CN113683902B - Method for preparing caramel pigment, caramel pigment and application thereof - Google Patents
Method for preparing caramel pigment, caramel pigment and application thereof Download PDFInfo
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- CN113683902B CN113683902B CN202111149835.XA CN202111149835A CN113683902B CN 113683902 B CN113683902 B CN 113683902B CN 202111149835 A CN202111149835 A CN 202111149835A CN 113683902 B CN113683902 B CN 113683902B
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- 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
- C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
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- 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
- A23L5/43—Addition of dyes or pigments, e.g. in combination with optical brighteners using naturally occurring organic dyes or pigments, their artificial duplicates or their derivatives
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- 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
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0096—Purification; Precipitation; Filtration
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Abstract
The invention belongs to the field of food additives, and particularly relates to a method for preparing caramel pigment, which comprises the following steps: mixing sugar solution with acid auxiliary agent, reacting under 0.03-0.5 MPa, reacting at a temperature higher than 100 ℃ but not higher than 200 ℃ to obtain a reaction product; adjusting the pH value of the reaction product to 3.5-7.5, and cooling to obtain caramel pigment; the invention also relates to the prepared caramel pigment and application thereof. The caramel pigment prepared by the method has the advantages of high viscosity, long resinification time, good stability and long shelf life.
Description
Technical Field
The invention belongs to the field of food additives, and particularly relates to a method for preparing caramel pigment, and also relates to the prepared caramel pigment and application thereof in foods.
Background
Caramel Color (Caramel Color) is one of the oldest and most widely used food colors to enhance naturally occurring colors, correct natural changes in Color, and protect colors that may be lost by photodegradation during food processing and storage. The caramel pigment has the characteristics of good water solubility, coloring capability, stability, safety and the like, so the caramel pigment becomes the edible pigment with the most wide application and the largest sales volume worldwide, and occupies more than 90 percent of the use amount of the edible pigment in developed European and American countries and China.
Important parameters of the caramel color include, but are not limited to, viscosity, hue index, resinification, density, alcohol solubility, salt stability, and beer testing. The viscosity is an important parameter of the caramel color, generally reflects the quality and the shelf life of the caramel color, and directly influences the transportation, stirring, mixing and the like of the caramel color. In practical application, too high or too low viscosity can affect the quality of caramel pigment products; the viscosity is too high, the pumping transportation is not facilitated, the resin is easy to be made, and the stability is poor; the viscosity is too low, the resinification is slow, the shelf life is long, but the effect of improving the state and wall-hanging property of the liquid seasoning is general. The caramel pigment prepared by the common method has the characteristics of high red yellow pigment index, ruddy color, high safety and the like, is more in line with the consumption concepts and environments of safety, green, natural and health, and has wide application in alcohol, flavouring (particularly Asian market) and baking industries. The caramel pigment is added into liquid seasonings such as soy sauce, so that the color intensity is improved, the batch-to-batch variation is reduced, the color adhesion of meat and noodles is improved, and the mouthfeel of the product is improved, therefore, the common caramel pigment for soy sauce needs to keep higher viscosity and higher stability, but the common caramel pigment is not available in the prior art.
Therefore, there is a need to obtain a common caramel color with high viscosity, good stability and long shelf life.
Disclosure of Invention
The invention aims to provide a method for preparing caramel pigment, which has the advantages of high viscosity, long resinification time, good stability and long shelf life; the invention also aims to provide the caramel pigment and the application thereof.
To achieve the above object, a first aspect of the present invention relates to a method for preparing caramel color, comprising the steps of:
(1) Mixing sugar solution with acid auxiliary agent, reacting under 0.03-0.5 MPa, the reaction temperature is higher than 100 ℃ but not higher than 200 ℃ (preferably 110-180 ℃, such as 130 ℃ and 150 ℃ and 180 ℃) to obtain a reaction product;
(2) Adjusting the pH value of the reaction product to 3.5-7.5 (such as 4.0, 5.0, 6.0, 6.5, 7.0 and 7.2), and cooling to obtain caramel pigment;
the cooling procedure comprises the following nine stages in sequence:
stage (1): reducing the reaction temperature to 96 ℃ -100 ℃ (e.g. 98 ℃ and 100 ℃) at a rate of 0.2-0.8 ℃/min (e.g. 0.5 ℃/min, 0.6 ℃/min);
stage (2): maintaining at 96-100deg.C (e.g., 98deg.C, 100deg.C) for 5-15 min (e.g., 10 min);
stage (3): reducing the temperature from 96 ℃ -100 ℃ (e.g. 98 ℃ and 100 ℃) to 86 ℃ -94 ℃ (e.g. 88 ℃, 90 ℃ and 92 ℃) at a rate of 0.2-0.8 ℃/min (e.g. 0.5 ℃/min and 0.6 ℃/min);
stage (4): maintaining at 86-94 deg.c (e.g. 88 deg.c, 90 deg.c, 92 deg.c) for 5-15 min (e.g. 10 min);
stage (5): reducing the temperature from 86 ℃ to 94 ℃ (e.g. 88 ℃, 90 ℃ and 92 ℃) to 77 ℃ to 84 ℃ (e.g. 78 ℃, 80 ℃ and 82 ℃) at a rate of 0.1 to 0.6 ℃/min (e.g. 0.3 ℃/min, 0.4 ℃/min);
stage (6): maintaining at 77-84 deg.c, e.g. 78 deg.c, 80 deg.c, 82 deg.c, for 5-15 min, e.g. 10 min;
stage (7): reducing the temperature from 77 ℃ to 84 ℃ (e.g. 78 ℃, 80 ℃, 82 ℃) to 65 ℃ to 75 ℃ (e.g. 68 ℃, 70 ℃, 72 ℃) at a rate of 0.05 to 0.2 ℃/min (e.g. 0.1 ℃/min, 0.15 ℃/min);
stage (8): maintaining at 65-75deg.C (e.g., 68deg.C, 70deg.C, 72deg.C) for 5-15 min (e.g., 10 min);
stage (9): rapidly cooling from 65 ℃ to 75 ℃ (e.g. 68 ℃, 70 ℃, 72 ℃) to below 63 ℃ (e.g. below 60 ℃).
In any embodiment of the first aspect of the present invention, in step (1), the reaction is carried out under a condition of 0.05 to 0.3MPa (preferably 0.05 to 0.2 MPa).
In any embodiment of the first aspect of the invention, in step (1), the reaction is continued for 30 to 200 minutes, preferably 30 to 180 minutes, for example 80 minutes, 100 minutes, 150 minutes, 180 minutes.
In any embodiment of the first aspect of the present invention, in step (1), the reaction is carried out under stirring conditions at a stirring speed of 20 to 200r/min, preferably 20 to 100r/min, for example 30r/min, 50r/min, 70r/min.
In any embodiment of the first aspect of the present invention, in step (2), cooling is performed under a condition of 0 MPa.
In any embodiment of the first aspect of the present invention, in step (2), the pH of the reaction product is adjusted using an alkaline reagent.
In any embodiment of the first aspect of the present invention, the alkaline agent is selected from the group consisting of aqueous solutions of one or more of sodium hydroxide, potassium hydroxide, sodium bicarbonate, calcium hydroxide, sodium carbonate, and potassium carbonate.
In any embodiment of the first aspect of the invention, in step (1), the weight of the acidic auxiliary agent is 0.1% to 1%, for example 0.2%, 0.22%, 0.248%, 0.25%, 0.37%, 0.5%, 0.561%, 0.7% of the weight of solids in the sugar solution.
In any embodiment of the first aspect of the present invention, in step (1), the sugar solution is selected from the group consisting of aqueous solutions of one or more of corn syrup, sucrose, glucose, fructose, invert sugar, fructose syrup, maltose syrup, and starch hydrolysate.
In any embodiment of the first aspect of the present invention, in step (1), the sugar solution has a solids content of 40% to 90%, preferably 60% to 90%, for example 70% to 80% by weight.
In any embodiment of the first aspect of the invention, in step (1), the DE value of the sugar solution is 40% to 80%, for example 50% to 70%.
In any embodiment of the first aspect of the present invention, in step (1), the acidic auxiliary is selected from an aqueous solution of one or more of sulfuric acid, hydrochloric acid, nitric acid, citric acid, tartaric acid, lactic acid and acetic acid.
In any embodiment of the first aspect of the present invention, in step (1), the concentration of the acidic auxiliary agent is 10wt% to 30wt%, for example 15wt%, 20wt%, 25wt%.
In any embodiment of the first aspect of the present invention, in step (2), cooling, filtering, and collecting filtrate, namely caramel color.
In any embodiment of the first aspect of the present invention, the caramel color is a normal process caramel color.
The second aspect of the invention relates to a caramel color obtainable by the process according to the first aspect of the invention.
In any of the embodiments of the second aspect of the present invention, the viscosity of the caramel color is 10000 to 23000cP, preferably 10000 to 20000cP, more preferably 12000 to 19000cP, as measured at 25℃using a viscometer.
In any of the embodiments of the second aspect of the present invention, the resinification time of the caramel color is 22 hours or more, preferably 22 to 50 hours, more preferably 22 to 40 hours or 25 to 40 hours.
In any embodiment of the second aspect of the invention, the method for determining the resinification time of the caramel color comprises: and (3) slightly sealing the sample in a glass tube, placing the glass tube in an oven at about 100 ℃ to start timing, keeping the temperature of the oven at about 100 ℃ until the sample is observed to have no fluidity, and ending timing to obtain the resinification time.
A third aspect of the invention relates to the use of the caramel color of the second aspect of the invention in food products.
In the present invention, unless otherwise specified, wherein:
the term "solids of the sugar solution" refers to the dry matter of the sugar solution after removal of the moisture;
the term "invert sugar" refers to a mixture of glucose and fructose in equivalent amounts obtained after the action of sucrose with dilute acid or an enzyme;
the term "DE value" is an abbreviation for glucose equivalent english Dextrose Equivalent, referring to the percentage of reducing sugar (in terms of glucose) to the solids of the sugar solution;
the term "starch hydrolysate" refers to the products of starch hydrolysis, such as sugar alcohols, dextrins, starch sugars, etc., wherein starch sugars include maltose, oligosaccharides, etc.
The invention has the beneficial effects that:
the caramel pigment prepared by the method has the advantages of high viscosity, long resinification time, good stability and long shelf life, and realizes the controllable adjustment of the rheological behavior of the caramel pigment.
Drawings
In order that the invention may be more readily understood, a more particular description of the invention will be rendered by reference to specific embodiments thereof that are illustrated in the appended drawings, in which
FIG. 1 is a flow chart of the process for preparing caramel color of examples 1-3.
Detailed Description
Embodiments of the present invention will now be described more fully hereinafter with reference to the accompanying examples, in which it is shown, however, that the examples are shown, and in which the invention is practiced. The following description of at least one exemplary embodiment is merely exemplary in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
As shown in fig. 1, a high-pressure reaction kettle with the volume of 25L is selected, 15kg of fructose syrup with the DE value of 50-70% and the solid content of 70-80% is taken and metered into the reaction kettle, and is stirred uniformly for standby; 28.68g of citric acid solution with the concentration of 30wt percent (2.48 per mill of the weight of solid matters in the raw material sugar) is added into a high-pressure reaction kettle, and stirred to prepare a reaction solution; the reaction solution was reacted under the following conditions: the reaction temperature is 130 ℃, the positive pressure is 0.05-0.20MPa, the reaction time is 180min, and the rotation speed of the stirrer is 50r/min; after the reaction was completed, the pH of the reaction product was adjusted to 6.5 using a 20wt% aqueous sodium hydroxide solution, and then cooled under 0MPa according to the following procedure:
(1) reducing the reaction temperature from 130 ℃ to 100 ℃ at a cooling rate of 0.5 ℃/min;
(2) maintaining at 100deg.C for 10 min;
(3) cooling from 100 ℃ to 90 ℃ at a cooling rate of 0.5 ℃/min;
(4) maintaining at 90 ℃ for 10 minutes;
(5) cooling from 90 ℃ to 80 ℃ at a cooling rate of 0.3 ℃/min;
(6) maintaining at 80 ℃ for 10 minutes;
(7) cooling from 80 ℃ to 70 ℃ at a cooling rate of 0.15 ℃/min;
(8) maintaining at 70 ℃ for 10 minutes;
(9) rapidly cooling from 70 ℃ to below 60 ℃;
and after the process is finished, filtering to obtain the caramel pigment liquid product 1 of the common method.
Example 2
As shown in fig. 1, a high-pressure reaction kettle with the volume of 25L is selected, and glucose-fructose syrup with the 15kgDE value of 50-70% and the solid content of 70-80% is metered into the reaction kettle and stirred uniformly for standby; 28.68g of citric acid solution with the concentration of 30wt percent (2.48 per mill of the weight of solid matters in the raw material sugar) is added into a high-pressure reaction kettle, and stirred to prepare a reaction solution; the reaction solution was reacted under the following conditions: the reaction temperature is 150 ℃, the positive pressure is 0.05-0.20MPa, the reaction time is 150min, and the rotation speed of a stirrer is 50r/min; after the reaction was completed, the pH of the reaction product was adjusted to 7.2 using a 20wt% aqueous sodium hydroxide solution; then cooling under 0MPa according to the procedure in example 1, and filtering after the cooling, thus obtaining the caramel pigment liquid product 2 of the common method.
Example 3
As shown in fig. 1, a high-pressure reaction kettle with the volume of 25L is selected, and glucose-fructose syrup with the 15kgDE value of 50-70% and the solid content of 70-80% is metered into the reaction kettle and stirred uniformly for standby; 28.68g of citric acid solution with the concentration of 30wt percent (2.48 per mill of the weight of solid matters in the raw material sugar) is added into a high-pressure reaction kettle, and stirred to prepare a reaction solution; the reaction solution was reacted under the following conditions: the reaction temperature is 180 ℃, the positive pressure is 0.05-0.20MPa, the reaction time is 100min, and the rotation speed of a stirrer is 50r/min; after the reaction was completed, the pH of the reaction product was adjusted to 4.0 using a 20wt% aqueous sodium hydroxide solution; then cooling under 0MPa according to the procedure in example 1, and filtering after the cooling, so as to obtain the caramel pigment liquid product 3.
Comparative example 1 reaction was not pressurized, and reaction temperature and time were not controlled cooperatively
The preparation of the reaction solution was the same as in example 2; the reaction solution was reacted under the following conditions: the reaction temperature is 180 ℃, the pressure is 0MPa, the reaction time is 150min, and the rotation speed of a stirrer is 50r/min; the procedure after the completion of the reaction was the same as in example 2 to obtain a liquid product A of caramel color of the ordinary method.
Comparative example 2 without adjusting the pH of the reaction product
Omitting the operation of adjusting the pH value after the reaction is completed, directly cooling the reaction product under the condition of 0MPa according to the procedure in the example 1, and obtaining the caramel pigment liquid product B by the common method by the rest operation as in the example 2.
Comparative example 3 does not employ a temperature reduction procedure
(1) The reaction product was adjusted to pH 7.2, immediately cooled to below 60℃under 0MPa, and the remainder was the same as in example 2 to give a liquid product C1 of caramel color of the conventional method;
(2) And (3) regulating the pH value of the reaction product to 7.2, slowly cooling to below 60 ℃ at the speed of 0.15-0.5 ℃/min, and obtaining a liquid product C2 of the caramel pigment by the common method by the rest of the operations in the example 2.
Comparative example 4 pH adjustment after cooling
The preparation and reaction process of the reaction solution are the same as in example 2; after the reaction, the reaction product was cooled under 0MPa according to the procedure in example 1, and then the pH of the reaction product was adjusted to 7.2 with a 20wt% aqueous sodium hydroxide solution, and filtered to obtain a liquid product D of caramel color of the general method.
Test case
Color ratio: measured according to the method specified in annex A of GB1886.64-2015 food safety national Standard food additive caramel color;
viscosity: the temperature was 25℃as measured using a DV-ll+Pro model viscometer from BROOKFIELD, U.S.A.;
density: measuring by a density balance method;
resinifying time: and (3) slightly sealing the sample in a glass tube, placing the glass tube in a high-temperature oven at about 100 ℃ to start timing, keeping the temperature of the oven at about 100 ℃ until no fluidity of the sample is observed, and ending timing to obtain the resinification time.
The parameters of the caramel color liquid products 1-3 and the caramel color liquid products A-B, C1, C2 and D were measured according to the above methods, and the results are shown in Table 1. It is worth to say that the viscosity of different samples at different temperatures is greatly different, and the temperature control is needed during measurement.
TABLE 1
As can be seen from Table 1, the ordinary caramel color products of the present invention have a higher viscosity than the ordinary caramel color products B, C, C2, D; compared with the caramel pigment products B, C, C2 and D, the caramel pigment product has longer resinification time, better stability and longer shelf life; although the viscosity of the caramel pigment product A of the common method is larger than that of the caramel pigment product of the invention, the too high viscosity leads to too short resinification time, poor stability and short service life of the caramel pigment product A of the common method; in addition, the color ratio of the caramel pigment product B by the common method is low; therefore, the caramel pigment product of the common method has higher viscosity, longer resinification time, good stability and long shelf life.
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. While still being apparent from variations or modifications that may be made by those skilled in the art are within the scope of the invention.
Claims (13)
1. A method of preparing caramel color comprising the steps of:
(1) Mixing sugar solution with acid auxiliary agent, reacting under 0.03-0.5 MPa, reacting at a temperature higher than 100 ℃ but not higher than 200 ℃ to obtain a reaction product;
(2) Adjusting the pH value of the reaction product to 3.5-7.5, and cooling to obtain caramel pigment;
the cooling procedure comprises the following nine stages in sequence:
stage (1): the reaction temperature is reduced to 96 ℃ to 100 ℃ at the speed of 0.2 to 0.8 ℃/min;
stage (2): maintaining at 96-100 deg.c for 5-15 min;
stage (3): reducing the temperature from 96 ℃ to 100 ℃ to 86 ℃ to 94 ℃ at the speed of 0.2 to 0.8 ℃/min;
stage (4): maintaining at 86-94 deg.c for 5-15 min;
stage (5): reducing the temperature from 86 ℃ to 94 ℃ to 77 ℃ to 84 ℃ at the speed of 0.1 to 0.6 ℃/min;
stage (6): maintaining at 77-84 deg.c for 5-15 min;
stage (7): reducing the temperature from 77 ℃ to 84 ℃ to 65 ℃ to 75 ℃ at the speed of 0.05 to 0.2 ℃/min;
stage (8): maintaining at 65-75 deg.c for 5-15 min;
stage (9): rapidly cooling from 65-75 ℃ to below 63 ℃.
2. The process according to claim 1, wherein in step (1), the reaction is carried out under a pressure of 0.05 to 0.3 MPa.
3. The method according to claim 1, wherein in the step (1), the reaction is continued for 30 to 200 minutes.
4. The method according to claim 1, wherein in the step (1), the reaction is carried out under stirring conditions at a stirring speed of 20 to 200r/min.
5. The method of claim 1, wherein in step (2), cooling is performed under 0 MPa.
6. The method of claim 1, wherein in step (2), the pH of the reaction product is adjusted using an alkaline reagent.
7. The method according to claim 6, wherein in the step (2), the alkaline agent is selected from the group consisting of aqueous solutions of one or more of sodium hydroxide, potassium hydroxide, sodium bicarbonate, calcium hydroxide, sodium carbonate and potassium carbonate.
8. The method of claim 1, wherein in step (1), the weight of the acidic auxiliary agent is 0.1% to 1% of the weight of solids in the sugar solution.
9. The method according to any one of claims 1 to 8, characterized by one or more of the following:
A. in the step (1), the sugar solution is selected from one or more aqueous solutions of corn syrup, sucrose, glucose, fructose, invert sugar, fructose syrup, maltose syrup and starch hydrolysate;
B. in the step (1), the solid content of the sugar solution is 40-90% by weight;
C. in the step (1), the DE value of the sugar solution is 40-80%;
D. in the step (1), the acid auxiliary agent is selected from one or more aqueous solutions of sulfuric acid, hydrochloric acid, nitric acid, citric acid, tartaric acid, lactic acid and acetic acid;
E. in the step (1), the concentration of the acid auxiliary agent is 10-30wt%;
F. in the step (2), cooling and filtering are carried out, and the filtered liquid is collected to obtain caramel pigment;
G. the caramel pigment is common caramel pigment.
10. A caramel color produced by the method of any one of claims 1 to 9.
11. The caramel color of claim 10, wherein the caramel color has a viscosity of 10000 to 23000cP as measured by a viscometer at 25 ℃.
12. The caramel color of claim 10, wherein the caramel color has a resinification time of 22 hours or more.
13. Use of the caramel color of any one of claims 10 to 12 in food products.
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