阅读说明：本技术 双重乳化水溶性色素乳液及其制备方法 (Double-emulsification water-soluble pigment emulsion and preparation method thereof ) 是由 黄国晃 黄薰毅 张陈莉 于 2021-01-14 设计创作，主要内容包括：本发明公开了一种双重乳化水溶性色素乳液及其制备方法,属于食品乳化技术领域。该制备方法先将食用水溶性色素采用特定的食品级亲油型乳化剂制备成W/O型乳液,再将该W/O型乳液采用改性淀粉和特定的亲水型助乳化剂并结合高压均质形成W/O/W型乳液,其通过二次乳化方式形成水/油/水结构,将水溶性色素包裹在乳液粒径最内层。该制备方法乳化效果好,乳液稳定,溶解性佳,且食用安全性高,适于大规模工业化生产；当应用到凝胶口感颗粒中后,凝胶口感颗粒的色泽可达到直接采用水溶性色素调色的水平,且该凝胶口感颗粒中的色素不会溶出到保存液中。(The invention discloses a double-emulsification water-soluble pigment emulsion and a preparation method thereof, belonging to the technical field of food emulsification. The preparation method comprises the steps of firstly preparing edible water-soluble pigment into W/O type emulsion by adopting a specific food-grade oleophilic emulsifier, then adopting modified starch and a specific hydrophilic auxiliary emulsifier for the W/O type emulsion, combining high-pressure homogenization to form W/O/W type emulsion, forming a water/oil/water structure by a secondary emulsification mode, and wrapping the water-soluble pigment on the innermost layer of the emulsion particle size. The preparation method has the advantages of good emulsification effect, stable emulsion, good solubility, high edible safety and suitability for large-scale industrial production; when the gel mouthfeel granule is applied, the color of the gel mouthfeel granule can reach the level of directly adopting water-soluble pigment for color matching, and the pigment in the gel mouthfeel granule can not be dissolved out into the preservation solution.)

1. A preparation method of a double-emulsification water-soluble pigment emulsion is characterized by mainly comprising the following steps:

s1 preparation of W/O emulsion of water-soluble pigment

S11, heating 50-80 parts by weight of edible vegetable oil to 60-90 ℃, adding 5-10 parts by weight of food-grade oleophilic emulsifier, and stirring to dissolve into a uniform oil phase mixture;

s12, adding 10-15 parts by weight of edible water-soluble pigment into 50-80 parts by weight of hot water, and shearing at high speed of 2000-5000rpm for 5-10min to form a water phase mixture;

s13, adding the water phase mixture into the oil phase mixture at a constant speed, and shearing at 6000-10000rpm for 5-10min at a high speed with zero conductivity to form water-soluble pigment W/O type emulsion;

s2 preparation of W/O/W type emulsion of water-soluble pigment

S21, adding 200-300 parts by weight of food-grade hydrophilic type co-emulsifier into 100-120 parts by weight of softened water, uniformly stirring, slowly adding 40-50 parts by weight of modified starch while heating, uniformly stirring, continuously adding 0.1-0.3 part by weight of food-grade preservative and 0.5-2.0 parts by weight of food-grade flavoring agent, and uniformly stirring;

s22, adding 0.5-2.0 parts by weight of food-grade antioxidant into 90-100 parts by weight of the water-soluble pigment W/O type emulsion, adding the mixture into the mixture obtained in the step S21, and shearing at 8000-15000rpm for 10-30 min;

s23, heating the mixture obtained in the step S22 to 65-70 ℃, homogenizing by using a high-pressure homogenizer, and cooling the mixture to normal temperature after the homogenization is finished to obtain the water-soluble pigment W/O/W type emulsion.

2. The method for preparing a double-emulsified water-soluble pigment emulsion according to claim 1, wherein: in the step S11, the edible vegetable oil is at least one of rapeseed oil, peanut oil, soybean oil, linseed oil, corn oil, castor oil, sunflower seed oil and sesame oil.

3. The method for preparing a double-emulsified water-soluble pigment emulsion according to claim 2, wherein: in step S11, the food-grade oleophilic emulsifier is polyglycerol ricinoleate.

4. The method for preparing a double-emulsified water-soluble pigment emulsion according to claim 1, wherein: the temperature of the hot water in step S12 is 70-90 ℃.

5. The method for preparing a double-emulsified water-soluble pigment emulsion according to claim 1, wherein: the food-grade hydrophilic co-emulsifier in the step S21 is at least one of sorbitol, polysorbate and sucrose fatty acid ester.

6. The method for preparing a double-emulsified water-soluble pigment emulsion according to claim 5, wherein: in the step S21, the food-grade hydrophilic co-emulsifier is sorbitol.

7. The method for preparing a double-emulsified water-soluble pigment emulsion according to claim 1, wherein: the heating temperature in step S21 is 40 to 50 ℃.

8. The method for preparing a double-emulsified water-soluble pigment emulsion according to claim 1, wherein: in step S21, the food-grade preservative is potassium sorbate and the food-grade flavoring agent is citric acid monohydrate; in step S22, the food grade antioxidant is natural vitamin E.

9. The method for preparing a double-emulsified water-soluble pigment emulsion according to claim 1, wherein: the processing condition of the high-pressure homogenizer in the step S23 is 8-30 MPa.

10. A double-emulsified water-soluble pigment emulsion is characterized in that: prepared by the preparation method of any one of claims 1 to 9.

Technical Field

The invention relates to the technical field of food, in particular to the technical field of food emulsification, and specifically relates to a double-emulsification water-soluble pigment emulsion and a preparation method thereof.

Background

The taste particle product is popular among the public due to the unique taste, is particularly popular among young people, and common products comprise crystal particles, Qguo, popping beads and the like. For the purposes of preservation and quality stability, the taste particle product is basically packaged by taste particles (edible colloid gel) and preservation solution (sugar solution) according to a certain proportion, and the flavors of the taste particle product comprise kiwi fruit chia seed flavor, black-extract black medlar flavor, watermelon raspberry flavor, mango yellow peach flavor, honey peach flavor, brown sugar flavor, coffee flavor, rose flavor and the like; the color can be blue, amber, pink, red, green, brown, orange, etc.

The colorful color comes from various edible pigment components used in the taste granules, common edible pigment components are divided into water-soluble pigments and fat-soluble pigments according to the solubility of the edible pigment components in a solvent, and most of the edible pigment components are O/W type emulsion of the water-soluble pigments and the fat-soluble pigments applied to the taste granules. The currently commonly used water-soluble pigments comprise lemon yellow, carmine, brilliant blue, caramel color and the like, and the commonly used O/W type emulsion of fat-soluble pigments comprise beta-carotene emulsion, cochineal emulsion and the like. When the O/W type emulsion of the fat-soluble pigment is applied to the taste particles, the pigment has good stability and can not be dissolved out into the preservation solution, so the taste particles can not fade; when the water-soluble pigment is applied to the taste granules, the pigment can be gradually dissolved into the preservation solution along with the prolonging of the quality guarantee period, so that the color of the taste granules is degraded.

The double emulsification technology has less research in the material industry or the medicine industry at present, and the difficulty lies in the selection of an emulsifier and an emulsification method, so the application is not wide; and the related research and development data in the food or beverage industry is less because the types of the emulsifying agents suitable for the food and beverage industry are less. Therefore, how to apply the water-soluble pigment to the taste granules and prevent the taste granules from fading when the taste granules are stored in the aqueous storage solution is of great significance in research and development in the field of food.

Disclosure of Invention

In order to solve the defect that the water-soluble pigment is easy to fade when applied to the taste granules in the prior art, the invention prepares the double-emulsified water-soluble pigment emulsion by optimizing the emulsifier and the emulsification method, the pigment emulsion prepared by the preparation method has the advantages of good stability and good solubility, and the pigment applied to the gel taste granules can not be dissolved out.

The technical scheme of the invention is as follows:

the invention discloses a preparation method of a double-emulsification water-soluble pigment emulsion, which mainly comprises the following steps:

s1 preparation of W/O emulsion of water-soluble pigment

S11, heating 50-80 parts by weight of edible vegetable oil to 60-90 ℃, adding 5-10 parts by weight of food-grade oleophilic emulsifier, and stirring to dissolve into a uniform oil phase mixture;

s12, adding 10-15 parts by weight of edible water-soluble pigment into 50-80 parts by weight of hot water, and shearing at high speed of 2000-5000rpm for 5-10min to form a water phase mixture;

s13, adding the water phase mixture into the oil phase mixture at a constant speed, and shearing at 6000-10000rpm for 5-10min at a high speed with zero conductivity to form water-soluble pigment W/O type emulsion;

s2 preparation of W/O/W type emulsion of water-soluble pigment

S21, adding 200-300 parts by weight of food-grade hydrophilic type co-emulsifier into 100-120 parts by weight of softened water, uniformly stirring, slowly adding 40-50 parts by weight of modified starch while heating, uniformly stirring, continuously adding 0.1-0.3 part by weight of food-grade preservative and 0.5-2.0 parts by weight of food-grade flavoring agent, and uniformly stirring;

s22, adding 0.5-2.0 parts by weight of food-grade antioxidant into 90-100 parts by weight of the water-soluble pigment W/O type emulsion obtained in the S1 step, adding the mixture into the mixture obtained in the S21, and shearing at a high speed of 15000rpm at 8000-30 min;

s23, heating the mixture obtained in the step S22 to 65-70 ℃, homogenizing by using a high-pressure homogenizer, and cooling the mixture to normal temperature after the homogenization is finished to obtain the water-soluble pigment W/O/W type emulsion.

The further technical scheme is as follows:

in step S11, the edible vegetable oil is at least one of rapeseed oil, peanut oil, soybean oil, linseed oil, corn oil, castor oil, sunflower seed oil and sesame oil, preferably rapeseed oil.

The further technical scheme is as follows:

the food grade oleophilic emulsifier in step S11 is polyglycerol ricinoleate (PGPR).

The further technical scheme is as follows:

the temperature of the hot water in step S12 is 70-90 ℃.

The further technical scheme is as follows:

the food-grade hydrophilic co-emulsifier in the step S21 is at least one of sorbitol, polysorbate and sucrose fatty acid ester, preferably sorbitol, and the sorbitol can be used as a humectant while being used as a hydrophilic emulsifier.

The further technical scheme is as follows:

the heating temperature in step S21 is 40 to 50 ℃.

The further technical scheme is as follows:

in the step S21, the food-grade preservative is potassium sorbate, the food-grade flavoring agent is citric acid monohydrate, and the potassium sorbate and the citric acid monohydrate are both water-soluble preservatives and water-soluble flavoring agents, wherein the water-soluble flavoring agents can also be water-soluble flavoring agents with other tastes according to the required flavors; in step S22, the food-grade antioxidant is natural vitamin E, which is an oil-soluble antioxidant. The selected preservative, flavoring agent and antioxidant have high edible safety and relatively high consumer acceptance.

The further technical scheme is as follows:

the processing condition of the high-pressure homogenizer in the step S23 is 8-30 MPa.

The invention also discloses a double-emulsified water-soluble pigment emulsion which is prepared by adopting the preparation method, and the particle size D90 of the prepared water-soluble pigment W/O/W type double-emulsified emulsion is less than 3 mu m.

The beneficial technical effects of the invention are as follows:

1. according to the invention, the edible water-soluble pigment is prepared into the W/O type emulsion, the W/O type emulsion is prepared to form the W/O/W type emulsion, the water/oil/water three-layer structure is formed in a secondary emulsification mode, the water-soluble pigment is wrapped at the center of the innermost layer of the emulsion particle size, the three-layer structure of the emulsion particle is stable, and the middle layer is oily, so that when the emulsion particle is in an aqueous preservation solution environment, the water-soluble pigment of the innermost layer is not easy to dissolve out, and the fading condition of the gel taste particle is avoided.

2. The invention adopts specific food-grade oleophilic emulsifier to be added into edible vegetable oil to form oil phase when first emulsification is carried out, adopts modified starch and specific hydrophilic auxiliary emulsifier to combine high-pressure homogenization to form nano-scale microemulsion when second emulsification is carried out, and has good emulsification effect, stable emulsion, good solubility and high safety.

3. The preparation method provided by the invention is simple in process, strong in operability and suitable for large-scale industrial production.

4. The double-emulsified water-soluble pigment emulsion prepared by the preparation method disclosed by the invention is good in stability, good in solubility and high in food safety, after the double-emulsified water-soluble pigment emulsion is applied to the gel taste particles, the color of the gel taste particles can reach the level of directly toning by using the water-soluble pigment, and the pigment in the gel taste particles cannot be dissolved out of the preservation solution.

Drawings

FIG. 1 is a graph showing a particle size analysis of an emulsion prepared in the following example 1;

FIG. 2 is a particle size analysis chart of the particle size of the emulsion prepared in example 2 of the present invention.

Detailed Description

In order to make the technical means of the present invention clearer and to make the technical means of the present invention capable of being implemented according to the content of the specification, the following detailed description of the embodiments of the present invention is made with reference to the accompanying drawings and examples, which are provided for illustrating the present invention and are not intended to limit the scope of the present invention. In addition, the components or raw materials involved in the invention are all conventional commercial products, or can be obtained by means of conventional techniques in the field; meanwhile, related materials and operation methods which are not mentioned are conventional technical means in the field, and therefore detailed description is omitted in the specific embodiments.

Detailed description of the preferred embodiment 1

A preparation method of a double-emulsified lemon yellow emulsion mainly comprises the following steps:

s1 preparation of lemon yellow W/O type emulsion

S11, heating 74.7 parts by weight of rapeseed oil to 85 ℃, adding 8.25 parts by weight of polyglycerol polyricinoleate (PGPR), and manually stirring to dissolve the mixture into a uniform oil phase mixture;

s12, adding 10 parts by weight of lemon yellow (85 wt.%) to 66 parts by weight of hot water at 85 ℃ and shearing at 3000rpm for 5min to form an aqueous phase mixture;

s13, adding the water phase mixture into the oil phase mixture at a constant speed, shearing at 7000rpm for 5min, and detecting no conductivity by using a conductivity meter to form lemon yellow W/O type emulsion;

s2 preparation of lemon yellow W/O/W type emulsion

S21, adding 250 parts by weight of sorbitol into 110.15 parts by weight of softened water, uniformly stirring, slowly adding 45 parts by weight of modified starch (PURITY GUM2000), heating to 40 ℃, uniformly stirring, continuously adding 0.25 part by weight of potassium sorbate and 1.1 part by weight of citric acid monohydrate, and uniformly stirring;

s22, adding 1.0 weight part of natural vitamin E into 92.5 weight parts of lemon yellow W/O type emulsion, adding the mixture into the mixture obtained in the step S21, and shearing at 11000rpm for 25 min;

s23, heating the mixture obtained in the step S22 to 65-70 ℃, homogenizing by using a high-pressure homogenizer under the condition of 8MPa/20MPa, and cooling the mixture to normal temperature after the homogenization is finished to obtain the lemon yellow W/O/W type emulsion.

Specific example 2

A preparation method of a double-emulsified carmine emulsion mainly comprises the following steps:

s1 preparation of carmine W/O emulsion

S11, heating 74.7 parts by weight of rapeseed oil to 85 ℃, adding 8.25 parts by weight of polyglycerol polyricinoleate (PGPR), and manually stirring to dissolve the mixture into a uniform oil phase mixture;

s12, adding 10 parts by weight of carmine (87 wt.%) to 66 parts by weight of hot water at 85 ℃ and shearing at 3000rpm for 5min to form an aqueous phase mixture;

s13, adding the water phase mixture into the oil phase mixture at a constant speed, shearing at 7000rpm for 5min, and detecting no conductivity by using a conductivity meter to form carmine W/O type emulsion;

s2 preparation of carmine W/O/W emulsion

S21, adding 250 parts by weight of sorbitol into 110.15 parts by weight of softened water, uniformly stirring, slowly adding 45 parts by weight of modified starch (PURITY GUM2000), heating to 40 ℃, uniformly stirring, continuously adding 0.25 part by weight of potassium sorbate and 1.1 part by weight of citric acid monohydrate, and uniformly stirring;

s22, adding 1.0 weight part of natural vitamin E into 92.5 weight parts of carmine W/O type emulsion, adding the mixture into the mixture obtained in the step S21, and shearing at 11000rpm for 25 min;

s23, heating the mixture obtained in the step S22 to 65-70 ℃, homogenizing by using a high-pressure homogenizer under the condition of 8MPa/20MPa, and cooling the mixture to normal temperature after homogenization is finished to obtain the carmine W/O/W type emulsion.

Specific example 3

A preparation method of a double-emulsified lemon yellow emulsion mainly comprises the following steps:

s1 preparation of lemon yellow W/O type emulsion

S11, heating 69.8 parts by weight of peanut oil to 80 ℃, adding 9.24 parts by weight of polyglycerol polyricinoleate (PGPR), and manually stirring to dissolve the mixture into a uniform oil phase mixture;

s12, adding 12 parts by weight of lemon yellow (85 wt.%) to 73 parts by weight of hot water at 85 ℃ and shearing at 4000rpm for 8min to form an aqueous phase mixture;

s13, adding the water phase mixture into the oil phase mixture at a constant speed, shearing at a high speed of 8000rpm for 8min, and detecting by a conductivity meter when no conductivity exists to form lemon yellow W/O type emulsion;

s2 preparation of lemon yellow W/O/W type emulsion

S21, adding 247 parts by weight of sorbitol into 115.23 parts by weight of softened water, uniformly stirring, slowly adding 50 parts by weight of modified starch (PURITY GUM2000), heating to 45 ℃, uniformly stirring, continuously adding 0.15 part by weight of potassium sorbate and 1.5 parts by weight of citric acid monohydrate, and uniformly stirring;

s22, adding 1.5 parts by weight of natural vitamin E into 93.5 parts by weight of lemon yellow W/O type emulsion, adding the mixture into the mixture obtained in the step S21, and shearing at 8000rpm for 30 min;

s23, heating the mixture obtained in the step S22 to 65-70 ℃, homogenizing by using a high-pressure homogenizer under the condition of 8MPa/20MPa, and cooling the mixture to normal temperature after the homogenization is finished to obtain the lemon yellow W/O/W type emulsion.

Comparative examples 1-2 were prepared with reference to specific example 1.

Comparative example 1

In the case of other oleophilic emulsifiers. The difference from the specific example 1 is that in step S11, 74.7 parts by weight of rapeseed oil is heated to 85 ℃, 8.25 parts by weight of composite emulsifier formed by compounding citric acid glyceride and glyceryl monostearate according to the mass ratio of 2:1 is added, and the mixture is manually stirred and dissolved into a uniform oil phase mixture. The other preparation steps were the same as in example 1.

Comparative example 2

In the case of other hydrophilic coemulsifiers. The difference from embodiment 1 is that 250 parts by weight of a co-emulsifier in which glycerin and maltitol are mixed in a mass ratio of 3:4 is added to 110.15 parts by weight of demineralized water and stirred uniformly in step S21. Other preparation methods and other preparation steps in the step are the same as those in embodiment 1.

Comparative example 3

The case where the water-soluble pigment is directly used in the gel particles.

Lemon yellow (85 wt.%) was added to the components used to make the gel particles, making the gel particles. The amount added was the same as that of the water-soluble pigment contained in the emulsion added to the gel particles in the specific example 1.

The emulsions prepared in the above specific examples and comparative examples were passed through a particle size analyzer to obtain a particle size analysis chart of the emulsion. The adopted particle size analyzer is a laser particle size analyzer with the model of Beckman Coulter LS 13320, the particle size analysis result is described in the following table 1, and the particle size analysis spectra of the specific example 1 and the specific example 2 are shown in the attached figure 1 and the attached figure 2 of the specification.

The pigment emulsions prepared in the specific examples and the comparative examples are equally applied to the same gel particles in the same amount to prepare the colored gel particles, and the preparation method of the colored gel particles is a conventional technical scheme in the field and is not repeated in the specific examples. The color of the gel particles prepared was evaluated by a sensory evaluation method and represented by a five-step scale, wherein "1" represents bright color, "2" represents slightly bright color, "3" represents moderate color, "4" represents dark color, and "5" represents dark color, and the five steps gradually decrease in both brightness and lightness of color with increasing number. The evaluation results are described in table 1 below.

The same amount of the colored gel particles prepared as described above was placed in a same amount of a preservation solution (sugar solution) and left for a certain period of time, and then the dissolution of the pigment in the gel particles was evaluated based on the dissolution of the pigment in the preservation solution. The evaluation method comprises the following steps: placing corresponding water-soluble pigment (the amount of which is equal to the amount of the water-soluble pigment applied to the colored gel particles) in a preservation solution to prepare a preservation solution of the water-soluble pigment, and detecting the absorbance A1 of the preservation solution of the water-soluble pigment at 520nm by using a spectrophotometer; after placing the colored gel particles in an equal amount of preservation solution, preserving for a period of time (30 days and 90 days, respectively), then extracting the preservation solution, detecting the absorbance A2 of the preservation solution at 520nm by using a spectrophotometer, and calculating the retention degree of the pigment in the colored gel particles by using the formula (A1-A2)/A1 × 100%. The evaluation results are described in table 1 below.

TABLE 1 evaluation table of particle diameter and application property of pigment emulsion of specific examples and comparative examples

As can be seen from the results shown in the above Table 1 and the accompanying drawings 1 and 2, the double emulsified water soluble pigment emulsion prepared by the preparation method described in the present application has a small average particle size, and the D90 is less than 3 μm; the pigment emulsion prepared by the method in the comparative example has a particle size D90 of more than 13 μm. It is demonstrated that fine emulsions with stable particle size can be obtained using the specific emulsifiers, co-emulsifiers and methods of preparation described herein. Furthermore, as can be seen from the results shown in table 1 above, the color of the gel taste particles using the emulsion prepared in the present application can reach a level where the color is toned directly with the water-soluble pigment, and the pigment in the gel taste particles does not dissolve out into the preservation solution, relative to the emulsions prepared in comparative examples 1 to 2, and relative to the gel particles prepared directly using the water-soluble pigment in comparative example 3.

The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, it should be noted that, for those skilled in the art, many modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.