A composition capable of stabilizing nanoemulsion, nanoemulsion composition, preparation method and application thereof
The stability of the nanoemulsion system was solved by using a composition of acryloyldimethylammonium taurate/VP copolymer, sodium mannose phosphate and a specific combination of nanoemulsifiers, combined with the phase-transformation process in the low-energy emulsification method. The problem of difficulty in taking into account both the permeability is difficult to take into account, and the preparation of nanoemulsion compositions with excellent stability and low stimulation is achieved.
Patent Information
- Application Number
- CN202410421996.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-04-09
- Publication Date
- 2025-02-14
- Estimated Expiration
- 2044-04-09
AI Technical Summary
The existing nanoemulsion system is difficult to take into account both stability and permeability. High concentrations of emulsifiers may cause skin irritation or allergies. The existing equipment is costly and complex in operation, making it difficult to be suitable for large-scale production.
Using a composition including acryloyldimethylammonium taurate/VP copolymer, mannose sodium phosphate and a specific combination, the nanoemulsifier is prepared by a phase-transformation process in a low-energy emulsification method to achieve stability Optimization of sexual and permeability.
The prepared nanoemulsion composition has excellent stability, and it is not easy to demulsify and delaminate when placed for a long time. The low concentration design of the nanoemulsifier reduces the irritability to the skin, making it suitable for large-scale production.
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Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of cosmetics, and in particular to a composition capable of stabilizing a nanoemulsion, a nanoemulsion composition, and a preparation method and application thereof. Background Art
[0002] In the cosmetics industry, nanoemulsification technology, as an emerging technical means, is gradually gaining favor in the industry. Nanoemulsion compositions, due to their nanometer-scale particle size, can achieve more efficient penetration and more stable storage, thereby improving the efficacy and use experience of cosmetics. At present, the formulation design of nanoemulsion compositions mainly revolves around key components such as active ingredients, emulsifiers, co-emulsifiers and aqueous phases, aiming to obtain a nanoemulsion system with high stability and strong permeability. Nanoemulsion is a non-equilibrium system, and its formation requires the help of external energy. In terms of preparation methods, existing technologies mainly rely on mechanical equipment such as high-pressure homogenization and ultrasonic emulsification: high-pressure homogenizers use high pressure and shear force to break large particles in the emulsion into small nano-scale particles to prepare nanoemulsions. At the same time, in order to enhance the stability of the emulsion, a certain amount of emulsifiers and co-emulsifiers are usually used in the formula. Emulsifiers reduce the tension at the oil-water interface, allowing the oil phase and the water phase to combine more stably to form a uniform emulsion system.
[0003] However, due to the complexity and instability of the nanoemulsion system, existing formulas often find it difficult to take into account all performance requirements: for example, the solubility of certain active ingredients in the nanoemulsion system is limited, making it difficult to achieve the ideal addition amount; at the same time, the selection and dosage of emulsifiers and co-emulsifiers also need to make a trade-off between stability and permeability. In order to prepare stable nanoemulsions, it is often necessary to use high concentrations of emulsifiers and cooperate with special process conditions. Since emulsifiers are amphiphilic, that is, they can be dissolved in both oil and water, high concentrations of emulsifiers may burden the skin and cause adverse reactions such as skin irritation or allergies. Secondly, from the perspective of preparation methods, although existing high-pressure homogenization, ultrasonic emulsification and other equipment can achieve the preparation of nanoemulsions, the equipment cost is high, the operation is complicated, and it is difficult to apply to large-scale production. In addition, these equipment may require high energy consumption and long processing time during the preparation process, increasing production costs and time costs.
[0004] The stability of nanoemulsions is also a major challenge in the prior art. Since nanoemulsions have a small particle size and a large specific surface area, they are easily affected by the external environment (such as temperature, light, pH value, etc.) and undergo physical or chemical changes, resulting in decreased emulsion stability. Therefore, it is necessary to provide a nanoemulsion composition with a low emulsifier content and a simple preparation method and stable properties. Summary of the invention
[0005] The purpose of the present invention is to overcome the shortcomings of the prior art and provide a composition capable of stabilizing nanoemulsion, a nanoemulsion composition, a preparation method and an application thereof.
[0006] To achieve the above object, in a first aspect of the present invention, the present invention provides a composition capable of stabilizing a nanoemulsion, the composition capable of stabilizing a nanoemulsion comprising the following components in parts by weight: 0.5-1.5 parts of ammonium acryloyldimethyltaurate / VP copolymer, 0.5-1.0 parts of sodium mannose phosphate, and 5-10 parts of a nanoemulsifier;
[0007] The nanoemulsifier comprises water, sunflower seed oil glycerides, sodium stearoyl glutamate and lauroyl wheat amino acid potassium.
[0008] In the composition capable of stabilizing the nanoemulsion provided by the present invention, by selecting the ammonium acryloyldimethyltaurate / VP copolymer, sodium mannose phosphate and the nanoemulsifier in a suitable mass range, the three have an obvious synergistic effect. In the subsequent application process, the nanoemulsion can be effectively stabilized on the basis of helping to achieve the preparation of small-particle nanoemulsion. The prepared nanoemulsion composition has excellent long-term storage stability and is not prone to demulsification and stratification.
[0009] Specifically, since sodium stearoyl glutamate and potassium lauroyl wheat amino acid in the nanoemulsifier are both anionic emulsifiers, in the subsequent application process, the emulsion droplets also carry partial negative charges under the action of the nanoemulsifier. Due to the repulsion of like charges, it is more difficult for the emulsion droplets to aggregate, thereby preventing the particle size of the emulsion droplets from increasing; ammonium acryloyldimethyltaurate / VP copolymer can increase the viscosity of the system, thereby reducing the floating speed of the emulsion droplets, and can also inhibit the aggregation of emulsion droplets, thereby improving the stability of the emulsion when subsequently applied to the emulsion; sodium mannose phosphate can make the external phase (aqueous phase) of the subsequently prepared emulsion carry negatively charged ions, and the emulsion droplets also carry partial negative charges under the action of the emulsifier. Due to the repulsion of like charges, it is more difficult for the emulsion droplets to aggregate together, thereby preventing the particle size of the emulsion droplets from increasing.
[0010] As a preferred embodiment of the composition capable of stabilizing nanoemulsion of the present invention, in the nanoemulsifier, the mass ratio of water, sunflower oil glycerides, sodium stearoyl glutamate, and lauroyl wheat amino acid potassium is 40:30:18:12.
[0011] The invention finds that the nanoemulsifier is a composition of water, sunflower oil glycerides, sodium stearoyl glutamate and lauroyl wheat amino acid potassium; the sunflower oil glycerides can form a stable emulsified layer on the oil-water interface, the glycerol part of the sunflower oil glycerides contains multiple hydroxyls and can form hydrogen bonds with water molecules, while the fatty acid part interacts with the oil phase, so that the interfacial tension can be effectively reduced, fine emulsified particles can be formed, and the stability of the emulsified system can be increased; the lauroyl wheat amino acid potassium and the sodium stearoyl glutamate are both mild amino acid type surfactants, have an amphiphilic structure, can be well oriented on the oil-water interface, form a solid interface film, and effectively prevent the aggregation of oil droplets, so as to achieve the stability of the emulsified system; the water, sunflower oil glycerides, sodium stearoyl glutamate and lauroyl wheat amino acid potassium in the nanoemulsifier work synergistically to form stable and fine nanoemulsifier particles; and at the same time, each component in the formula of the nanoemulsifier has high mildness and will not cause irritation to the skin. Therefore, the selection of the mass ratio of the components in the nanoemulsifier will affect the subsequent effect of stabilizing the emulsion. When the mass ratio of the components in the nanoemulsifier is further selected to be the above value, the three can have a better synergistic effect. When it is subsequently applied to the preparation of the emulsion composition, the stability of the obtained nanoemulsion composition is more excellent.
[0012] As a preferred embodiment of the composition capable of stabilizing nanoemulsion of the present invention, the preparation method of the nanoemulsifier comprises the following steps:
[0013] (1) dissolving sodium stearoyl glutamate and potassium lauroyl wheat amino acid in water to obtain an aqueous phase;
[0014] (2) adding the aqueous phase to the sunflower seed oil glycerides, maintaining a stirring speed of 250-350 rpm during the addition process, and stirring for 8-12 minutes after the addition is completed to obtain a nanoemulsifier.
[0015] The stability of nanoemulsifiers is related to the composition, particle size, preparation process, etc. Unstable nanoemulsifiers have Ostwald ripening. ripening) phenomenon, that is, when the particle size is polydisperse, since the solubility of small particles is greater than that of large particles, oil molecules diffuse from small particles to large particles and diffuse through the continuous phase (aqueous phase); using this nanoemulsifier is not conducive to the subsequent preparation of a stable nanoemulsion composition; the present invention has found that by adopting the preparation method of the nanoemulsifier in the present invention, specifically the sudden phase transition process in the low-energy emulsification method, by slowly adding the water phase to the oil phase, when 3%-8% water is added, due to the excess oil phase, a W / O type emulsion is formed, and a gel can be seen at this time; continuing to add the water phase will change the curvature of the system surfactant; when the emulsion phase inversion point is reached, the surface tension is the smallest at this time; after the emulsion phase inversion point, when the water phase is continued to be added, the O / W type emulsion is also formed, and a nanoemulsifier that can further cooperate with ammonium acryloyldimethyltaurate / VP copolymer and sodium mannose phosphate to achieve a stable nanoemulsion composition is also formed. At the same time, the sudden phase transition process can achieve emulsification under low energy input, which reduces energy consumption in the production process and improves production efficiency. Compared with the conventional high-pressure homogenization method, it does not require high-pressure equipment and special processes, and nanoemulsions can be made through conventional emulsification processes, which can be put into industrial large-scale production.
[0016] In a second aspect of the present invention, the present invention provides a use of the composition capable of stabilizing nanoemulsion in preparing a nanoemulsion composition.
[0017] In the third aspect of the present invention, the present invention provides a nanoemulsion composition, wherein the nanoemulsion composition comprises the composition capable of stabilizing nanoemulsion according to the present invention.
[0018] By adding the composition capable of stabilizing nanoemulsions to the nanoemulsion composition provided by the present invention, the preparation of an emulsion with a nano-particle size can be achieved, and the obtained nanoemulsion composition has excellent stability and will not show demulsification and stratification phenomenon when placed under high temperature, low temperature, light or room temperature environment for 30 days.
[0019] As a preferred embodiment of the nanoemulsion composition of the present invention, the nanoemulsion composition further comprises an emollient, a moisturizer, an antioxidant, and a chelating agent.
[0020] As a preferred embodiment of the nanoemulsion composition of the present invention, the nanoemulsion composition comprises the following components in mass percentage: 5-15% of the composition capable of stabilizing the nanoemulsion of the present invention, 1-10% of an emollient, 2-10% of a moisturizer, 0.1-1% of an antioxidant, 0.01-0.1% of a chelating agent, and the balance of water.
[0021] Preferably, the nanoemulsion composition comprises the following components in percentage by mass: 9.8% of the composition capable of stabilizing the nanoemulsion of the present invention, 3% of an emollient, 6.5% of a moisturizer, 0.45% of an antioxidant, 0.03% of a chelating agent, and the remainder of water.
[0022] The present invention has found that when the mass percentages of the components of the nanoemulsion composition are further selected to be within the above range, the obtained nanoemulsion composition is mild and non-irritating, has a moderate particle size, and has excellent stability.
[0023] As a preferred embodiment of the nanoemulsion composition of the present invention, the emollient includes at least one of octyl polymethylsiloxane and isononyl isononanoate.
[0024] Preferably, the mass ratio of the octyl polymethylsiloxane to isononyl isononanoate is 1:1.
[0025] The present invention has found that when octyl polymethicone and isononyl isononanoate are selected as the emollients, the comprehensive performance of the obtained product is better; specifically, isononyl isononanoate has a stable molecular structure and a long carbon chain, and its molecules can easily penetrate into the deep layer of the skin to provide long-term nourishment and moisturizing for the skin; the silicon oxygen chain in octyl polymethicone forms a thin film on the skin surface to lock in moisture and effectively prevent skin dryness; the molecular structure of isononyl isononanoate helps to form a stable emulsification system, and octyl polymethicone can enhance the stability of the emulsification interface and prevent emulsion stratification or demulsification; the combined effect of the two enables the nano-emulsification product to maintain stable texture and performance.
[0026] As a preferred embodiment of the nanoemulsion composition of the present invention, the moisturizing agent includes at least one of glycerol, 1,2-hexanediol and butylene glycol.
[0027] Preferably, the mass ratio of the glycerol, 1,2-hexanediol and butanediol is 10:1:2.
[0028] The present invention has found that glycerol, 1,2-hexanediol and butylene glycol are used as moisturizers. Since the molecular structure of the above ingredients contains multiple hydroxyl groups, glycerol has strong hygroscopicity and moisturizing properties; 1,2-hexanediol provides antibacterial protection, while butylene glycol penetrates deep into the skin for deep moisturizing; this combination can not only provide comprehensive moisturizing care for the skin, but also ensure the safety and stability of the product. In addition, glycerol can form hydrogen bonds with water molecules, increase the viscosity of the continuous phase of the emulsion system, thereby helping to reduce the aggregation and sedimentation of emulsion droplets; 1,2-hexanediol can also adjust the osmotic pressure of the emulsion system, prevent water from evaporating too quickly from the emulsion system, and thus maintain the stability of the emulsion system.
[0029] As a preferred embodiment of the nanoemulsion composition of the present invention, the antioxidant includes p-hydroxyacetophenone.
[0030] The present invention has found that p-hydroxyacetophenone, as an antioxidant, has phenolic hydroxyl groups in its molecular structure that can effectively remove or neutralize free radicals, preventing free radicals from causing oxidative damage to other ingredients in the product; this helps to extend the shelf life of the product and maintain the color, aroma and efficacy of the product.
[0031] As a preferred embodiment of the nanoemulsion composition of the present invention, the chelating agent includes EDTA-disodium.
[0032] EDTA-disodium can significantly improve the stability of the product by chelating heavy metal ions, while reducing its potential irritation to the skin and ensuring the safe use of the product.
[0033] In a fourth aspect of the present invention, the present invention provides a method for preparing the nanoemulsion composition, the preparation method comprising the following steps:
[0034] (1) Mix the materials of phase A and stir at 200-300 rpm for 4-6 min, then heat to 60-75°C;
[0035] (2) Mix the materials of phase B and heat them to 60-75° C., then add them to the phase A in step (1), and stir at a speed of 150-300 rpm until the system changes from a gel state to a liquid state, to obtain a mixture 1;
[0036] (3) Mix the materials of phase C and heat them to 60-75° C., then add them to the mixture 1 in step (2), stir them at a speed of 300-350 rpm for 8-12 min, then homogenize them at a speed of 10000-12000 rpm for 3-5 min, and then cool them to 40-45° C. to obtain a mixture 2;
[0037] (4) adding the phase D material to the mixture 2 of step (3), and stirring at a speed of 500-800 rpm for 3-5 min to obtain a nanoemulsion composition;
[0038] The phase A material is a nanoemulsifier and an emollient; the phase B material is part of water; the phase C material is a moisturizer, a chelating agent, an antioxidant, ammonium acryloyldimethyltaurate / VP copolymer and the remaining water; and the phase D is sodium mannose phosphate.
[0039] The preparation method provided by the present invention can prepare a nanoemulsion composition with excellent stability.
[0040] In a fifth aspect of the present invention, the present invention provides a use of a nanoemulsion composition in preparing a skin care product.
[0041] The nanoemulsion composition provided by the present invention can maintain good stability, and can help improve the stability of skin care products and extend the shelf life.
[0042] Compared with the prior art, the present invention has the following advantages:
[0043] 1. The present invention provides a composition capable of stabilizing a nanoemulsion, and by selecting a specific composition ratio of ammonium acryloyldimethyltaurate / VP copolymer, sodium mannose phosphate and a nanoemulsifier, the subsequent stabilization of the nanoemulsion composition can be achieved;
[0044] 2. The present invention provides a method for preparing a composition capable of stabilizing nanoemulsions. Based on the sudden phase transition process in the low-energy emulsification method, the water phase is slowly added to the oil phase continuously to achieve the transformation of the emulsion from the W / O type to the O / W type, thereby forming a nanoemulsifier. By controlling the mass ratio of the components, the phase transition point of the emulsion can be accurately adjusted. Near the phase transition point, the surface tension reaches a minimum, which helps to form a more stable and uniform emulsified system. The preparation process does not require special equipment and processes and is suitable for large-scale production. When the prepared nanoemulsifier is used in the preparation of subsequent products, it can effectively stabilize the product.
[0045] 3. The nanoemulsion composition provided by the present invention can achieve a moderate particle size range and excellent high temperature, low temperature, light and room temperature stability by adding a composition that can stabilize the nanoemulsion; and the preparation method of the nanoemulsion composition provided by the present invention is simple to operate and is conducive to actual production. BRIEF DESCRIPTION OF THE DRAWINGS
[0046] Figure 1 is a particle size distribution diagram of the nanoemulsion composition of Examples 1-3;
[0047] Figure 2 Graph showing particle size distribution of the nanoemulsion compositions of Comparative Examples 1-16. DETAILED DESCRIPTION
[0048] To better illustrate the purpose, technical solutions and advantages of the present invention, the present invention will be further described below in conjunction with specific examples. Other materials, reagents, etc. used in the examples, unless otherwise specified, can be obtained from commercial sources.
[0049] Examples 1-3 and Comparative Examples 1-13
[0050] The present invention provides a nanoemulsion composition according to the embodiment and comparative example. The component contents (mass percentage) of the nanoemulsion composition are shown in Table 1-2.
[0051] Table 1
[0052]
[0053]
[0054] Table 2
[0055]
[0056]
[0057] Wherein, the nanoemulsifier in Examples 1-3 and Comparative Examples 1-13 is a mixture of water, sunflower oil glycerides, sodium stearoyl glutamate, and lauroyl wheat amino acid potassium in a mass ratio of 40:30:18:12.
[0058] The method for preparing the nanoemulsion composition provided in Example 1 comprises the following steps:
[0059] (1) Preparation of nanoemulsifier: Sodium stearoyl glutamate and potassium lauroyl wheat amino acid are first dissolved in water to obtain an aqueous phase; the aqueous phase is added to sunflower oil glycerides, and the mixture is stirred at a speed of 300 rpm for 10 minutes during the addition process. The system is observed to be in a yellow gel state, thereby obtaining a nanoemulsifier;
[0060] (2) Add the phase A materials into a stirred tank and stir with a blade-shaped stirring paddle at a speed of 250 rpm for 5 minutes to ensure uniform mixing, then heat to 60-75°C and stir until phase A is completely dissolved and mixed uniformly;
[0061] (3) Heat the phase B material to 60-75°C and slowly add it to the phase A. Observe the system until it changes from liquid to gel and finally to liquid. Stir at a speed of 200 rpm to obtain a mixture 1.
[0062] (3) After the C phase material is evenly dissolved, the mixture is kept at 60-75°C and added to the mixture 1. After addition, the mixture is stirred at 300 rpm for 10 min, then homogenized at 11000 rpm for 4 min, and then cooled to 45°C to obtain the mixture 2;
[0063] (4) Add phase D in the formula to mixture 2, stir at a speed of 600 rpm for 4 minutes, stir evenly, cool, and discharge to obtain a nanoemulsion composition.
[0064] Comparative Example 14
[0065] The comparative example of the present invention provides a nanoemulsion composition, wherein the only difference between the nanoemulsion composition and Example 1 is that soybean glycerides are used instead of sunflower oil glycerides.
[0066] Comparative Example 15
[0067] The comparative example of the present invention provides a nanoemulsion composition, wherein the only difference between the nanoemulsion composition and Example 1 is that sodium lauroyl glutamate is used instead of sodium stearoyl glutamate.
[0068] Comparative Example 16
[0069] The comparative example of the present invention provides a nanoemulsion composition, wherein the only difference between the nanoemulsion composition and Example 1 is that sodium lauroyl oat amino acids are used instead of potassium lauroyl wheat amino acids.
[0070] Effect example
[0071] The effect examples of the present invention verify the performance of the nanoemulsion compositions prepared by Examples 1-3 and Comparative Examples 1-16, including the following aspects:
[0072] 1. Particle size test of nanoemulsion composition
[0073] (1) Test method: Dynamic light scattering technology is used to measure the average particle size of particles in the serum;
[0074] (2) Index description: Dynamic Light Scattering (DLS) is an effective method for measuring the particle size and distribution of submicron and nanoparticles. The particles in the dispersion system are subject to Brownian motion. DLS measures the Brownian motion of particles in the dispersion system and is used to determine the hydrodynamic size of the particles. The rate of Brownian motion can be quantified by the translational diffusion coefficient, usually represented by D. In a dispersion system, smaller particles diffuse faster and larger particles diffuse slower. Since the particles to be measured may have different shapes and the surface of the particles may be bound to other substances, such as ions or polymers, the shape of the particles to be measured is generally equivalent to a sphere with the same diffusion rate, and the diameter of the sphere is used as the hydrodynamic size of the particle.
[0075] (3) Test results: The particle size test results of the nanoemulsion compositions prepared in Examples 1-3 and Comparative Examples 1-16 after emulsification and standing for 48 hours are shown in Tables 3 and Figure 1-2 As shown, Figure 1 The particle size test results of Examples 1-3 are as follows: Figure 2 The particle size test results of Comparative Examples 1-16 are shown below:
[0076] Table 3
[0077] Group Particle size / nm Group Particle size / nm Example 1 95.86 Comparative Example 9 1423 Example 2 50.55 Comparative Example 10 622.4 Example 3 56.95 Comparative Example 11 299.5 Comparative Example 1 48.17 Comparative Example 12 218.5 Comparative Example 2 784.2 Comparative Example 13 43.44 Comparative Example 3 142.6 Comparative Example 14 326.7 Comparative Example 4 146.9 Comparative Example 15 214.1 Comparative Example 5 102.6 Comparative Example 16 254.5 Comparative Example 6 156.5 Comparative Example 7 222.7 Comparative Example 8 118.3
[0078] As can be seen from Table 3, the particle size of the nanoemulsion composition prepared by the technical solution of the present invention is moderate, ranging from 50.55 to 95.86 nm;
[0079] It can be seen from Example 2 and Comparative Example 2 that when the nanoemulsifier is missing, the nano-sized nanoemulsion composition cannot be prepared; it can be seen from Example 2 and Comparative Examples 4-7 that when the mass ratio of the nanoemulsifier, ammonium acryloyldimethyltaurate / VP copolymer and sodium mannose phosphate is not within the range given by the present invention, the particle size of the obtained nanoemulsion composition also shows an upward trend; it can be seen from Example 2 and Comparative Example 8 that when the mass percentage of the composition capable of stabilizing the nanoemulsion added to the nanoemulsion composition is too much, the particle size of the obtained product shows an upward trend; it can be seen from Example 2 and Comparative Example 9 that when the nanoemulsion When the mass percentage of the composition capable of stabilizing the nanoemulsion added to the composition is too small, a nano-sized product cannot be prepared; it can be seen from Example 2 and Comparative Examples 10-12 that when any one of the nanoemulsifier, ammonium acryloyldimethyltaurate / VP copolymer and sodium mannose phosphate is replaced by other components, the particle size of the obtained product shows a significant upward trend; it can be seen from Example 2 and Comparative Examples 14-16 that the sunflower seed oil glycerides, sodium stearoyl glutamate and lauroyl wheat amino acid potassium in the nanoemulsifier can achieve excellent synergistic effects, and when other analogs are used as substitutes, products with good particle sizes cannot be obtained.
[0080] 2. Stability test
[0081] Test method: Test according to T / GDCQMA 002-2023 "Cosmetic Stability Test Specification" issued by the Guangdong Cosmetics Quality Management Association in the National Group Standard Information Platform. The nanoemulsion compositions prepared in Examples 1-3 and Comparative Examples 1-16 were placed at 25°C, 5°C, -18°C, and 50°C, respectively, and stability tests were performed for 0 days, 5 days, 10 days, 20 days, and 30 days under light conditions; the stability test results are shown in Table 4 below;
[0082] Table 4
[0083]
[0084]
[0085]
[0086]
[0087] Note: The stability of the test results is indicated as follows: stable test results are ++, slightly stable test results are +, relatively poor stability is -, and poor stability is - ( ++ is normal, + is slightly coarse, - is slightly oily, - is demulsified and stratified ) .
[0088] It can be seen from the results in Table 4 above that the nanoemulsion composition prepared by the technical solution of the present invention has excellent high temperature, low temperature, light and room temperature stability, and will not delaminate or demulsify when placed under various conditions for 30 days. It can be seen from the data of Example 2 and Comparative Example 1 that, without the addition of ammonium acryloyldimethyltaurate / VP copolymer, although a nanostructure with a smaller particle size can be made, its stability has demulsified and delaminated at high or low temperatures; it can be seen from Example 2 and Comparative Example 2 that when no nanoemulsifier is added, Table 3 shows that an emulsion product with a nanostructure cannot be prepared. Although the finished product can be stable for several days, due to the absence of an emulsifier, surface oil floating has already appeared on the fifth day. It can be analyzed from the data of Comparative Example 3 that without the addition of sodium mannose phosphate, its stability is good in the early stage, but demulsification and demulsification begin to appear on the tenth day, and the product cannot be stable for a long time;
[0089] It can be seen from Example 2 and Comparative Examples 4-6 that when the weight percentage of a single raw material in the system increases, the system will become unstable; Comparative Example 7 changes the mass ratio between the nanoemulsifier, ammonium acryloyldimethyltaurate / VP copolymer and sodium mannose phosphate, and the stability of the obtained product also shows a downward trend;
[0090] It can be seen from Example 2 and Comparative Examples 8-9 that when the mass percentage of the composition capable of stabilizing the nanoemulsion added to the nanoemulsion composition is too low or too high, the stability of the obtained product shows a certain downward trend;
[0091] It can be seen from Example 2 and Comparative Examples 10-12 that when other substances are used to replace the nanoemulsifier, ammonium acryloyldimethyltaurate / VP copolymer and sodium mannose phosphate, the stability of the obtained products shows a certain downward trend, and it can be seen from Table 3 that the particle size of the obtained products is relatively large;
[0092] It can be seen from Example 2 and Comparative Examples 14-16 that when the components in the nanoemulsifier are changed alone or not added, a product with excellent stability cannot be obtained.
[0093] 3. Closed patch irritation test
[0094] Test method: refer to the 2015 edition of the Cosmetic Safety Technical Specifications, select qualified spot test equipment, place about 0.020g-0.025g of the test substance in the patch device, apply the patch device with the test substance to the back of the subject with a low-allergenic tape, and gently press it with the palm of your hand to evenly apply it to the skin for 24 hours. Observe the skin reaction according to the standards in Table 5 0.5h (after the indentation disappears), 24h and 48h after removing the test substance patch tester and record the observation results. The products prepared by Examples 1-3 and Comparative Example 13 were tested, with a total of 30 valid subjects, and the subjects were in good health.
[0095] The test standards are shown in Table 5 below:
[0096] Table 5
[0097]
[0098] The results obtained are shown in Table 6;
[0099] Table 6
[0100]
[0101] As shown in Table 6 above, Comparative Example 13 has a certain irritation, while Examples 1-3 are relatively mild. The conventional nanoemulsifier polyglycerol-3 methyl glucose distearate is used to prepare a nanoemulsion with a smaller particle size, but the amount of the nanoemulsifier is much greater than that of Example 2, and a high concentration of the nanoemulsifier will have a greater irritation to human skin. The nanoemulsifier of the present application can achieve a stable emulsification effect at a low concentration while having a low irritation to the human body.
[0102] Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention rather than to limit the scope of protection of the present invention. Although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solution of the present invention can be modified or replaced by equivalents without departing from the essence and scope of the technical solution of the present invention.
Claims
1. A composition capable of stabilizing a nanoemulsion, characterized in that: The composition capable of stabilizing the nanoemulsion comprises the following components in parts by weight: 0.5-1.5 parts of ammonium acryloyldimethyltaurate / VP copolymer, 0.5-1.0 parts of sodium mannose phosphate, and 5-10 parts of a nanoemulsifier; The nanoemulsifier comprises water, sunflower oil glycerides, sodium stearoyl glutamate and lauroyl wheat amino acid potassium; in the nanoemulsifier, the mass ratio of water, sunflower oil glycerides, sodium stearoyl glutamate and lauroyl wheat amino acid potassium is 40:30:18:
12.
2. The composition capable of stabilizing nanoemulsion according to claim 1, characterized in that: The preparation method of the nanoemulsifier comprises the following steps: (1) dissolving sodium stearoyl glutamate and potassium lauroyl wheat amino acid in water to obtain an aqueous phase; (2) Add the aqueous phase to the sunflower oil glycerides, maintain a stirring speed of 250-350 rpm during the addition process, and stir for 8-12 minutes after the addition is completed to obtain a nanoemulsifier.
3. Use of the composition capable of stabilizing nanoemulsion according to any one of claims 1 to 2 in the preparation of a nanoemulsion composition.
4. A nanoemulsion composition, characterized in that The nanoemulsion composition comprises the composition capable of stabilizing nanoemulsion according to any one of claims 1 to 2.
5. The nanoemulsion composition according to claim 4, characterized in that The nanoemulsion composition also includes an emollient, a moisturizer, an antioxidant, and a chelating agent.
6. The nanoemulsion composition according to claim 5, characterized in that The nanoemulsion composition comprises the following components in mass percentage: 5-15% of the composition capable of stabilizing the nanoemulsion according to any one of claims 1 to 2, 1-10% of an emollient, 2-10% of a moisturizer, 0.1-1% of an antioxidant, 0.01-0.1% of a chelating agent, and the balance of water.
7. The nanoemulsion composition according to claim 6, characterized in that The emollient comprises at least one of octyl polymethylsiloxane and isononyl isononanoate; And / or, the humectant includes at least one of glycerol, 1,2-hexanediol, and butylene glycol; and / or, the antioxidant comprises p-hydroxyacetophenone; And / or, the chelating agent comprises EDTA-disodium.
8. The method for preparing the nanoemulsion composition according to any one of claims 4 to 7, characterized in that: The preparation method comprises the following steps: (1) Mix the materials of phase A and stir at 200-300 rpm for 4-6 minutes, then heat to 60-75°C; (2) Mix the materials of phase B and heat them to 60-75° C., then add them to the phase A in step (1), and stir at a speed of 150-300 rpm until the system changes from a gel state to a liquid state, to obtain a mixture 1; (3) Mix the materials of phase C and heat them to 60-75° C., then add them to the mixture 1 in step (2), stir them at a speed of 300-350 rpm for 8-12 min, then homogenize them at a speed of 10000-12000 rpm for 3-5 min, and then cool them to 40-45° C. to obtain a mixture 2; (4) adding the phase D material to the mixture 2 of step (3) and stirring at a speed of 500-800 rpm for 3-5 minutes to obtain a nanoemulsion composition; The phase A material is a nanoemulsifier and an emollient; the phase B material is part of water; the phase C material is a moisturizer, a chelating agent, an antioxidant, ammonium acryloyldimethyltaurate / VP copolymer and the remaining water; and the phase D is sodium mannose phosphate.
9. Use of the nanoemulsion composition according to any one of claims 4 to 7 in the preparation of skin care products.
Citation Information
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