great improvement of the color stability of the color lake by adopting the specific addition amount and the addition sequence. Compared with the prior art without ethanol, the indigo lake prepared by the new process can still keep bright blue after being stored for a long time, and the color stability of the indigo lake is greatly improved.
3. The invention adjusts the relation between calcium carbonate crystallization and adsorption through the use of ethanol, so that calcium carbonate forms a special microstructure, the combination effect between the calcium carbonate and pigment is obviously enhanced, the adsorption stability of the lake is improved, and the application range of the calcium carbonate edible lake is widened.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and 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 inventive step, are intended to be within the scope of the present invention.
Example 1
Dissolving 2.0g of sodium carbonate in 180mL of water to obtain a sodium carbonate solution; adding 50.0mg of indigo disulfonic acid sodium into a sodium carbonate solution, and fully stirring to completely dissolve the pigment to obtain a mixed solution; adding 20mL of absolute ethyl alcohol into the mixed solution, fully mixing, adding a proper amount of hydrochloric acid, and adjusting the pH value of the mixed solution to 10.5; dissolving 2.1g of calcium chloride in 22.5mL of water, adding 2.5mL of absolute ethyl alcohol, uniformly mixing, adding into a solution with the pH value of 10.5, stirring and carrying out ultrasonic treatment for 2min at the ultrasonic frequency of 40kHz, rapidly centrifuging by using a centrifugal machine, and collecting the calcium carbonate precipitate adsorbed with the pigment; the obtained pigment-adsorbed calcium carbonate precipitate is dried in an oven at 60 ℃ and then ground to obtain an edible calcium carbonate-based lake.
Example 2
Dissolving 2.0g of sodium carbonate in 180mL of water to obtain a sodium carbonate solution; adding 80.0mg of brilliant blue into a sodium carbonate solution, and fully stirring to completely dissolve the pigment to obtain a mixed solution; adding 20mL of absolute ethyl alcohol into the mixed solution, fully mixing, adding a proper amount of hydrochloric acid, and adjusting the pH value of the mixed solution to 10; dissolving 2.1g of calcium chloride in 22.5mL of water, adding 2.5mL of absolute ethyl alcohol, uniformly mixing, adding into a solution with the pH value of 10, stirring and carrying out ultrasonic treatment for 3min at the ultrasonic frequency of 40kHz, rapidly centrifuging by using a centrifuge, and collecting the calcium carbonate precipitate adsorbed with the pigment; the resulting pigment-adsorbed calcium carbonate precipitate was dried in an oven at 50 c and then ground to obtain a calcium carbonate-based edible lake.
Example 3
Dissolving 2.0g of sodium carbonate in 180mL of water to obtain a sodium carbonate solution; adding 50.0mg of indigo disulfonic acid sodium into a sodium carbonate solution, and fully stirring to completely dissolve the pigment to obtain a mixed solution; adding 20mL of absolute ethyl alcohol into the mixed solution, fully mixing, adding a proper amount of hydrochloric acid, and adjusting the pH value of the mixed solution to 10.5; dissolving 3.0g of calcium bicarbonate in 22.5mL of water, adding 2.5mL of absolute ethyl alcohol, uniformly mixing, adding into a solution with the pH value of 10.5, stirring and carrying out ultrasonic treatment for 1min at the ultrasonic frequency of 40kHz, rapidly centrifuging by using a centrifugal machine, and collecting calcium carbonate precipitate adsorbed with pigment; the obtained pigment-adsorbed calcium carbonate precipitate is dried in an oven at 60 ℃ and then ground to obtain an edible calcium carbonate-based lake.
Example 4
Dissolving 2.0g of sodium carbonate in 180mL of water to obtain a sodium carbonate solution; adding 57.0mg of lemon yellow into a sodium carbonate solution, and fully stirring to completely dissolve the pigment to obtain a mixed solution; adding 20mL of absolute ethyl alcohol into the mixed solution, fully mixing, adding a proper amount of hydrochloric acid, and adjusting the pH value of the mixed solution to 10.5; dissolving 2.1g of calcium chloride in 22.5mL of water, adding 2.5mL of absolute ethyl alcohol, uniformly mixing, adding into a solution with the pH value of 10.5, stirring and carrying out ultrasonic treatment for 3min at the ultrasonic frequency of 60kHz, rapidly centrifuging by using a centrifugal machine, and collecting the calcium carbonate precipitate adsorbed with the pigment; the obtained pigment-adsorbed calcium carbonate precipitate is dried in an oven at 80 ℃ and then ground to obtain an edible lake based on calcium carbonate.
Example 5
2.0g of sodium carbonate is dissolved in 190mL of water to obtain a sodium carbonate solution; adding 50.0mg of indigo disulfonic acid sodium into a sodium carbonate solution, and fully stirring to completely dissolve the pigment to obtain a mixed solution; adding 25mL of absolute ethyl alcohol into the mixed solution, fully mixing, adding a proper amount of hydrochloric acid, and adjusting the pH value of the mixed solution to 10; dissolving 2.1g of calcium chloride in 22.5mL of water, adding 2.5mL of absolute ethyl alcohol, uniformly mixing, adding into a solution with the pH value of 10, stirring and carrying out ultrasonic treatment for 3min at the ultrasonic frequency of 80kHz, rapidly centrifuging by using a centrifuge, and collecting the calcium carbonate precipitate adsorbed with the pigment; the obtained pigment-adsorbed calcium carbonate precipitate is dried in an oven at 60 ℃ and then ground to obtain an edible calcium carbonate-based lake.
Example 6
Dissolving 2.0g of potassium carbonate in 180mL of water to obtain a potassium carbonate solution; adding 50.0mg of indigo disulfonic acid sodium into potassium carbonate solution, and fully stirring to completely dissolve the pigment to obtain mixed solution; adding 20mL of absolute ethyl alcohol into the mixed solution, fully mixing, adding a proper amount of hydrochloric acid, and adjusting the pH value of the mixed solution to 10; dissolving 1.6g of calcium chloride in 22.5mL of water, adding 2.5mL of absolute ethyl alcohol, uniformly mixing, adding into a solution with the pH value of 10, stirring and carrying out ultrasonic treatment for 2.5min at the ultrasonic frequency of 60kHz, rapidly centrifuging by using a centrifugal machine, and collecting the calcium carbonate precipitate adsorbed with the pigment; the obtained pigment-adsorbed calcium carbonate precipitate is dried in an oven at 60 ℃ and then ground to obtain an edible calcium carbonate-based lake.
Comparative example 1
2.0g of sodium carbonate is dissolved in 200mL of water to obtain a sodium carbonate solution; adding 50.0mg of indigo disulfonic acid sodium into a sodium carbonate solution, and fully stirring to completely dissolve the pigment to obtain a mixed solution; adding a proper amount of hydrochloric acid into the mixed solution, and adjusting the pH value of the mixed solution to be 10.5; dissolving 2.1g of calcium chloride in 25mL of water, adding the calcium chloride into a solution with the pH value of 10.5, stirring and carrying out ultrasonic treatment for 2min at the ultrasonic frequency of 40kHz, rapidly centrifuging by using a centrifuge, and collecting the calcium carbonate precipitate adsorbed with the pigment; the obtained pigment-adsorbed calcium carbonate precipitate is dried in an oven at 60 ℃ and then ground to obtain an edible calcium carbonate-based lake.
Comparative example 2
Dissolving 2.0g of sodium carbonate in a mixed solution of 180mL of water and 20mL of ethanol to obtain a sodium carbonate/ethanol/water solution; adding 50.0mg of indigo disulfonic acid sodium into a sodium carbonate/ethanol/water solution, and fully stirring to completely dissolve the pigment to obtain a mixed solution; adding a proper amount of hydrochloric acid into the mixed solution, and adjusting the pH value of the mixed solution to be 10.5; dissolving 2.1g of calcium chloride in a mixed solution of 22.5mL of water and 2.5mL of ethanol, adding the solution into a solution with the pH value of 10.5, stirring and carrying out ultrasonic treatment for 2min at the ultrasonic frequency of 40kHz, rapidly centrifuging by using a centrifuge, and collecting the calcium carbonate precipitate adsorbed with the pigment; the obtained pigment-adsorbed calcium carbonate precipitate is dried in an oven at 60 ℃ and then ground to obtain an edible calcium carbonate-based lake.
Comparative example 3
2.0g of sodium carbonate is dissolved in 140mL of water to obtain a sodium carbonate solution; adding 50.0mg of indigo disulfonic acid sodium into a sodium carbonate solution, and fully stirring to completely dissolve the pigment to obtain a mixed solution; adding 60mL of absolute ethyl alcohol into the mixed solution, fully mixing, adding a proper amount of hydrochloric acid, and adjusting the pH value of the mixed solution to 10.5; dissolving 2.1g of calcium chloride in 17.5mL of water, adding 7.5mL of absolute ethyl alcohol, uniformly mixing, adding into a solution with the pH value of 10.5, stirring and carrying out ultrasonic treatment for 2min at the ultrasonic frequency of 40kHz, rapidly centrifuging by using a centrifugal machine, and collecting the calcium carbonate precipitate adsorbed with the pigment; the obtained pigment-adsorbed calcium carbonate precipitate is dried in an oven at 60 ℃ and then ground to obtain an edible calcium carbonate-based lake.
Comparative example 4
Dissolving 2.0g of sodium carbonate in 100mL of water to obtain a sodium carbonate solution; adding 50.0mg of indigo disulfonic acid sodium into a sodium carbonate solution, and fully stirring to completely dissolve the pigment to obtain a mixed solution; adding 100mL of absolute ethyl alcohol into the mixed solution, fully mixing, adding a proper amount of hydrochloric acid, and adjusting the pH value of the mixed solution to 10.5; dissolving 2.1g of calcium chloride in 12.5mL of water, adding 12.5mL of absolute ethyl alcohol, uniformly mixing, adding into a solution with the pH value of 10.5, stirring and carrying out ultrasonic treatment for 2min at the ultrasonic frequency of 40kHz, rapidly centrifuging by using a centrifugal machine, and collecting the calcium carbonate precipitate adsorbed with the pigment; the obtained pigment-adsorbed calcium carbonate precipitate is dried in an oven at 60 ℃ and then ground to obtain an edible calcium carbonate-based lake.
The detection method comprises the following steps:
pigment adsorption rate: in the preparation of the sample, 4mL of the supernatant was collected by a syringe after centrifugation and filtered through a 0.22 μm filter, and the content of sodium indigo disulfonate in the supernatant was measured by spectrophotometry of the filtrate to calculate the adsorption rate a (%) of the pigment.
Color: 150mg of the sample was weighed into a No. 0 self-sealing bag and then pressed flat to obtain a flat lake surface. The L, a and b values of the lakes obtained in the examples and comparative examples were measured using a color difference meter, respectively. Blue lakes compare b values, with lower b values indicating a darker blue shade.
Color stability of lake under light conditions: the sample prepared in the color performance detection is placed in a light incubator, the light intensity is set to 12000LX, and the light temperature is 25 ℃. Detecting the change of the lake color value b along with the time, and measuring the change delta b of the blue color value b after 48h1Delta b as a measure of the color stability of the lake1A smaller absolute value of (a) indicates a higher color stability.
Adsorption stability of pigment in lake: 200mg of the lake was weighed into a No. 0 sealed bag and then pressed flat to obtain a flat lake surface. The b values of the samples obtained in the examples and comparative examples were measured by a color difference meter and recorded as b1. The lake in the sealed bag was then transferred to 100mL artificial Saliva Simulant (SSF), magnetically stirred at 100rpm for 2min at 37 deg.C, and then placed in a 50mL centrifuge tube and centrifuged (5000rpm, 15 min)) Removing supernatant, drying the precipitate in oven to obtain new lake sample, flattening in No. 0 sealing film, detecting sample b value with color difference meter, and recording as b2. Change of b value of lake by delta b2(b2-b1) As a measure of adsorption stability, the smaller the change in b value (. DELTA.b)2Smaller absolute value) indicates higher adsorption stability.
The test results are shown in table 1.
Table 1 performance testing of example 1 and comparative lake
Example 1 is a sample prepared according to the present invention; comparative example 1 is a sample prepared according to the current calcium carbonate edible lake preparation patent; comparative example 2 was conducted to investigate the effect of the order of addition of ethanol on the lake performance; comparative examples 3 and 4 were conducted to investigate the effect of different ethanol addition amounts on the lake performance. Wherein, the ethanol addition amount of example 1 is 10% (v/v), the ethanol addition amount of comparative example 3 is 30% (v/v), and the ethanol addition amount of comparative example 4 is 50% (v/v).
As can be seen from the results of the tests in the table, in example 1, the pigment adsorption rate (A), the color (b), and the color stability (. DELTA.b) of example 1 were higher than those of comparative examples 1 and 21) Adsorption stability (. DELTA.b)2) And color after rinsing (b)2) The method realizes synchronous optimization and promotion, improves the practicability of the calcium carbonate edible color lake, and simultaneously proves that the key steps of adding the ethanol and the key steps of adding the ethanol in the color lake preparation technology, which are required to be protected by the invention, have practical effects after the sodium carbonate and the pigment are completely dissolved in water.
Example 1 compares with comparative examples 3 and 4, and comparative examples 3 and 4 only indicate the adsorption stabilityLabel (Delta b)2) And this is probably due to their significantly lower pigment adsorption rate. Example 1 other indicators include pigment adsorption (A), color (b), color stability (. DELTA.b)1) And color after rinsing (b)2) The aspect shows higher promotion. The pigment adsorption rate of example 1 is about 1.5 to 1.9 times that of comparative example 3 and comparative example 4, the color index is about 1.8 to 5.5 times that of comparative example 3 and comparative example 4, the color stability is about 1.7 to 1.8 times that of comparative example 3 and comparative example 4, and the color b after washing2About 1.7-45.6 times of that of comparative examples 3 and 4, the content of ethanol in the pigment paste is proved to have obvious influence on the color and the stability of the color lake, and meanwhile, the addition amount of ethanol in the pigment paste is a key step and has practical effect.
Table 1 presents only the results of the study of example 1, and the tests described above were also performed for other examples, which are similar to the results of example 1 and therefore omitted, and which demonstrate the general applicability of the solution claimed in this patent.
Experimental results show that the preparation method for improving the color and stability of the edible calcium carbonate lake, provided by the invention, keeps the safety advantage of the existing preparation technology of the edible calcium carbonate lake on one hand, and greatly improves the stability and color performance of the edible calcium carbonate lake on the other hand, and the technology is simple and easy to implement, convenient to operate and low in cost, widens the application range of the edible calcium carbonate lake and has great market value.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent substitutions, improvements, etc. within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method for improving the color and the stability of an edible calcium carbonate lake is characterized by comprising the following steps:
s1, dissolving carbonate in water to prepare a carbonate aqueous solution;
s2, adding water-soluble anionic pigment into the carbonated aqueous solution obtained in the S1 to obtain a mixed solution;
s3, adding ethanol into the S2 mixed solution, fully mixing, and adjusting the pH value to 9-11;
s4, dissolving the calcium salt in water, adding ethanol, mixing uniformly, mixing with the solution obtained in S3, carrying out ultrasonic treatment for 1-10 minutes, and centrifuging to collect the calcium carbonate precipitate adsorbed with the pigment.
2. The method of claim 1, further comprising step S5 after step S4 of drying and grinding the calcium carbonate precipitate obtained in step S4 to obtain a calcium carbonate-based edible lake.
3. The method as claimed in claim 1, wherein the carbonate is sodium carbonate or potassium carbonate in step S1.
4. The method as claimed in claim 1, wherein the carbonate solution is added in a concentration of 0.9-1.2% by mass in step S1.
5. The method as claimed in claim 1, wherein the water-soluble anionic pigment is a pigment containing sulfonic acid group or a pigment containing carboxylic group in step S2.
6. The method according to claim 5, wherein the pigment containing sulfonic acid groups comprises one or more of sodium indigo disulfonate, brilliant blue, lemon yellow, sunset yellow, amaranth, new red, carmine, and allura red, and the pigment containing carboxylic groups is erythrosine.
7. The method of claim 1, wherein in step S3, ethanol is 9% to 11% of the total volume of the solution obtained by mixing the solution of S2 with the calcium carbonate.
8. The method as claimed in claim 1, wherein the calcium salt is water-soluble calcium salt selected from calcium chloride and calcium bicarbonate in step S4.
9. The method of claim 1, wherein the calcium carbonate is added in a molar ratio of calcium salt to carbonate salt of 1:1 in step S4.
10. The method as claimed in claim 1, wherein the ultrasonic frequency used in step S4 is 25-100 kHz.
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| CN108795096A (en) * | 2018-05-18 | 2018-11-13 | 山东中惠生物科技股份有限公司 | Natural plants color lake and preparation method thereof |
| CN110183873A (en) * | 2019-06-14 | 2019-08-30 | 北京工商大学 | A kind of preparation method of the edible color lake based on calcium carbonate |
| CN110194906A (en) * | 2019-06-17 | 2019-09-03 | 广州素旺生物科技有限公司 | A kind of food grade shellac mixed liquor and preparation method thereof |
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| CN1044671A (en) * | 1990-02-28 | 1990-08-15 | 孙博南 | Manufacturing method of fluorescent ink |
| CN108795096A (en) * | 2018-05-18 | 2018-11-13 | 山东中惠生物科技股份有限公司 | Natural plants color lake and preparation method thereof |
| CN110183873A (en) * | 2019-06-14 | 2019-08-30 | 北京工商大学 | A kind of preparation method of the edible color lake based on calcium carbonate |
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