High-solubility compound haematochrome and preparation method thereof

Abstract

The invention discloses a high-solubility compound haematochrome and a preparation method thereof, and relates to the field of food additives. The preparation method of the high-solubility compound haematochrome comprises the following steps: S1, uniformly stirring 9.5 wt%-15.5 wt% of a natural pigment, 8 wt%-12 wt% of an emulsifier, 18 wt%-25 wt% of maltodextrin and the balance of a monascus red concentrated solution to obtain a premix; s2, performing homogenization treatment on the premix for the first time to obtain an emulsion; s3, adding a wall material solution into the emulsion, uniformly mixing, and carrying out second homogenization treatment to obtain an embedded modified emulsion; and S4, carrying out spray drying granulation on the embedded modified emulsion. The maximum absorption peak of the high-solubility compound haematochrome is in the range of 505-510 nm, and the high-solubility compound haematochrome is amaranth in appearance, not prone to agglomeration in water and high in dissolution speed.

Description

Technical Field

[0001] This application relates to the field of food additives, and particularly to a highly soluble compound red pigment and a preparation method thereof. Background Art

[0002] Monascus red pigment products are currently widely used in various food processing industries due to their good safety and stability. However, Monascus red pigment is difficult to disperse sufficiently in water, which easily leads to uneven color in the finally processed food, and is not conducive to improving the quality stability and aesthetics of the food.

[0003] There are mainly two categories of existing methods for improving the solubility of Monascus red pigment. The first category is physical modification technology, which changes the particle size of Monascus red pigment by ultrafine grinding to improve its water solubility. The second category is to introduce hydrophilic groups into the molecular structure of Monascus red pigment or use surfactants to enhance its water solubility. Although these two methods can improve the solubility of Monascus red pigment to a certain extent, there are still problems of easy agglomeration.

[0004] In addition, Monascus red pigment is a single pigment, and the maximum absorption peak of the sample is between 495 nm and 505 nm (excluding 505 nm), and the appearance is red. Among them, the test method for the maximum absorption peak of the sample mentioned in this application is as follows: Dissolve the Monascus red sample in 100 ml of ethanol aqueous solution (1+1) to obtain a sample solution with a color value range of 0.4 - 0.8 u / ml, scan the sample solution under visible light, and record the maximum absorption peak. However, some customers require Monascus red pigment with a purplish-red appearance (the maximum absorption peak of the sample is between 505 - 510 nm). Therefore, how to obtain a compound Monascus red pigment with a purplish-red appearance, good solubility, and beneficial to improving the color uniformity of the product has important research value. Summary of the Invention

[0005] In order to make the appearance of Monascus red pigment purplish-red and have good solubility to improve the color uniformity of the product, this application provides a highly soluble compound red pigment and a preparation method thereof.

[0006] A preparation method of a highly soluble compound red pigment includes the following steps: S1. Premixing: Stir 9.5 wt% - 15.5 wt% natural pigment, 8 wt% - 12 wt% emulsifier, 18 wt% - 25 wt% maltodextrin, and the balance of Monascus red concentrate evenly to obtain a premix; S2. First homogenization: Perform the first homogenization treatment on the premix to obtain an emulsion; S3. Secondary homogenization: Add the wall material solution to the emulsion. After mixing evenly, perform the second homogenization treatment to obtain the embedded and modified emulsion; the wall material solution is a mixed solution of colloid, antioxidant, and water, and the weight ratio of the colloid, antioxidant, and water is (0.65 - 0.95):(0.85 - 1.8):(55 - 60); S4. Spray drying: Perform spray drying granulation on the embedded and modified emulsion to obtain the highly soluble compound pigment.

[0007] In this application, natural pigments are used to adjust the color appearance of monascus red, shift the absorption peak of the compound pigment to 505 - 510 nm, and achieve the purple - red appearance of the compound pigment to meet the specific needs of customers; emulsifiers help form a stable emulsion, prevent pigment particles from aggregating, and improve solubility; Maltodextrin, as a filler, plays a role in adjusting the color value of the product, and at the same time provides a certain viscosity, which helps the formation of the emulsion and improves the stability of the emulsion. In the wall material solution, the colloid, as a film - forming substance, is used to embed the core material mainly composed of monascus pigment, improve the agglomeration problem during the dissolution of the compound pigment, and help improve the solubility of the compound pigment. Antioxidants are mainly used to improve the problem of oxidative deterioration of the compound pigment during storage or use.

[0008] Among them, in this application, a specific proportion of natural pigments, emulsifiers, maltodextrin, and monascus red concentrate are stirred evenly and then subjected to the first homogenization treatment to form a stable emulsion. Then, the wall material solution is added to the emulsion. After the second homogenization treatment, the wall material solution wraps around the outer surface of the fine particles in the emulsion to form a stable embedded and modified emulsion. Finally, the embedded and modified emulsion is spray - dried to form granular compound pigment. The compound pigment has a micro - capsule structure, appears purple - red in appearance, the maximum absorption peak of the sample is at 505 - 510 nm, is not prone to agglomeration problems during the process of dissolving in water, has a high dissolution efficiency, and the wall material of the compound pigment can block air. Under the barrier of the wall material, the compound pigment is not prone to photo - oxidation and thermal oxidation, and has good photo - stability and thermal stability.

[0009] In some specific embodiments, in S1, the natural pigments include E100 beet red and E20 capsicum red, and the weight ratio of E100 beet red to E20 capsicum red is (1 - 2.4):(0.5 - 1).

[0010] In some specific embodiments, in S1, the emulsifier uses a composition of soy lecithin and glycerol monostearate, and the weight ratio of soy lecithin to glycerol monostearate is (0.8 - 1.2):(1 - 1.5).

[0011] In this application, the emulsifier uses a composition of soybean phospholipid and glycerol monostearate in a specific ratio. The combination of the two is beneficial to improving the stability of the emulsion, reducing the aggregation of particles in the emulsion, increasing the weight percentage of the compound red pigment in the range of 80 - 120 mesh, and increasing the embedding rate of the compound red pigment, thereby improving the dissolution efficiency of the compound red pigment in water and reducing the dust problem at the same time.

[0012] In some specific embodiments, both the first homogenization treatment in S2 and the second homogenization treatment in S3 are carried out at 0.8 MPa - 1.0 MPa.

[0013] In this application, the aggregation force between the original particles is effectively broken through two homogenization treatments, which is beneficial to achieving uniform dispersion of various substances, increasing the weight percentage of the compound red pigment in the range of 80 - 120 mesh, and increasing the embedding rate of the compound red pigment, further improving the dissolution efficiency of the compound red pigment in water and reducing the dust problem at the same time.

[0014] In some specific embodiments, the colloid uses at least one of xanthan gum, carrageenan, guar gum, arabic gum, gelatin, water-soluble cellulose, and water-soluble chitosan.

[0015] In some specific embodiments, the antioxidant uses at least one of tea polyphenols, sodium erythorbate, and vitamin E.

[0016] In some specific embodiments, in S4, the mass ratio of the emulsion to the wall material solution is 1:(2.5 - 3.5).

[0017] In this application, the mass ratio of the emulsion to the wall material solution is controlled to be 1:(2.5 - 3.5), which is beneficial to increasing the embedding rate of the compound red pigment and further improving the dissolution efficiency of the compound red pigment in water.

[0018] In some specific embodiments, in S4, during the spray drying granulation process, the inlet air temperature is 190 - 220 °C and the outlet air temperature ≥ 95 °C.

[0019] In the second aspect, this application provides a highly soluble compound red pigment, which is prepared by the preparation method of a soluble compound red pigment described in any one of the above.

[0020] To sum up, this application includes at least the following beneficial technical effects: 1. Different from the common monascus red pigment whose maximum absorption peak of the sample is between 495 nm and 505 nm (excluding 505 nm), the maximum absorption peak of the sample of the highly soluble compound red pigment of this application is at 505 -  510 nm, presenting a purplish red appearance, not easily agglomerating in water, and having a fast dissolution rate. At the same time, under the barrier effect of the wall material, this compound red pigment is not prone to photooxidation and thermal oxidation, and has good photo - stability and thermal stability.

[0021] 2. Through the cooperation of a specific emulsifier and two - stage homogenization, this application can increase the weight ratio of the compound red pigment with a particle size in the range of 80 - 120 mesh, and improve the embedding rate of the compound red pigment, thereby improving the dissolution efficiency of the compound red pigment in water and reducing the problem of dusting at the same time. Brief Description of the Drawings

[0022] Figure 1 is a schematic flow chart of the preparation method of the highly soluble compound red pigment of this application.

[0023] Description of the Reference Numerals in the Drawings: S1, premixing; S2, primary homogenization; S3, secondary homogenization; S4, spray drying. Detailed Embodiments

[0024] The following further illustrates this application with specific experiments. Among them, the monascus red concentrated solution used in this application is prepared by the following method: (1) Inoculate the monascus mold strain into the basal medium, control the temperature at 35 °C, and shake - flask culture for 6 days; among them, the basal medium includes 10 g of rice flour, 2 g of corn steep liquor dry powder, 1 g of glucose, 10 g of peptone, 15 g of sodium nitrate, 0.2 g of magnesium sulfate, 0.15 g of potassium dihydrogen sulfate, and 61.65 g of water, and adjust the pH to 7.0; the monascus mold strain is any one of the purpureus monascus mold strains with the numbers CGMCC No.3.15548, CGMCC No.3.15547, CGMCC No.3.15546, CGMCC No.3.898, and CGMCC No.3.896 purchased from the Institute of Microbiology, Chinese Academy of Sciences. In each example of this application, the purpureus monascus mold strain with the number CGMCC No.3.1554 is taken as an example; (2) After the colonies in step S1 are mature, centrifuge to separate and take the solid residue, add 4 times the volume of alcohol with a concentration of 95%, stir at a stirring speed of 100 r / min for 10 h, then separate the solid and liquid to take the liquid, and concentrate it at 50 °C by a low - temperature vacuum concentrator to obtain the monascus red concentrated solution. Examples

[0025]

Example 1

[0026]

Example 2

[0027]

Example 3

[0028] Comparative example

Comparative Example 1

Example 1

[0029]

Comparative Example 2

Example 1

[0030] The treatment step of S3 in this comparative example is as follows: The material after the first homogenization is directly subjected to the second homogenization treatment, the pressure is 0.8 MPa and the time is 30 min.

[0031]

Comparative Example 3

[0032] Performance detection test (1) Determination of the maximum absorption peak: Take appropriate amounts of the samples prepared in each example and comparative example, dissolve them in 100 ml of ethanol aqueous solution (1+1) to obtain a sample solution with a color value range of 0.4-0.8 u / ml. Scan the sample solution under visible light, record the maximum absorption peak, and record the appearance of the sample.

[0033] (2) Dissolution performance test: 1. Test method 1 (static dissolution): Accurately weigh 10 g of the compound red pigment sample, slowly pour it into a 250 ml graduated cylinder containing 100 mL of distilled water at 25°C, and keep it in a natural sedimentation state. Calculate the time required for the sample to completely sink to the bottom from the moment it touches the water surface.

[0034] 2. Test method 2 (dynamic dissolution): Accurately weigh 20 g of the compound red pigment sample and add it to 100 mL of distilled water at 25°C. Immediately turn on the magnetic stirrer and adjust the rotation speed to 350 rpm. Start timing and record the time required for the sample to completely dissolve in water.

[0035] (3) Particle size distribution test: Randomly take 100 g of the compound red pigment powder from each example and comparative example, and then pass it through 80-mesh, 120-mesh, 150-mesh, and 200-mesh vibrating sieves in sequence. Calculate the weight percentage of the compound red pigment powder in different particle size ranges.

[0036] Table 1 Comparison of the maximum absorption peak wavelength and appearance of each compound red pigment sample Table 2 Comparison of the dissolution time of each compound red pigment sample Table 3 Comparison of the powder particle size of each compound red pigment sample Combined with the content recorded in Table 1, it can be seen that the maximum absorption peak wavelengths of the compound red pigment samples prepared in Examples 1-3 of the present application are concentrated in the range of 508-510 nm, and the appearance is uniform purple-red powder; while the maximum absorption peak wavelengths of the red pigment samples prepared in Comparative Examples 1-3 are lower than those of the examples, and the powder appearance is also duller and less vivid than that of the examples. Thus, it can be seen that after adopting the microcapsule embedding technology, the core components of the compound red pigment are protected to a certain extent, reducing the interference caused by external environmental factors (such as temperature, light, air oxidation, etc.).

[0037] It can be seen from the content recorded in Table 2 that for the compound red pigment samples prepared in Examples 1-3 of the present application, hydrophilic wall materials can accelerate water penetration and shorten the wetting time, thus significantly improving the dissolution time of the compound red pigment in water. In Comparative Examples 1-3, omitting the primary homogenization step or not adding the wall material solution in the secondary homogenization step, or omitting both the primary and secondary homogenization steps, are all likely to cause a decrease in the solubility of the compound red pigment, which is caused by a decrease in the embedding rate of the compound red pigment or affected by the particle size of the compound red pigment.

[0038] It can be seen from the content recorded in Table 3 that in the compound red pigment samples prepared in Examples 1-3 of the present application, the weight percentage of the compound red pigment with a particle size range of 80-120 mesh is > 85%, while in Comparative Examples 1-3, the weight percentage of the compound red pigment with a particle size range of 80-120 mesh is only 74.65%-80.04%, indicating that the compound red pigment in Examples 1-3 is more concentrated in the range of 80-120 mesh and has better particle uniformity. Secondly, in the compound red pigment of Examples 1-3, the weight percentage of the compound red pigment with a particle size ≥ 80 mesh is < 3% (the proportion of coarse particles is extremely low), and the weight percentage of the compound red pigment with a particle size range of 150-200 mesh is stable at about 3%. That is, in Examples 1-3 of the present application, both the proportion of coarse particles and the proportion of ultrafine powder are effectively controlled, which can prevent the problems of decreased dissolution rate caused by over-large compound red pigment particles or precipitation during application, and at the same time prevent the problem of dust flying caused by over-small compound red pigment particles. In addition, in Comparative Examples 1-2, the weight percentage of the compound red pigment with a particle size ≥ 80 mesh is as high as 6.87-8.97%, indicating that there are more large particles in Comparative Examples 1-2, which are likely to cause a decrease in the dissolution rate and precipitation during product application; while in Comparative Examples 2-3, the weight percentage of the compound red pigment with a particle size range of 150-200 mesh is as high as 8.14%-10.02%, indicating that there are more ultrafine dusts in the compound red pigment of Comparative Examples 2-3, and dust flying is likely to occur during the processing of the compound red pigment.

[0039] This specific implementation manner is only an interpretation of the present application and does not limit the present application. After reading this specification, those skilled in the art can make modifications without creative contributions to this specific implementation manner as needed, but as long as it is within the scope of the claims of the present application, it is protected by the patent law.

Claims

1. A preparation method of a highly soluble compound red pigment, characterized in that, Including the following steps: S1. Premixing: Stir 9.5wt%-15.5wt% natural pigment, 8wt%-12wt% emulsifier, 18wt%-25wt% maltodextrin and the balance of monascus red concentrate evenly to obtain a premix; S2. First homogenization: Conduct the first homogenization treatment on the premix to obtain an emulsion; S3. Second homogenization: Add a wall material solution to the emulsion, mix evenly, and then conduct the second homogenization treatment to obtain an embedded modified emulsion; the wall material solution is a mixed solution of a colloid, an antioxidant and water, and the weight ratio of the colloid, the antioxidant and water is (0.65-0.95):(0.85-1.8):(55-60); S4. Spray drying: Conduct spray drying granulation on the embedded modified emulsion to obtain a highly soluble compound red pigment.

2. The preparation method of the highly soluble compound red pigment according to claim 1, characterized in that: In S1, the natural pigment includes E100 beet red and E20 capsicum red, and the weight ratio of E100 beet red to E20 capsicum red is (1-2.4):(0.5-1).

3. The preparation method of the highly soluble compound red pigment according to claim 1, characterized in that: In S1, the emulsifier adopts a composition of soybean phospholipid and glycerol monostearate, and the weight ratio of soybean phospholipid to glycerol monostearate is (0.8-1.2):(1-1.5).

4. The preparation method of the highly soluble compound red pigment according to claim 1, wherein: Both the first homogenization treatment in S2 and the second homogenization treatment in S3 are carried out at 0.8MPa-1.0MPa.

5. The preparation method of the highly soluble compound red pigment according to claim 1, wherein: The colloid adopts at least one of xanthan gum, carrageenan, guar gum, arabic gum, gelatin, water-soluble cellulose, water-soluble chitosan.

6. The preparation method of the highly soluble compound red pigment according to claim 1, characterized in that: The antioxidant adopts at least one of tea polyphenols, sodium erythorbate, vitamin E.

7. The preparation method of the highly soluble compound red pigment according to claim 1, characterized in that: In S4, the mass ratio of the emulsion to the wall material solution is 1:(2.5-3.5).

8. The preparation method of the highly soluble compound red pigment according to claim 1, characterized in that: In S4, during the spray drying granulation process, the inlet air temperature is 190-220°C, and the outlet air temperature ≥95°C.

9. A highly soluble compound red pigment, characterized in that: Prepared by the preparation method of a highly soluble compound red pigment according to any one of claims 1-8.

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