Composition and application thereof in preparation of product with sunscreen effect
By scientifically combining surface-modified zinc oxide and titanium dioxide complex with chemical sunscreens, along with specific solvents and repairing ingredients, the problems of white residue, skin irritation, and environmental risks associated with traditional sunscreens have been solved, achieving highly efficient and stable sun protection and repair functions.
Patent Information
- Application Number
- CN202511036255.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-07-26
- Publication Date
- 2025-11-07
AI Technical Summary
Existing sunscreen products suffer from problems such as white residue, skin irritation, environmental risks, limited sun protection mechanisms, limited formulations, and insufficient repair functions.
A complex of surface-modified zinc oxide and titanium dioxide, along with chemical sunscreens such as diethylaminobenzoyl benzoate, ethylhexyl triazine, and bis-ethylhexylphenol methoxyphenyl triazine, were combined with isododecane and butanediol solvents. Ingredients including diethylhexyl naphthaleneate, photolyase, collagen, and β-1,3-glucan were added. Bisabolol microcapsules and asiaticoside inclusion complexes were prepared via spray drying, optimizing the extraction of Pueraria lobata extract.
It achieves broad-spectrum sun protection, improves the dispersion stability and skin feel of sunscreen ingredients, enhances the product's environmental friendliness, provides repair and antioxidant functions, and is suitable for long-term use.
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Abstract
Description
TECHNICAL FIELD
[0001] The present application belongs to the technical field of sunscreen products, and particularly relates to a composition and application thereof in the preparation of products with sunscreen effect. BACKGROUND
[0002] Sunscreen products are an important part of daily skincare, mainly used to prevent the damage of ultraviolet rays to the skin. Traditional sunscreen creams mainly rely on single or simple compounding of chemical sunscreen agents and physical sunscreen agents, such as physical sunscreen agents such as zinc oxide and titanium dioxide, or chemical sunscreen agents such as oxybenzone and avobenzone. However, these traditional formulas have obvious defects: physical sunscreen agents such as zinc oxide and titanium dioxide are prone to form white residues on the surface of the skin, affecting the appearance; chemical sunscreen agents can cause skin allergy or irritation, and long-term use also has environmental accumulation risks. In addition, the sunscreen mechanism of existing sunscreen products is relatively single, relying only on physical shielding or only on chemical absorption, and it is difficult to balance high protection effect and use comfort.
[0003] In the prior art, some products attempt to improve the skin feel by nanoizing physical sunscreen agents, such as reducing the particle size of zinc oxide to the nanometer level to reduce white marks. However, the dispersion stability of nano particles is poor, and they are prone to agglomeration, resulting in uneven sunscreen effect. Some products add multiple chemical sunscreen agents to broaden the protection band, but the compounding of chemical sunscreen agents can cause interactions between components, reducing stability. For example, avobenzone is prone to degradation when mixed with certain ultraviolet absorbers, and the sunscreen effect quickly decays over time. In addition, traditional sunscreen products often ignore the repair function and cannot cope with the oxidative stress and inflammatory response caused by ultraviolet rays, resulting in damage to the skin barrier.
[0004] Another problem of existing sunscreen products is the limitation of dosage form. Although the water-in-oil system can improve water resistance, it has a strong greasy feeling and is not suitable for daily use; the water-based formula is refreshing, but the sunscreen ingredients are prone to volatilization and need to be frequently re-applied. In addition, most products do not consider environmental friendliness, and the use of silicone oil components is difficult to degrade and poses a potential risk to aquatic ecosystems.
[0005] Therefore, it is necessary to design a composition and application thereof in the preparation of products with sunscreen effect. SUMMARY
[0006] In order to overcome the defects in the prior art, a composition and application thereof in the preparation of products with sunscreen effect are provided.
[0007] In order to achieve the above-mentioned purpose, the present application provides the following technical solutions: A composition, the composition comprising the following components by weight percentage: physical sunscreen agent 5-25%, chemical sunscreen agent 1-15%, and solvent in the rest amount. The physical sunscreen agent is at least one of zinc oxide or titanium dioxide; the chemical sunscreen agent comprises diethylamino hydroxybenzoyl hexyl benzoate, ethylhexyl triazone, bis-ethylhexyl phenol methoxyphenyl triazine, the solvent is a mixture of isododecane and butylene glycol, and the volume ratio of the isododecane to butylene glycol is 1:1-3.
[0008] The physical sunscreen agent is a compound of surface-modified zinc oxide and titanium dioxide, and the mass ratio of the surface-modified zinc oxide to titanium dioxide is 1:0.5-2.
[0009] The preparation method of the surface-modified zinc oxide is as follows: a wet chemical precipitation method is used, 0.1-0.3 mol / L zinc nitrate solution and 0.4-0.6 mol / L ammonium bicarbonate solution are reacted in a constant-temperature water bath at 92-98℃ for 6-10 hours to generate an alkali zinc carbonate precursor, the precursor is washed by centrifugation and calcined at 400-500℃ for 3-5 hours to obtain a zinc oxide crude product; then the zinc oxide crude product is dispersed in isododecane, 2-4% polydimethylsiloxane based on the mass of the zinc oxide crude product is added, and stirring is carried out at 50-70℃ for 1-3 hours to obtain the surface-modified zinc oxide.
[0010] The chemical sunscreen agent is a compound of diethylamino hydroxybenzoyl hexyl benzoate, ethylhexyl triazone and bis-ethylhexyl phenol methoxyphenyl triazine, and the mass ratio of diethylamino hydroxybenzoyl hexyl benzoate, ethylhexyl triazone and bis-ethylhexyl phenol methoxyphenyl triazine is 1:0.8-1.2:0.8-1.2.
[0011] The composition further comprises diethylhexyl naphthalate 3-7%, photolyase 3-5%, collagen 3-5%, β-1.3 glucan 0.3-0.5%, a repairing agent 0.1-5%, an oxidizing agent 0.01-1%, an emulsifying agent 0.1-3%, plant extract 0.05-2%, the repairing agent is at least one of hydroxyl asiatic acid and its ester inclusion compound or bisabolol microcapsule, the antioxidant is at least one of tocopherol or ammonium glycyrrhizate, the emulsifying agent is at least one of cetyl PEG / PPG-10 / 1 dimethicone or PEG-30 dipolyhydroxystearate, and the plant extract is wild kudzu root extract.
[0012] The preparation method of the hydroxyl asiatic acid and its ester inclusion compound is as follows: hydroxyl asiatic acid and its ester and β-cyclodextrin are dissolved in ethanol according to a molar ratio of 1:1.5-3, and reaction is carried out at 50-60℃ for 3-5 hours to obtain the inclusion compound after freeze-drying.
[0013] The preparation method of the bisabolol microcapsule is as follows: bisabolol is used as a core material, and polymethylsilsesquioxane is used as a wall material, and the mass ratio of bisabolol to polymethylsilsesquioxane is 1:0.4-0.6. Dissolve the core material, bisabolol, in sunflower seed oil to form an oil solution with a mass concentration of 0.3-0.6%, and dissolve the wall material, polymethylsilsesquioxane, and the emulsifier, sodium dodecyl sulfonate, in water to form a homogeneous aqueous solution with a wall material concentration of 8-15% and an emulsifier concentration of 3-5%; Slowly add the oil solution into the aqueous solution, and use a high-shear emulsifier to shear at 25000-28000 rpm for 3-5 minutes to form a stable emulsion with a particle size of 10-20 microns, and the emulsification temperature is controlled below 60 DEG C to obtain an emulsion; Use a spray drying method to spray dry the emulsion to obtain bisabolol microcapsules.
[0014] The spray drying parameters are as follows: the inlet temperature is 170-180 DEG C, the feeding rate is 20 mL / min, the outlet temperature is 70-80 DEG C, and the atomization pressure is 0.2-0.4 MPa.
[0015] The extraction method of the wild kudzu root extract is as follows: dry wild kudzu root is crushed to 60 mesh, and the obtained wild kudzu root powder is refluxed with an ethanol-water mixed solvent at 60-80 DEG C for 4-8 hours, and the solid-liquid ratio is 1:5-10 to obtain an extract; the extract is concentrated to a paste under reduced pressure at 55-60 DEG C and under a pressure of-0.1 MPa, and then purified by a macroporous resin to obtain a wild kudzu root extract.
[0016] The composition is used for preparing a product with sunscreen effect.
[0017] Compared with the prior art, the advantages and beneficial effects of the present application are as follows: 1. The composition of the present application realizes a broad-spectrum sunscreen effect by scientific compounding of physical sunscreen agents and chemical sunscreen agents, and can block UVA and UVB band ultraviolet rays at the same time. In terms of physical sunscreen, surface modified zinc oxide is compounded with titanium dioxide, and the surface of the zinc oxide is coated with polydimethylsiloxane through a specific modification process. This treatment not only solves the white mark problem of traditional physical sunscreen agents, but also significantly improves the dispersion stability of the particles.
[0018] 2. The surface modification process of the zinc oxide in the present application uses polydimethylsiloxane coating to significantly improve the dispersibility and stability of the zinc oxide, and solves the technical problem of easy agglomeration of nanoparticles. The reaction temperature and calcination temperature are accurately controlled during the modification process to ensure that zinc oxide with an ideal crystal structure is obtained. After compounding with titanium dioxide at a mass ratio of 1:0.5-2, the two components can cover a wider ultraviolet band and provide more comprehensive protection effect.
[0019] 3. The chemical sunscreen system of the present application selects a compound of diethylaminohydroxybenzoyl hexyl benzoate, ethylhexyl triazone, and bis-ethylhexyl phenol methoxyphenyl triazine. Through synergistic effect, high-efficiency broad-spectrum sunscreen is achieved. Diethylaminohydroxybenzoyl hexyl benzoate is specially used for UVA band, especially with significant absorption peak at 354 nm, strong light stability and not easy to react with other ingredients, which can effectively prevent photoaging. Ethylhexyl triazone is used for UVB band with absorption rate of 310 nm peak, light and thin texture and low cost. Bis-ethylhexyl phenol methoxyphenyl triazine is used as a broad-spectrum sunscreen, covering UVA and UVB at the same time, with absorption peaks at 310 nm and 340 nm, excellent light stability, and large molecular weight, not easy to penetrate the skin, and high safety. The combination has light and thin skin feel and high protection efficiency of chemical sunscreen, balancing performance and safety.
[0020] 4. The solvent system of the present application uses a mixture of isododecane and butylene glycol with a volume ratio of 1:1-3. This ratio ensures the solubility of sunscreen ingredients and improves the skin feel of the product, solving the problems of greasiness of traditional water-in-oil systems and volatility of water-based formulations. Isododecane, as a volatile silicone oil substitute, has better environmental friendliness, reducing the potential risk of traditional silicone oil to aquatic ecosystems. The addition of butylene glycol enhances the moisturizing performance of the product, making the sunscreen product have skin care efficacy.
[0021] 5. The hydroxyl asiaticoside inclusion complex is prepared by β-cyclodextrin inclusion technology, which significantly improves the stability and bioavailability of the active ingredient. The farnesol is microencapsulated by polymethylsilsesquioxane, with a coating rate of more than 90%. The spray drying process parameters are optimized, with an inlet temperature of 170-180°C and an outlet temperature of 70-80°C, which ensures the integrity of the microcapsules and avoids the degradation of the active ingredient. The synergistic effect of the two repair ingredients can effectively alleviate the skin inflammation and oxidative stress caused by ultraviolet rays, realizing the integration of sunscreen and repair.
[0022] 6. The antioxidant system of the present application selects tocopherol or ammonium glycyrrhizinate with an addition amount of 0.01-1%. This concentration range can effectively scavenge free radicals without affecting the stability of the formula.
[0023] 7. The emulsifier uses cetyl PEG / PPG-10 / 1 dimethicone or PEG-30 dipolyhydroxystearate with an addition amount of 0.1-3%, which ensures the stability and good spreadability of the formula.
[0024] 8. The wild kudzu root extract is obtained by optimizing the extraction process, using 60-80°C reflux extraction for 4-8 hours with a solid-liquid ratio of 1:5-10, and then purified by macroporous resin. The flavonoid content in the extract is high, with significant antioxidant and anti-inflammatory effects.
[0025] 9. The addition of diethylhexyl naphthalate, photolyase, collagen and beta-1, 3-glucan in sunscreen not only provides physical and chemical complex sunscreen, but also achieves the trinity effect of "protection-repair-nourishment" through bioactive ingredients, suitable for sensitive skin and anti-aging needs. Diethylhexyl naphthalate can absorb ultraviolet rays and provide skin protection, combined with photolyase to repair ultraviolet-induced DNA damage and reduce the risk of photoaging. Photolyase directly repairs DNA damage through a light-activated mechanism, while collagen supplements skin structural proteins, improves elasticity and reduces collagen degradation caused by ultraviolet rays, and beta-1, 3-glucan reduces inflammatory factors and enhances skin barrier function through antioxidant and immunomodulatory effects. Collagen and beta-1, 3-glucan together enhance moisturizing performance and relieve post-sun dryness, while the immunomodulatory ability of glucan can reduce erythema and edema induced by ultraviolet rays.
[0026] 10. The entire formulation system is carefully designed, and the components synergize with each other. Physical sunscreen provides immediate protection, chemical sunscreen supplements blind areas, repair ingredients prevent photodamage, antioxidant system against free radicals, forming a multi-level protection network. The product not only has a long-lasting and stable sunscreen effect, with high SPF and PA values, but also has good skin feel and safety, suitable for long-term daily use. DETAILED DESCRIPTION
[0027] The technical solutions in the embodiments of the present application will be described below in a clear and complete manner. Obviously, the described embodiments are only some of the embodiments of the present application, not all. Based on the embodiments in the present application, all other embodiments obtained by those of ordinary skill in the art without creative labor fall within the scope of the present application.
[0028] In this application, the sources of various raw materials are briefly described as follows: Polymethylsilsesquioxane: purchased from Momentive Performance Materials, model MK. Zinc oxide: Z-COTE HP1 produced by BASF, Germany. Titanium dioxide: purchased from Covestro Chemicals, model TIO2 P25, anatase type. Butyl methoxydibenzoylmethane purchased from Beichu Chang Biomedicine Technology Co., Ltd., model Shield Biso-A PLUS. Ethylhexyl triazone purchased from Wuhan Mayceer Chemical Co., Ltd., model Escalol 557. Bis-ethylhexyl phenol methoxyphenyl triazine purchased from Hubei Hongfuda Biological Technology Co., Ltd., model Tinosorb S. Isododecane: ISOPAR L from Arkema, France, solvent grade, boiling point range 180-210℃. Butylene glycol: 1,3-butylene glycol from Mitsubishi Chemical, Japan, purity 99.5%, cosmetic grade. Diethylhexyl 2,6-naphtalene dicarboxylate purchased from Symrise, model Corapan®TQ. Collagen and photolyase purchased from Peptide Source Biotech (Guangzhou) Co., Ltd. β-1,3-glucan purchased from Puliwei Biomedicine, water-soluble natural yeast β-glucan, CAS: 160872-27-5. Asiaticoside: provided by Sabinsa Corporation, India, standard extract, purity more than 90%. Farnesol: produced by Symrise, Germany, natural source, purity 99%. β-cyclodextrin: purchased from Binzhou Zhihui Biological Technology, Shandong, food grade, purity 98%. Sodium lauryl sulfonate: STEPANOL WA-EXTRA from Dow Chemical, USA, emulsifier grade. Sunflower seed oil: refined product from Sophia Group, France, cosmetic grade, acid value less than 0.5 mg / g. Tocopherol: mixed tocopherol provided by DSM, Netherlands, purity 96%. Ammonium glycyrrhizate: standard pharmaceutical grade from Maruzen Pharmaceutical Co., Ltd., Japan, purity 98%. Ceteth-10-PEG / PPG-10 / 1 dimethicone: SILSOFT 074 from Momentive Performance Materials, USA. PEG-30 dipolyhydroxystearate: ARLACEL P135 produced by Croda, UK.
[0029] A composition comprising the following components in weight percentage: physical sunscreen 5-25%, chemical sunscreen 1-15%, solvent the rest; The physical sunscreen is at least one of zinc oxide or titanium dioxide; the chemical sunscreen comprises butyl methoxydibenzoylmethane, ethylhexyl triazone, bis-ethylhexyl phenol methoxyphenyl triazine, and the solvent is a mixture of isododecane and butylene glycol in a volume ratio of 1:1-3.
[0030] The physical sunscreen is a complex of surface-modified zinc oxide and titanium dioxide in a mass ratio of 1:0.5-2.
[0031] The surface-modified zinc oxide is prepared by the following method: 0.1-0.3 mol / L zinc nitrate solution and 0.4-0.6 mol / L ammonium bicarbonate solution are reacted in a 92-98℃ constant-temperature water bath for 6-10 hours to form a basic zinc carbonate precursor, which is washed by centrifugation and calcined at 400-500℃ for 3-5 hours to obtain a crude zinc oxide; then the obtained crude zinc oxide is dispersed in isododecane, 2-4% polydimethylsiloxane based on the mass of the crude zinc oxide is added, and stirring is carried out at 50-70℃ for 1-3 hours to obtain the surface-modified zinc oxide.
[0032] The chemical sunscreen agent is a complex of diethylaminohydroybenzoyl hexyl benzoate, ethylhexyl triazone and bis-ethylhexyl phenol methoxyphenyl triazine, and the mass ratio of diethylaminohydroybenzoyl hexyl benzoate, ethylhexyl triazone and bis-ethylhexyl phenol methoxyphenyl triazine is 1:0.8-1.2:0.8-1.2.
[0033] The composition further comprises 3-7% diethylhexyl naphthalate, 3-5% photolyase, 3-5% collagen, 0.3-0.5% β-1.3 glucan, 0.1-5% repair agent, 0.01-1% oxidizing agent, 0.1-3% emulsifier, 0.05-2% plant extract, the repair agent is at least one of hydroxyl asiatic acid glycoside inclusion compound or bisabolol microcapsule, the antioxidant is at least one of tocopherol or ammonium glycyrrhizate, the emulsifier is at least one of cetyl PEG / PPG-10 / 1 dimethicone or PEG-30 dipolyhydroxystearate, and the plant extract is kudzu root extract.
[0034] The preparation method of the hydroxyl asiatic acid glycoside inclusion compound is as follows: hydroxyl asiatic acid glycoside and β-cyclodextrin are dissolved in ethanol according to a molar ratio of 1:1.5-3, and the reaction is carried out at 50-60℃ for 3-5 hours, and the inclusion compound is obtained after freeze-drying.
[0035] The preparation method of the bisabolol microcapsule is as follows: bisabolol is used as the core material, and polymethylsilsesquioxane is used as the wall material, and the mass ratio of bisabolol to polymethylsilsesquioxane is 1:0.4-0.6; bisabolol is dissolved in sunflower seed oil to form an oil solution with a mass concentration of 0.3-0.6%, and polymethylsilsesquioxane and emulsifier sodium dodecyl sulfonate are dissolved in water to form a homogeneous aqueous solution, and the concentration of the wall material is 8-15% and the concentration of the emulsifier is 3-5%; The oil solution is slowly added into the aqueous solution, and a stable emulsion with a particle size of 10-20 μm is formed by shearing at 25000-28000 rpm for 3-5 minutes using a high-shear emulsifier, and the emulsification temperature is controlled below 60°C, to obtain an emulsion; The emulsion is spray-dried by a spray-drying method to obtain the farnesol microcapsule.
[0036] The spray-drying parameters are as follows: an inlet temperature of 170-180°C, a feeding rate of 20 mL / min, an outlet temperature of 70-80°C, and an atomization pressure of 0.2-0.4 MPa.
[0037] The extraction method of the Pueraria lobata extract is as follows: the dried Pueraria lobata is ground to 60 mesh, and the obtained Pueraria lobata powder is extracted with an ethanol-water mixed solvent at 60-80°C for 4-8 hours, and the solid-liquid ratio is 1:5-10, to obtain an extract; the extract is concentrated to a paste under reduced pressure at 55-60°C and at a pressure of-0.1 MPa, and then purified by a macroporous resin, to obtain the Pueraria lobata extract.
[0038] The technical solutions of the present application are further illustrated by the following examples and comparative examples, but the protection scope of the present application is not limited thereto.
[0039] Example 1 The composition of this example comprises: a physical sunscreen agent 25%, surface-modified zinc oxide and titanium dioxide with a mass ratio of 1:2. Modification process parameters: zinc nitrate 0.3 mol / L, ammonium bicarbonate 0.5 mol / L, reaction temperature 95°C, calcination temperature 400°C, and polydimethylsiloxane 2%. A chemical sunscreen agent 15%, and the mass ratio of diethylaminohydroxybenzoyl hexyl benzoate, ethylhexyl triazone, and bis-ethylhexyl phenol methoxyphenyl triazine is 1:1:1. The volume ratio of the solvents is 3:1. A repair agent 0.1%, the molar ratio of β-cyclodextrin to hydroxyl asiatic acid is 1.5:1. Diethylhexyl naphthalate 7%, photolyase 4%, collagen 3%, β-1.3 glucan 0.5%, antioxidant 1%, emulsifier 0.1%, and plant extract 2%. The core-to-wall ratio of farnesol microcapsules is 1:0.4, the spray-drying inlet temperature is 170°C, and the outlet temperature is 80°C.
[0040] Example 2 The composition of this example comprises: physical sunscreen 5%, mass ratio of zinc oxide to titanium dioxide 1:0.5. Modification parameters: zinc nitrate 0.1 mol / L, ammonium bicarbonate 0.6 mol / L, reaction temperature 92℃, calcination temperature 500℃, polydimethylsiloxane 4%. Chemical sunscreen 1%, mass ratio of diethylamino hydroxybenzoyl hexyl benzoate, ethylhexyl triazone, bis-ethylhexyl phenol methoxyphenyl triazine 1:0.8:1.2. Solvent volume ratio 1:1. Repair agent 5%, mass ratio of bisabolol to polymethylsilsesquioxane 1:0.6. Diethylhexyl naphthalate 5%, photolyase 3%, collagen 5%, β-1.3 glucan 0.4%, antioxidant 0.01%, emulsifier 3%, plant extract 0.05%. Spray drying inlet temperature 180℃, outlet temperature 70℃.
[0041] Example 3 The composition of this example comprises: physical sunscreen 15%, mass ratio 1:1. Modification parameters: zinc nitrate 0.2 mol / L, ammonium bicarbonate 0.4 mol / L, reaction temperature 98℃, calcination temperature 450℃, polydimethylsiloxane 3%. Chemical sunscreen 8%, wherein the mass ratio of diethylamino hydroxybenzoyl hexyl benzoate, ethylhexyl triazone, bis-ethylhexyl phenol methoxyphenyl triazine is 1:1.2:0.8. Solvent volume ratio 2:1. Diethylhexyl naphthalate 3%, photolyase 5%, collagen 4%, β-1.3 glucan 0.3%, repair agent 2.5%, molar ratio of β-cyclodextrin to hydroxyl asperosaponin 3:1. Antioxidant 0.5%, emulsifier 1.5%, plant extract 1%. Bisabolol microcapsule core wall ratio 1:0.5, spray drying inlet temperature 175℃, outlet temperature 75℃.
[0042] Comparative Example 1
[0043] In this example, the same as in Example 1, the differences are described as follows: using unmodified zinc oxide.
[0044] Comparative Example 2
[0045] In this example, the same as in Example 2, the differences are described as follows: only diethylamino hydroxybenzoyl hexyl benzoate is used.
[0046] Comparative Example 3
[0047] In this example, the same as in Example 3, the differences are described as follows: solvent volume ratio 1:4.
[0048] Comparative Example 4
[0049] In this example, the same as in Example 1, the differences are described as follows: using ordinary asperosaponin.
[0050] Comparative Example 5
[0051] In this embodiment, the similarities with Embodiment 2 will not be repeated, and the differences are as follows: only titanium dioxide is used.
[0052] Test Results and Analysis
[0053] The compositions obtained in the examples and comparative examples were subjected to performance tests to verify their effects, as shown in Table 1.
[0054] Table 1 Test Results
[0055] As shown in Table 1, the SPF and PA rating tests revealed that Examples 1-3 exhibited significantly better sun protection than all comparative examples. Example 3 achieved an SPF of 50.1, 21.8 higher than Comparative Example 3, primarily due to its scientifically balanced ratio of 15% intermediate content of physical sunscreen and 8% intermediate content of chemical sunscreen. Notably, Comparative Example 3's SPF plummeted to 28.3 due to an imbalanced solvent ratio (1:4), demonstrating that a 1:1-3 volume ratio of isododecane to butanediol is a crucial threshold for ensuring stable dispersion of the sunscreen ingredients. Regarding PA rating, Examples 1 and 3 both achieved ++++, while Comparative Example 5 only achieved ++, directly confirming the necessity of the zinc oxide and titanium dioxide combination for UVA protection.
[0056] In the white mark index test, all three examples remained within the excellent range of 1.0-1.5, while Comparative Example 1 soared to 4.8, and Comparative Example 2 was 2.3. Further analysis revealed that when using unmodified zinc oxide in Comparative Example 1, particle agglomeration was observed under a microscope, while in Example 1, after surface modification, the average particle size was 120 nm. This nanoscale dispersion significantly reduced visible light scattering. Example 3, by controlling the calcination temperature at a midpoint of 450°C, achieved a more regular zinc oxide crystal structure, further optimizing the white mark index to 1.0.
[0057] The water resistance test used a 40-minute water bath method. The retention rates of the sunscreen ingredients in Examples 1-3 were all greater than 88%, with Example 3 reaching the highest value of 94.0%. Comparative Example 3 had a retention rate of only 65.4%. Infrared spectroscopy analysis revealed that its solvent imbalance led to uneven distribution of the film-forming agent, resulting in obvious component dissolution peaks upon contact with water. Although Example 2 had the lowest physical sunscreen agent content (5%), it still maintained 88.3% water resistance through a precise 1:1 solvent ratio, indicating that the solvent system's regulatory effect on water resistance is greater than the absolute content of the sunscreen agent.
[0058] The repair effect test uses a UVB-induced erythema model, and Example 3 shows the best performance (70.2% reduction in erythema). Micro-CT shows that the β-cyclodextrin inclusion technology used by it increases the skin penetration rate of hydroxyl asiaticoside by 2.3 times. When Comparative Example 4 uses ordinary asiaticoside, the retention amount of the active ingredient in the stratum corneum is 47% lower than that of Example 1, which directly leads to a 14.6 percentage point decrease in repair effect. It is worth noting that although Example 2 has the highest repair agent content (5%), the core-to-wall ratio of the β-asarone microcapsule is at a maximum (1:0.6), and the insufficient thickness of the wall material leads to a decrease in sustained-release efficiency. The repair effect (62.1%) is actually lower than that of Example 3.
[0059] The present application realizes high-efficiency protection with an SPF value of 50.1 and a PA++++ by scientific compounding of physical and chemical sunscreens, optimization of surface modification process, and synergistic design of repair systems, while reducing the white mark index to 1.0, achieving a waterproofness of 94%, and improving the repair effect to 70.2%, thereby breaking through the technical bottlenecks of traditional sunscreen products in terms of protection effect, use experience, and function integration.
[0060] The above describes the preferred embodiments of the present application. It should be noted that for those skilled in the art, without departing from the principles of the present application, a number of improvements and refinements can be made, and these improvements and refinements should also be considered within the scope of protection of the present application.
Claims
1. A composition characterized in that, The composition comprises the following components in percentage by weight: physical sunscreen 5-25%, chemical sunscreen 1-15%, solvent balance; The physical sunscreen is at least one of zinc oxide or titanium dioxide; the chemical sunscreen comprises diethylamino hydroxybenzoyl hexyl benzoate, ethylhexyl triazone, bis-ethylhexyl phenol methoxyphenyl triazine, the solvent is a mixture of isododecane and butylene glycol, and the volume ratio of isododecane to butylene glycol is 1:1-3.
2. A composition according to claim 1, characterised in that: The physical sunscreen is a compound of surface-modified zinc oxide and titanium dioxide, and the mass ratio of the surface-modified zinc oxide to titanium dioxide is 1:0.5-2.
3. A composition according to claim 2, wherein, The preparation method of the surface-modified zinc oxide is as follows: a 0.1-0.3 mol / L zinc nitrate solution and a 0.4-0.6 mol / L ammonium bicarbonate solution are reacted in a constant-temperature water bath at 92-98℃ for 6-10 hours to generate a basic zinc carbonate precursor, the precursor is washed by centrifugation and calcined at 400-500℃ for 3-5 hours to obtain a zinc oxide crude product; then the zinc oxide crude product is dispersed in isododecane, 2-4% of polydimethylsiloxane based on the mass of the zinc oxide crude product is added, and stirring is carried out at 50-70℃ for 1-3 hours to obtain the surface-modified zinc oxide.
4. The composition of claim 1, wherein: The chemical sunscreen is a compound of diethylamino hydroxybenzoyl hexyl benzoate, ethylhexyl triazone and bis-ethylhexyl phenol methoxyphenyl triazine, and the mass ratio of diethylamino hydroxybenzoyl hexyl benzoate, ethylhexyl triazone and bis-ethylhexyl phenol methoxyphenyl triazine is 1:0.8-1.2:0.8-1.
2.
5. The composition of claim 1, wherein: The composition further comprises diethylhexyl naphthalate 3-7%, photolyase 3-5%, collagen 3-5%, β-1.3 glucan 0.3-0.5%, repair agent 0.1-5%, oxidizing agent 0.01-1%, emulsifier 0.1-3%, and plant extract 0.05-2%, the repair agent is at least one of hydroxyl asiatic acid glycoside inclusion compound or bisabolol microcapsule, the antioxidant is at least one of tocopherol or ammonium glycyrrhizate, the emulsifier is at least one of cetyl PEG / PPG-10 / 1 dimethicone or PEG-30 dipolyhydroxystearate, and the plant extract is kudzu root extract.
6. A composition according to claim 5, wherein: The preparation method of the hydroxyl asiatic acid glycoside inclusion compound is as follows: hydroxyl asiatic acid glycoside and β-cyclodextrin are dissolved in ethanol according to a molar ratio of 1:1.5-3, and the reaction is carried out at 50-60℃ for 3-5 hours, and the inclusion compound is obtained after freeze-drying.
7. A composition according to claim 5, wherein: The preparation method of the bisabolol microcapsule is as follows: bisabolol is used as the core material, and polymethylsilsesquioxane is used as the wall material, and the mass ratio of bisabolol to polymethylsilsesquioxane is 1:0.4-0.6; bisabolol is dissolved in sunflower seed oil to form an oil solution with a mass concentration of 0.3-0.6%, and polymethylsilsesquioxane and emulsifier sodium dodecyl sulfonate are dissolved in water to form a homogeneous aqueous solution, and the concentration of the wall material is 8-15% and the concentration of the emulsifier is 3-5%; The oil solution is slowly added into the water solution, and a stable emulsion with a particle size of 10-20 μm is formed by shearing at 25000-28000 rpm for 3-5 minutes using a high-shear emulsifier, and the emulsification temperature is controlled below 60°C, to obtain an emulsion; The emulsion is spray-dried to obtain the β-bisabolol microcapsule.
8. A composition according to claim 7, wherein: The spray-drying parameters are as follows: inlet temperature: 170-180°C, feeding rate: 20 mL / min, outlet temperature: 70-80°C, and atomization pressure: 0.2-0.4 MPa.
9. The composition of claim 5, wherein: The extraction method of the Pueraria lobata extract is as follows: the dried Pueraria lobata is ground to 60 mesh, and the obtained Pueraria lobata powder is extracted with an ethanol-water mixed solvent at 60-80°C for 4-8 hours, and the solid-liquid ratio is 1:5-10, to obtain an extract; the extract is concentrated to a paste under reduced pressure at 55-60°C and at a pressure of-0.1 MPa, and then purified by a macroporous resin, to obtain the Pueraria lobata extract.
10. Use of a composition according to any one of claims 1 to 9 for the manufacture of a product having a sunscreen effect, characterized in that: The composition is used for preparing a product with a sunscreen effect.