CN112870148B - Preparation method of probiotics microsphere with microecological balance based on traction structure - Google Patents
Preparation method of probiotics microsphere with microecological balance based on traction structure Download PDFInfo
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Abstract
The invention discloses a preparation method of probiotics microspheres based on microecological balance of a traction structure, which takes a probiotics compound as an active core layer and takes multilayer composite hyaluronic acid as a coating shell to form the probiotics compound microspheres, wherein the multilayer composite hyaluronic acid contains tetrahydro-methyl pyrimidine carboxylic acid, and the invention also provides a specific preparation method. The invention solves the problem of difficult microbial barrier repair, forms a physical-biological double repair system by using the probiotic compound to be matched with a physical water retention system of hyaluronic acid, greatly improves the protection effect of skin, and forms a physical repair system of a water anion system by using the tetrahydro-methyl pyrimidine carboxylic acid, thereby greatly improving the protection effect.
Description
Technical Field
The invention relates to a preparation method of probiotics microspheres based on microecological balance of a traction structure, and belongs to the field of skin care.
Background
It is well known that the skin, the largest organ of the human body, protects our body against external environmental insults. The stratum corneum in the epidermis is composed of a dense layer of cells, and plays an extremely important barrier role for the human body due to its compact structure. With the development and improvement of the technology, the skin is layered more and more carefully, and in addition to needing to pay attention to the physical barrier of the skin which is often contacted, the newly introduced skin microbial barrier is not separated from the health of the skin in daily skin care.
As a human body surface barrier-skin, there are often some microorganisms present, some of which may be parasitic on the skin of the human body for a longer period of time as a result of long-term adaptation, known as the normal skin microflora, also known as the normal skin flora. The normal flora and the host macroorganisms and the external environment form a habitat, microorganisms in the habitat colonize certain organs of the macroorganisms to form microbial localization, and the skin is also one of the localizations. This interdependence constitutes an ecosystem. The skin has 'good flora' which is the crucial point of the good state of our skin, and the microbial barrier and the skin physical barrier play the role of protecting our skin at the same time.
With the development of modern society, the daily work and rest time of people is not regular, the environmental condition is worse and worse, and the adverse effects on the skin are worse and worse due to the mental pressure from all aspects and the frequent cosmetic and makeup removing habits. The physical and microbial barriers of the skin are damaged, and the skin is subjected to various troubles, and the skin becomes fragile, but the current skin repair is mainly based on physical repair, and the microbial barrier damage on the surface still exists, so that the true repair is difficult to achieve.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a preparation method of probiotics microspheres based on the microecological balance of a traction structure, so as to solve the problem of difficult microbial barrier repair. The probiotic compound is matched with a physical water retention system of hyaluronic acid to form a physical-biological dual repair system, so that the protection effect of skin is greatly improved, and meanwhile, the physical repair system of a water anion system is formed by utilizing the tetrahydro-methyl pyrimidine carboxylic acid, so that the protection effect is greatly improved.
In order to achieve the purpose, the invention adopts the following technical scheme:
the probiotics microsphere based on the microecological balance of the traction structure is formed by taking a probiotics compound as an active core layer and taking multilayer composite hyaluronic acid as a coating shell, wherein the multilayer composite hyaluronic acid contains tetrahydro-methyl pyrimidine carboxylic acid, the mass content of the probiotics compound is 55-75%, and the mass content of the tetrahydro-methyl pyrimidine carboxylic acid is 5-8%.
The probiotic microspheres can be directly smeared on the skin surface after being mixed with water, and can also be further used for producing cosmetics or medicaments to be reapplied on the skin surface.
The probiotics microspheres are stored in glycerin, and the mass ratio of the glycerin to the probiotics milk balls is 15.
The water anions of the tetrahydro-methyl pyrimidine carboxylic acid form traction, so that the adsorption stability is improved, and meanwhile, the anions contribute to the adsorption of impurities on the skin, so that the cleanness of the surface of the skin is ensured; meanwhile, the milk globule taking the hyaluronic acid as the shell layer can stably wrap the probiotic compound in the core layer, so that the long-term stability of the probiotic compound is ensured, and the service life of the probiotic compound is prolonged; meanwhile, hyaluronic acid and glycerol form a weak reversible reaction of carboxyl and alcoholic hydroxyl, hyaluronic acid in the whole glycerol is subjected to the bonding traction force of the glycerol, the milk globules are suspended in the glycerol by matching the viscosity of the glycerol, a boundary structure taking the hyaluronic acid as a protective shell is formed based on the insolubility of the glycerol and the hyaluronic acid, and the probiotic compound is isolated from the glycerol, so that the relative stability is realized; in the using process, the hyaluronic acid shell layer on the surface of the prebiotics milk ball is pressed and broken in the stress extrusion process, and the probiotic compound in the prebiotics milk ball is released to form the effects of promoting the expression of skin antibacterial peptide and improving the composition of skin flora, so that the skin state is comprehensively improved, and the skin problems such as atopic dermatitis, sensitive skin and the like can be better improved; meanwhile, hyaluronic acid can form stable physical barrier repair, and water is kept on the skin; the repairing effect is formed in two directions of physics and bacterial colony, the skin is helped to reestablish a complete structure cuticle and establish a healthy and good microbial colony ecological ring, and therefore the skin state is improved; in the process, a stable physical protection system of an anion system is formed in the physical protection layer based on the water anion characteristic of the tetrahydro-methyl pyrimidine carboxylic acid, and a weak anion structure can promote a colony system.
Glycerin and hyaluronic acid all belong to the humectant, and in the in-service use in-process, hyaluronic acid and glycerin form compound double-deck water retention structure, and effectual promotion is protected water the effect, and both belong to different material structures, form the physics repair system of composite system on skin surface, reach long-term water retention effect.
In order to improve the viscosity of the glycerol, carbomer is added, the adding amount is 0.01-0.05% of the mass of the glycerol, and carbomer 940 or carbomer 934 is adopted as the carbomer.
The preparation method of the probiotic microspheres comprises the following steps: step 1, adding hyaluronic acid into distilled water, performing low-temperature ultrasonic dispersion to form a solution, and then performing constant-temperature granulation to form microsphere particles; the concentration of the hyaluronic acid in distilled water is 30-60 g/L, the low-temperature ultrasonic temperature is 10-20 ℃, and the ultrasonic dispersion is 40-90 kHz; the temperature of the constant-temperature granulation is 130-150 ℃, and the particle size of the granulation is 3-8 mm; step 2, uniformly stirring carbomer and absolute ethyl alcohol, adding tetrahydro-methyl pyrimidine carboxylic acid to obtain a mixed solution, uniformly spraying the mixed solution on the surfaces of the microsphere particles to form a surface wet film, performing surface spraying by adopting the solution in the step 1, and drying to obtain composite microsphere particles; the mass of the carbomer and the absolute ethyl alcohol is 0.1-0.2 percent 2 (ii) a The spraying amount of the surface spray is 0.4-0.7 mL/cm 2 The drying temperature is 100-120 ℃; step 3, injecting the mixed probiotics into the microsphere particles in a needle injection mode to obtain the probiotics milk balls; the injection amount of the mixed probiotics is 125-300% of the mass of the microsphere particles.
The probiotic compound comprises symbiotic prebiotics, distilled water and oat kernel oil, and the probiotic compound comprises the following components in percentage by mass: 10 to 20 parts of symbiotic probiotics, 2 to 5 parts of distilled water and 3 to 6 parts of oat kernel oil.
The symbiotic prebiotics are composed of 70% of alpha-glucan oligosaccharide by mass, 19% of beta-fructo-oligosaccharide by mass and a mixed strain of lactobacillus casei and lactobacillus acidophilus in any proportion. The lactobacillus casei and the lactobacillus acidophilus are both subjected to freeze drying and inactivation.
From the above description, it can be seen that the present invention has the following advantages:
1. the invention solves the problem of difficult microbial barrier repair, forms a physical-biological double repair system by using the probiotic compound to be matched with a physical water retention system of hyaluronic acid, greatly improves the protection effect of skin, and forms a physical repair system of a water anion system by using the tetrahydro-methyl pyrimidine carboxylic acid, thereby greatly improving the protection effect.
2. The invention utilizes the coating effect of hyaluronic acid to form the stability of the probiotic compound, forms suspension dispersion in glycerol and forms a double physical repair water retention system with the glycerol.
Detailed Description
The present invention will be described in detail with reference to examples, but the present invention is not limited to the claims.
Example 1
A probiotics microsphere based on micro-ecological balance of a traction structure is formed by taking a probiotics compound as an active core layer and taking multilayer composite hyaluronic acid as a coating shell, wherein the multilayer composite hyaluronic acid contains tetrahydro-methyl pyrimidine carboxylic acid.
The probiotics microspheres are stored in glycerin, and the mass ratio of the glycerin to the probiotics milk balls is 15.
In order to improve the viscosity of the glycerol, carbomer is added, wherein the adding amount is 0.01 percent of the mass of the glycerol, and carbomer 940 is adopted.
The preparation method of the probiotic microspheres comprises the following steps: step 1, adding hyaluronic acid into distilled water, performing low-temperature ultrasonic dispersion to form a solution, and then performing constant-temperature granulation to form microsphere particles; the concentration of the hyaluronic acid in distilled water is 30g/L, the low-temperature ultrasonic temperature is 10 ℃, and the ultrasonic dispersion is 40kHz; the temperature of the constant-temperature granulation is 130 ℃, and the particle size of the granulation is 3mm; step 2, uniformly stirring carbomer and absolute ethyl alcohol, adding tetrahydro-methyl pyrimidine carboxylic acid to obtain a mixed solution, uniformly spraying the mixed solution on the surfaces of the microsphere particles to form a surface wet film, performing surface spraying by adopting the solution in the step 1, and drying to obtain composite microsphere particles; of carbomer with absolute ethanolThe mass of the mixed solution is 0.1 percent 2 (ii) a The amount of the surface spray was 0.4mL/cm 2 The drying temperature is 100 ℃; step 3, injecting the mixed probiotics into the microsphere particles in a needle injection manner to obtain the probiotics milk balls; the injection amount of the mixed probiotics is 125 percent of the mass of the microsphere particles.
The probiotic compound comprises symbiotic prebiotics, distilled water and oat kernel oil, and the probiotic compound comprises the following components in percentage by mass: 10 parts of symbiotic prebiotics, 2 parts of distilled water and 3 parts of oat kernel oil.
The symbiotic prebiotics are composed of alpha-glucan oligosaccharide with the mass ratio of 70%, beta-fructo-oligosaccharide with the mass ratio of 19% and mixed strains of lactobacillus casei and lactobacillus acidophilus, and the ratio of the lactobacillus casei to the lactobacillus acidophilus is 3. The lactobacillus casei and the lactobacillus acidophilus are both subjected to freeze drying and inactivation.
The probiotic milk globules prepared in this example were 8mm in diameter, suspended in glycerol to form a stable suspension.
Example 2
The probiotics microsphere based on the microecological balance of the traction structure is formed by taking a probiotics compound as an active core layer and taking multilayer composite hyaluronic acid as a coating shell, wherein the multilayer composite hyaluronic acid contains tetrahydro-methyl pyrimidine carboxylic acid, the probiotics microsphere is stored in glycerin, and the mass ratio of the glycerin to the probiotics milk sphere is 15.
In order to improve the viscosity of the glycerol, carbomer is added, wherein the adding amount is 0.05 percent of the mass of the glycerol, and carbomer is carbomer 934.
The preparation method of the probiotic microspheres comprises the following steps: step 1, adding hyaluronic acid into distilled water, performing low-temperature ultrasonic dispersion to form a solution, and then performing constant-temperature granulation to form microsphere particles; the concentration of the hyaluronic acid in distilled water is 60g/L, the temperature of low-temperature ultrasonic treatment is 20 ℃, and ultrasonic dispersion is 90kHz; the temperature of the constant-temperature granulation is 150 ℃, and the particle size of the granulation is 8mm; step 2, mixing carbomer with anhydrousUniformly stirring ethanol, adding tetrahydro-methyl pyrimidine carboxylic acid to obtain a mixed solution, uniformly spraying the mixed solution on the surfaces of the microsphere particles to form a surface wet film, performing surface spraying by adopting the solution in the step 1, and drying to obtain composite microsphere particles; the mass of the carbomer and absolute ethyl alcohol is 0.2 percent, the adding amount of the tetrahydro-methyl pyrimidine carboxylic acid is 12 percent of the mass of the absolute ethyl alcohol, and the spraying amount of the uniform spraying is 0.4mL/cm 2 (ii) a The amount of the surface spray was 0.7mL/cm 2 The drying temperature is 120 ℃; step 3, injecting the mixed probiotics into the microsphere particles in a needle injection mode to obtain the probiotics milk balls; the injection amount of the mixed probiotics is 300 percent of the mass of the microsphere particles.
The probiotic compound comprises symbiotic prebiotics, distilled water and oat kernel oil, and the probiotic compound comprises the following components in percentage by mass: 20 parts of symbiotic prebiotics, 5 parts of distilled water and 6 parts of oat kernel oil.
The symbiotic prebiotics comprise alpha-glucan oligosaccharide with the mass ratio of 70%, beta-fructo-oligosaccharide with the mass ratio of 19% and mixed strains of lactobacillus casei and lactobacillus acidophilus, and the mass ratio of the lactobacillus casei to the lactobacillus acidophilus is 9. The lactobacillus casei and the lactobacillus acidophilus are both subjected to freeze drying and inactivation.
The probiotic milk globules prepared in this example were 13mm in diameter, suspended in glycerol to form a stable suspension.
Example 3
The probiotics microsphere based on the microecological balance of the traction structure is formed by taking a probiotics compound as an active core layer and taking a multilayer composite hyaluronic acid as a coating shell, wherein the multilayer composite hyaluronic acid contains tetrahydro-methyl pyrimidine carboxylic acid, the probiotics microsphere is stored in glycerin, and the mass ratio of the glycerin to the probiotics milk ball is 5.
The preparation method of the probiotic microspheres comprises the following steps: step 1, adding hyaluronic acid into distilled water, performing low-temperature ultrasonic dispersion to form a solution, and then performing constant-temperature granulation to form microsphere particles; the concentration of hyaluronic acid in distilled water is 50g/L, the temperature of low-temperature ultrasonic treatment is 15 ℃, and the temperature of ultrasonic treatment is ultraThe acoustic dispersion was 70kHz; the temperature of the constant-temperature granulation is 140 ℃, and the particle size of the granulation is 6mm; step 2, uniformly stirring carbomer and absolute ethyl alcohol, adding tetrahydro-methyl pyrimidine carboxylic acid to obtain a mixed solution, uniformly spraying the mixed solution on the surfaces of the microsphere particles to form a surface wet film, performing surface spraying by adopting the solution in the step 1, and drying to obtain composite microsphere particles; the mass of the carbomer and the absolute ethyl alcohol is 0.1 percent 2 (ii) a The amount of the surface spray was 0.6mL/cm 2 The drying temperature is 110 ℃; step 3, injecting the mixed probiotics into the microsphere particles in a needle injection manner to obtain the probiotics milk balls; the injection amount of the mixed prebiotics is 250 percent of the mass of the microsphere particles.
The probiotic compound comprises symbiotic prebiotics, distilled water and oat kernel oil, and the probiotic compound comprises the following components in percentage by mass: 15 parts of symbiotic prebiotics, 4 parts of distilled water and 5 parts of oat kernel oil.
The symbiotic prebiotics comprise alpha-glucan oligosaccharide with the mass ratio of 70%, beta-fructo-oligosaccharide with the mass ratio of 19% and mixed strains of lactobacillus casei and lactobacillus acidophilus, and the mass ratio of the lactobacillus casei to the lactobacillus acidophilus is 1. The lactobacillus casei and the lactobacillus acidophilus are both subjected to freeze drying and inactivation.
The probiotic milk globules prepared in this example were 11mm in diameter, suspended in glycerol to form a stable suspension.
Comparative experiment
(1) Test for repairing and moisturizing
40 volunteers were randomly selected and divided into 2 experimental groups of 20 individuals each, with no significant difference between groups. Group 1 volunteers were evenly coated with 0.1mL of the suspension of lactoglobulin from example 1 continuously for 8 weeks using the method: the administration is given in the morning and evening, respectively, 1 time per day. 2 groups of natural states, without any skin care product, the effect of the probiotic milk balls on improving various aspects of the skin is examined, and the skin is moistened by clear water before use.
And (3) symptom evaluation: randomized assessments were performed by dermatologists at 4 and 8 weeks prior to use, in combination with self-assessment by volunteers. The moisture retention was measured using a kernometer CM 825.
The symptoms are characterized in that: dryness, scaling, erythema, pruritus and overall severity.
Index grading: 0= none; 1= lighter; 2= medium; 3= severe.
The test results were as follows:
degree of itching
Moisture retention
| Humidity keeping (0 week) | Humidity keeping (4 weeks) | Humidity (8 weeks) | |
| Example 1 | 6％ | 39％ | 45％ |
| Comparative example | 6％ | 5％ | 5％ |
(2) Improvement of the general condition of the skin
40 volunteers were randomly selected and divided into 2 experimental groups of 20 individuals each, with no significant difference between groups. Group 1 volunteers were evenly coated with 0.1mL of the suspension of lactoglobulin from example 1 continuously for 8 weeks using the method: the administration is given in the morning and evening, respectively, 1 time per day. 2 groups of natural state without any skin care product.
Testing an instrument: VISA digital skin analyzer, skin melanin and heme tester, skin elasticity tester and skin moisture tester
Test items: skin percutaneous water loss, fineness, whiteness, smoothness and elasticity
Grading standard: the test results were very satisfactory for 5 points (the degree of improvement of the test results was more than 50% compared to the test results before the test), satisfactory for 3 points (the degree of improvement of the test results was 20 to 50% compared to the test results before the test), and unsatisfactory for 0 points (the test results were not improved any more than before the test).
The test result shows that the product of the example 1 has good effects on improving the skin fineness, whiteness, smoothness, elasticity and the like, and the score is more than 4.8.
(3) Skin texture test
a. Test instrument
Multifunctional skin image analysis system
b. Test method
The subjects were 20 wrinkled subjects with an average age of 35 to 45 years. The test subject smears the water aqua accounting for 5% of the product in the example 1 on the experimental part of the left arm twice a day in the morning and at night, and the experimental part of the right arm is used as a control and is not smeared with a sample.
After 4 weeks of continuous observation, the relative reduction rate of the skin roughness at the fourth week is more than 14%, good anti-wrinkle and anti-wrinkle effects are shown, and the obvious difference of the surfaces of the left arm and the right arm in mutual contrast also proves the anti-wrinkle effect.
In summary, the invention has the following advantages:
1. the invention solves the problem of difficult microbial barrier repair, forms a physical-biological double repair system by using the probiotic compound to be matched with a physical water retention system of hyaluronic acid, greatly improves the protection effect of skin, and forms a physical repair system of a water anion system by using the tetrahydro-methyl pyrimidine carboxylic acid, thereby greatly improving the protection effect.
2. The invention utilizes the coating effect of hyaluronic acid to form the stability of the probiotic compound, forms suspension dispersion in glycerol and forms a double physical repair water retention system with the glycerol.
It should be understood that the detailed description of the invention is merely illustrative of the invention and is not intended to limit the invention to the specific embodiments described. It will be appreciated by those skilled in the art that the present invention may be modified or substituted equally as well to achieve the same technical result; as long as the use requirements are met, the method is within the protection scope of the invention.
Claims (2)
1. A suspension containing probiotics microspheres and glycerin is characterized in that:
taking a probiotic compound as an active core layer and taking a multilayer compound hyaluronic acid as a coating shell to form a probiotic microsphere, wherein the multilayer compound hyaluronic acid contains tetrahydro-methyl pyrimidine carboxylic acid; the mass content of the probiotic compound is 55-75%, and the mass content of the tetrahydro-methyl pyrimidine carboxylic acid is 5-8%;
the probiotic microspheres are stored in glycerol; and the mass ratio of the glycerol to the probiotics microsphere is 15;
the probiotic complex consists of: symbiotic prebiotics, distilled water and oat kernel oil; the probiotic compound comprises the following components in percentage by mass: 10-20 parts of symbiotic prebiotics, 2-5 parts of distilled water and 3-6 parts of oat kernel oil;
the symbiotic prebiotics consist of alpha-glucan oligosaccharide with the mass ratio of 70 percent, beta-fructo-oligosaccharide with the mass ratio of 19 percent and mixed strains of lactobacillus casei and lactobacillus acidophilus;
preparation method of probiotic microspheresComprises the following steps: step 1, adding hyaluronic acid into distilled water, performing low-temperature ultrasonic dispersion to form a solution, and then performing constant-temperature granulation to form microsphere particles; the concentration of the hyaluronic acid in distilled water is 30-60 g/L, the low-temperature ultrasonic temperature is 10-20 ℃, and the ultrasonic dispersion is 40-90 kHz; the temperature of the constant-temperature granulation is 130-150 ℃, and the particle size of the granulation is 3-8 mm; step 2, uniformly stirring carbomer and absolute ethyl alcohol, adding tetrahydro-methyl pyrimidine carboxylic acid to obtain a mixed solution, uniformly spraying the mixed solution on the surfaces of the microsphere particles to form a surface wet film, performing surface spraying by adopting the solution in the step 1, and drying to obtain composite microsphere particles; the mass of the carbomer and the absolute ethyl alcohol is 0.1-0.2 percent, the adding amount of the tetrahydro-methylpyrimidine carboxylic acid is 10-12 percent of the mass of the absolute ethyl alcohol, and the spraying amount of the uniform spraying is 0.2-0.4 mL/cm 2 (ii) a The spraying amount of the surface spray is 0.4-0.7 mL/cm 2 The drying temperature is 100-120 ℃; step 3, injecting the mixed probiotics into the microsphere particles in a needle injection mode to obtain the probiotics microspheres; the injection amount of the mixed probiotics is 125-300% of the mass of the microsphere particles.
2. Use of a suspension comprising probiotic microspheres and glycerol according to claim 1, for the preparation of a medicament and/or a cosmetic product for the repair and/or prevention of physical barrier damages and/or microbial barrier damages of the skin.
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