A sunscreen composition, method of making and use thereof
Patent Information
- Application Number
- CN202611324042.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-08-28
- Publication Date
- 2026-10-30
AI Technical Summary
但是这些现有技术均未解决上述技术问题,防晒产品的防护性能仍有待提升
(1)本发明采用酯类油脂作为油脂增效剂(尤其优选癸二酸二乙基己酯),其对多种化学防晒剂具有优良的溶解能力,能使防晒剂稳定溶解于油相中,避免结晶析出,充分发挥防晒剂的紫外线吸收效率;实施例表明,本发明在SPF 10、SPF 30和SPF 50体系中均表现出最高的SPF实测值和最优的光稳定性,且全面满足欧盟UVA防护标准;
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Figure CN122997980A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of daily cosmetics technology, and in particular to a sunscreen composition, its preparation method, and its application. Background Technology
[0002] With increasing awareness of UV protection, sunscreen cosmetics have become an essential part of daily skincare. Currently, commercially available sunscreens primarily achieve their protective effect by adding organic UV absorbers (chemical sunscreens) or inorganic UV blockers (physical sunscreens). Chemical sunscreens, in particular, are widely used in various sunscreen formulations due to their advantages such as low dosage, high sun protection efficiency, and lightweight feel. However, chemical sunscreens are mostly oil-soluble active ingredients, and their solubility and dispersion uniformity in the formulation directly determine the final sun protection efficacy (SPF / PFA value), photostability, and skin feel of the sunscreen product. Therefore, how to construct a reasonable oil system to fully dissolve and stably carry chemical sunscreens has always been a core technical challenge in sunscreen product development.
[0003] In existing technologies, chemical sunscreen agents in sunscreen compositions often fail to achieve an ideal solubility in the formulation system. When sunscreen agents cannot be fully dissolved, they are prone to recrystallization during storage or use, resulting in an uneven sunscreen film and a significantly lower actual sun protection effect than the theoretical design value, failing to fully utilize their UV absorption efficiency. Furthermore, incompletely dissolved sunscreen particles can cause a rough skin feel, whitening after application, and other unpleasant experiences, even affecting the overall stability and safety of the formulation. Chinese invention patent application CN115463054A discloses a sunscreen composition and its preparation method. By using fine-grained inorganic sunscreen powder and organopolysiloxanes with polyglycerol segments in the sunscreen composition, combined with high-pressure microfluidic homogenization treatment, the problems of oil production, sedimentation, and excessive viscosity in the sunscreen composition are solved, achieving stable suspension and highly effective sun protection. Chinese invention patent CN117064781A discloses a safe and gentle sunscreen composition and its application. This composition, using an ethanol-free water-in-oil sunscreen with macromolecular chemical sunscreens and ingredients such as lauroyl lysine, solves the problems of heavy texture and toxicity associated with existing sunscreens, achieving a highly effective and gentle sun protection effect suitable for sensitive skin. However, these existing technologies have not solved the aforementioned technical problems, and the protective performance of sunscreen products still needs improvement.
[0004] Against this backdrop, there is an urgent need to develop a solution that can balance sun protection performance, formula stability, and skin feel, so that sunscreen agents can fully exert their intended protective performance. Summary of the Invention
[0005] To address the aforementioned technical problems, the first aspect of this invention provides a sunscreen composition, wherein the raw materials for preparing the sunscreen composition, by weight percentage, include: 0.5-15% oil synergist, 1-30% sunscreen agent, 1-10% moisturizer, 0.5-12% emollient, 1-5% emulsifier, and the remainder being solvent.
[0006] Optionally, the oil synergist is selected from at least one of diethylhexyl sebacate, dibutyl adipate, diisopropyl sebacate, dibutyl sebacate, diethyl sebacate, dibutyloctyl sebacate, dibutyloctyl sebacate, diisopropyl adipate, diisooctyl adipate, diisobutyl adipate, dibutyl adipate, butanediol dioctanoate / didecanoate, C12-15 alcohol benzoate, and phenethyl benzoate.
[0007] Optionally, the oil synergist is selected from diethylhexyl sebacate; the amount of diethylhexyl sebacate added to the sunscreen composition is 0.8-13%.
[0008] Optionally, the raw materials for preparing the sunscreen composition, by weight percentage, include: Phase A: Chelating agent 0-0.2%, humectant 1-10%, thickener 0-0.5%, solvent replenishment balance; Phase B: Oil enhancer 0.5-15%, sunscreen 1-30%, emollient 0.5-2%, emulsifier 1-5%; Phase C: pH adjuster 0.1-2%, preservative 0.1-1%.
[0009] Optionally, the sunscreen agent includes at least two of the following: bis-ethylhexyloxyphenol methoxyphenyl triazine, diethylaminohydroxybenzoyl hexyl benzoate, ethylhexyl methoxycinnamate, ethylhexyl triazine ketone, ethylhexyl salicylate, butyl methoxydibenzoylmethane, benzophenone-3, bis-ethylhexyloxyphenol methoxyphenyl triazine, butyl methoxydibenzoylmethane, diethylaminohydroxybenzoyl hexyl benzoate, diethylhexylbutamidotriazine ketone, ethylhexyl triazine ketone, and methylene bis-benzotriazolyltetramethylbutylphenol.
[0010] Optionally, the softener includes at least one of cetearyl alcohol ethylhexanoate, ethylhexyl palmitate, polydimethylsiloxane, cetearyl alcohol, or the following.
[0011] Optionally, the emulsifier includes glyceryl stearate, cetearyl alcohol, sodium lauroyl glutamate, and sodium stearoyl lactylate.
[0012] Optionally, the moisturizer includes one or more of the following: glycerin, propylene glycol, 1,3-butanediol, dipropylene glycol, sorbitol, sodium PCA, sodium lactate, sodium hyaluronate, hydrolyzed hyaluronic acid, acetylated hyaluronic acid, trehalose, betaine, panthenol, erythritol, xylitol, mannitol, fructose, glucose, sucrose, maltitol, polyethylene glycol, tremella polysaccharide, β-glucan, hydroxyethyl urea, ceramide, and allantoin.
[0013] Optionally, the thickener includes one or more of the following: carbomer, acrylate / C10-30 alkanol acrylate crosspolymer, polyacrylate, ammonium acryloyl dimethyl taurate / VP copolymer, hydroxyethyl acrylate / sodium acryloyl dimethyl taurate copolymer, sodium polyacrylate, xanthan gum, hydroxyethyl cellulose, hydroxypropyl methyl cellulose, sodium carboxymethyl cellulose, microcrystalline cellulose, cellulose gum, hydroxypropyl starch phosphate, aluminum octenyl succinate of starch, sodium alginate, carrageenan, gellan gum, pectin, gum arabic, and guar gum.
[0014] A second aspect of the present invention provides a method for preparing the sunscreen composition as described above, wherein the preparation steps of the sunscreen composition include: mixing the raw materials for preparing the sunscreen composition evenly to obtain the final product.
[0015] A third aspect of the present invention provides an application of the sunscreen composition as described above, said sunscreen composition being applied to creams, lotions, foundations, gels, sprays or mousses.
[0016] Beneficial effects: This invention provides a sunscreen composition, its preparation method, and its application, which have the following advantages: (1) The present invention uses ester oils as oil synergists (especially diethylhexyl sebacic acid), which has excellent solubility for a variety of chemical sunscreens, enabling the sunscreens to be stably dissolved in the oil phase, avoiding crystallization and precipitation, and fully utilizing the ultraviolet absorption efficiency of the sunscreens; the examples show that the present invention exhibits the highest measured SPF value and the best photostability in the SPF 10, SPF 30 and SPF 50 systems, and fully meets the EU UVA protection standards; (2) The ester oils used in this invention have a velvety soft touch, good spreadability, and no greasy residue. At the same time, they avoid the rough skin feel and whitening problem caused by undissolved sunscreen particles, so that the product has both high sun protection and a refreshing and silky user experience. (3) The present invention can be flexibly formulated into sunscreen products with multiple SPF values such as SPF 10, SPF 30, and SPF 50+ according to different usage scenarios, and can be widely used in various dosage forms such as creams, lotions, sprays, and gels to meet diverse needs; (4) The sunscreen composition of the present invention does not separate, precipitate or change color after being stored at 4°C, 45°C and room temperature for 3 months. The pH and viscosity remain stable and the micro-dispersion is uniform and fine, and it has good temperature resistance and storage stability. (5) The preparation method of the present invention is simple, requires no harsh conditions, is compatible with the existing sunscreen product production process, can be directly used to achieve large-scale production, and is highly operable. Attached Figure Description
[0017] Figure 1 Results of the oil-soluble capacity test; Figure 2 Results of microscopic stability evaluation of sunscreen composition formulations in Examples 1-4. Detailed Implementation
[0018] The first aspect of the present invention provides a sunscreen composition, wherein the raw materials for preparing the sunscreen composition, by weight percentage, include: 0.5-15% oil synergist, 1-30% sunscreen agent, 1-10% moisturizer, 0.5-12% emollient, 1-5% emulsifier, and the balance being solvent.
[0019] The dosage of the oil synergist can be listed as 0.5wt%, 0.6wt%, 0.7wt%, 0.8wt%, 0.9wt%, 1wt%, 2wt%, 2.5wt%, 3wt%, 3.5wt%, 4wt%, 4.5wt%, 5wt%, 5.5wt%, 6wt%, 6.5wt%, 7wt%, 7.5wt%, 8wt%, 8.5wt%, 9wt%, 9.5wt%, 10wt%, 10.5wt%, 11wt%, 11.5wt%, 12wt%, 12.5wt%, 13wt%, 14wt%, 15wt%, etc.
[0020] Optionally, the oil synergist is selected from at least one of diethylhexyl sebacate, dibutyl adipate, diisopropyl sebacate, dibutyl sebacate, diethyl sebacate, dibutyloctyl sebacate, dibutyloctyl sebacate, diisopropyl adipate, diisooctyl adipate, diisobutyl adipate, dibutyl adipate, butanediol dioctanoate / didecanoate, C12-15 alcohol benzoate, and phenethyl benzoate.
[0021] Optionally, the oil synergist is selected from diethylhexyl sebacate; the amount of diethylhexyl sebacate added to the sunscreen composition is 0.8-13%.
[0022] To address the technical problems in existing sunscreen compositions where chemical sunscreen agents are insufficiently dissolved in conventional oil systems, leading to recrystallization and precipitation during storage and / or use, significantly lower actual sun protection efficacy (especially SPF value) than theoretically designed values, poor photostability, and unpleasant application and skin feel, this invention employs specific ester oils (especially diethylhexyl sebate) as oil synergists in combination with sunscreen agents. This results in sunscreen compositions with high sun protection efficiency and excellent photostability. The reason for this is speculated to be that the ester oils described in this invention contain one or more ester bonds (-COO-) in their molecular structure. These ester bonds have strong polarity, enabling intermolecular forces (such as dipole-dipole interactions and transient dipole induction) to form with chemical sunscreen molecules that also possess a certain degree of polarity. This results in excellent solubility of the chemical sunscreen agents, making the sunscreen composition more effective. It can stably dissolve in the oil system at the molecular level, avoiding crystallization and uneven sunscreen film caused by insufficient solubility. In particular, the diethylhexyl sebacate molecule contains two ester bonds and has a moderate carbon chain length, which is highly compatible with the molecular structures of various chemical sunscreens (such as bis-ethylhexyloxyphenol methoxyphenyl triazine, diethylaminohydroxybenzoyl hexyl benzoate, ethylhexyl methoxycinnamate, and ethylhexyl triazine ketone). This provides sufficiently strong intermolecular attraction, allowing the sunscreen to remain completely dissolved even at high concentrations. This ensures that the sunscreen is stably and uniformly dispersed in the oil phase, forming a continuous and dense sunscreen film after application to the skin, significantly improving the measured SPF value and its retention rate after sun exposure. At the same time, the stable solubility also avoids the adverse effects of undissolved sunscreen particles on the skin feel, giving the product a good user experience.
[0023] In some embodiments, the raw materials for preparing the sunscreen composition, by weight percentage, include: Phase A: Chelating agent 0-0.2%, humectant 1-10%, thickener 0-0.5%, solvent replenishment balance; Phase B: Oil enhancer 0.5-15%, sunscreen 1-30%, emollient 0.5-2%, emulsifier 1-5%; Phase C: pH adjuster 0.1-2%, preservative 0.1-1%.
[0024] In some embodiments, the chelating agent may include disodium EDTA, octanoyl hydroxamic acid, tetrasodium glutamate diacetate, etc.; further options include disodium EDTA.
[0025] In some embodiments, the moisturizer may include glycerin, propylene glycol, 1,3-butanediol, dipropylene glycol, sorbitol, sodium PCA, sodium lactate, sodium hyaluronate, hydrolyzed hyaluronic acid, acetylated hyaluronic acid, trehalose, betaine, panthenol, erythritol, xylitol, mannitol, fructose, glucose, sucrose, maltitol, polyethylene glycol, tremella polysaccharide, β-glucan, hydroxyethyl urea, ceramide, allantoin, etc.; further options include glycerin.
[0026] In some embodiments, the thickener may include carbomer, acrylate / C10-30 alkanol acrylate crosspolymers, polyacrylates, ammonium acryloyl dimethyl taurate / VP copolymers, hydroxyethyl acrylate / sodium acryloyl dimethyl taurate copolymers, sodium polyacrylate, xanthan gum, hydroxyethyl cellulose, hydroxypropyl methyl cellulose, sodium carboxymethyl cellulose, microcrystalline cellulose, cellulose gum, hydroxypropyl starch phosphate, aluminum octenyl succinate of starch, sodium alginate, carrageenan, gellan gum, pectin, gum arabic, guar gum, etc.; further options include carbomer.
[0027] In some embodiments, phase A may also contain 0-2% anionic emulsifier, such as potassium cetyl phosphate, sodium stearoyl lactylate, sodium stearoyl lactylate, sodium cetearyl sulfate, sodium stearoyl glutamate, C20-22 alkyl phosphate, etc.; further options include potassium cetyl phosphate.
[0028] In some embodiments, the sunscreen agent may include bis-ethylhexyloxyphenol methoxyphenyl triazine, hexyl diethylaminohydroxybenzoylbenzoate, ethylhexyl methoxycinnamate, ethylhexyl triazine ketone, butyl methoxydibenzoylmethane, octocrylene, humosasulfate, ethylhexyl salicylate, benzophenones, dimethyl PABA ethylhexyl ketone, phenylbenzimidazole sulfonic acid, terephthalimide dicamphor sulfonic acid, cresoltrazolium trisiloxane, methylene bis-benzotriazolyl tetramethylbutylphenol, diethylhexylbutamidotriazine ketone, sinoxalate, disodium phenyl dibenzimidazole tetrachloroester, p-methoxycinnamate, etc.
[0029] Further selectable from at least two of bis-ethylhexyloxyphenol methoxyphenyl triazine, diethylaminohydroxybenzoyl hexyl benzoate, ethylhexyl methoxycinnamate, ethylhexyl triazine ketone, ethylhexyl salicylate, butyl methoxydibenzoylmethane, benzophenone-3, bis-ethylhexyloxyphenol methoxyphenyl triazine, butyl methoxydibenzoylmethane, diethylaminohydroxybenzoyl hexyl benzoate, diethylhexylbutamidotriazine ketone, ethylhexyl triazine ketone, and methylene bis-benzotriazolyltetramethylbutylphenol.
[0030] Further optionally, the sunscreen agent includes bis-ethylhexyloxyphenol methoxyphenyl triazine, hexyl diethylaminohydroxybenzoyl benzoate, ethylhexyl methoxycinnamate, and ethylhexyl triazine ketone; wherein the mass ratio of bis-ethylhexyloxyphenol methoxyphenyl triazine, hexyl diethylaminohydroxybenzoyl benzoate, ethylhexyl methoxycinnamate, and ethylhexyl triazine ketone is (1.0-2.5):(3.0-4.5):(4-8):(2-4).
[0031] Further optionally, the sunscreen agent includes ethylhexyl salicylate, butyl methoxydibenzoylmethane, ethylhexyl methoxycinnamate, and ethylhexyl triazine ketone; wherein the mass ratio of ethylhexyl salicylate, butyl methoxydibenzoylmethane, ethylhexyl methoxycinnamate, and ethylhexyl triazine ketone is (3.0-6.0):(2.0-5.5):(4-12):(2-5).
[0032] Further optionally, the sunscreen agent includes hexyl diethylaminohydroxybenzoylbenzoate, bis-ethylhexyloxyphenol methoxyphenyl triazine, and ethylhexyl methoxycinnamate; the mass ratio of hexyl diethylaminohydroxybenzoylbenzoate, bis-ethylhexyloxyphenol methoxyphenyl triazine, and ethylhexyl methoxycinnamate is (1.0-4.0):(0.5-2.5):(2-6).
[0033] In some embodiments, the emollient may include cetearyl alcohol ethylhexanoate, ethylhexyl palmitate, polydimethylsiloxane, cetearyl alcohol, isononyl isononanoate, squalane, caprylic / capric triglyceride, isopropyl myristate, isooctyl palmitate, butylene glycol dicaprylic / capric didecanoate, decyl oleate, sucrose tetraisostearate, glyceryl caprylate, hydrogenated coconut oil, polydimethylsiloxane / vinyl polydimethylsiloxane crosspolymer, phenyltrimethylsiloxane, stearoxypolymethoxysiloxane / polydimethylsiloxane copolymer, polydimethylsiloxane alcohol, diphenylsiloxyphenyl polytrimethylsiloxane, tris(octyldodecyl)citrate, isohexadecane, cetyl palmitate, cocoyl caprylate, isocetyl stearyloxy stearate, argan oil polyglycerol-6 Esters, hydrogenated vegetable oils, avocado oil, castor oil, jojoba oil, coconut oil, almond oil, olive oil, sesame oil, perilla seed oil, oat kernel oil, mineral oil, petrolatum, lanolin, etc.; further, at least one of cetearyl alcohol ethylhexanoate, ethylhexyl palmitate, polydimethylsiloxane, and cetearyl alcohol may be selected.
[0034] Further optionally, the mass ratio of ethylhexyl palmitate, polydimethylsiloxane and cetearyl alcohol is (1.0-3.0):(0.5-1.5):(0.1-1).
[0035] In some embodiments, the emulsifier may include glyceryl stearate / cetearearyl alcohol / sodium lauroyl glutamate / sodium stearoyl lactylate, stearyl alcohol polyether-2, stearyl alcohol polyether-21, oleyl alcohol polyether-10, PEG-100 stearate, cetearyl alcohol polyether-20, methyl glucose sesquistearate, sucrose polystearate (and) hydrogenated polyisobutylene, polyglycerol-3 diisostearate, polyglycerol-2 dihydroxystearate, polyglycerol-10 Stearates, sorbitan olive oil esters, cetearyl olive oil esters, hydrogenated lecithin, lecithin, cetyl polyethylene glycol / polypropylene glycol-10 / 1 dimethylsiloxane, bis-PEG / PPG-14 / 14 dimethylsiloxane, methoxy PEG / PPG-25 / 4 dimethylsiloxane, etc.; further optionally, a mixture of glyceryl stearate, cetearyl alcohol, sodium lauroyl glutamate and sodium stearoyl lactylate.
[0036] In some embodiments, the preservative may include phenoxyethanol, sodium benzoate, benzoic acid, sorbic acid, benzyl alcohol, dehydroacetic acid, salicylic acid, chlorphenesin, methylparaben, ethylparaben, propylparaben, butylparaben, potassium sorbate, benzalkonium chloride, methylisothiazolinone, etc.; it may also be selected from phenoxyethanol.
[0037] In some embodiments, the pH adjuster may include sodium hydroxide, lactic acid, citric acid, sodium citrate, triethanolamine, tromethamine, potassium hydroxide, phosphoric acid, tartaric acid, sodium dihydrogen phosphate, gluconolactone, sodium lactate, etc.; further, it may be selected from sodium hydroxide and / or lactic acid.
[0038] The present invention does not impose any particular limitation on the solvent, such as water.
[0039] The present invention may also add skin conditioning agents, antioxidants, film-forming agents, colorants, fragrances, skin feel modifiers, cooling agents, anti-inflammatory agents, defoamers, solubilizers, cosolvents, dispersants, fillers, propellants (applicable to spray products), etc., according to the application needs of the sunscreen composition; all of the above auxiliary ingredients can be selected and combined according to the actual dosage form (such as lotion, cream, spray, gel, etc.) and the expected use scenario. Those skilled in the art can determine their types and dosages through conventional experiments, without any particular limitation.
[0040] A second aspect of the present invention provides a method for preparing a sunscreen composition, wherein the preparation steps of the sunscreen composition include: mixing the raw materials for preparing the sunscreen composition evenly to obtain the sunscreen composition.
[0041] In some embodiments, the preparation steps of the sunscreen composition include: S1. Weigh the A phase raw material, stir until completely dissolved, heat to 70-85℃ to obtain liquid one; S2. Weigh the B phase raw material, heat it to 70-85℃, and stir until completely dissolved to obtain liquid two; S3. Add liquid 2 to liquid 1, stir and homogenize, and cool to below 65℃ to obtain liquid 3; S4. Add the C phase raw material to the liquid solution, cool it to below 40°C, stir evenly, and obtain the sunscreen composition.
[0042] In some embodiments, the raw materials for preparing the sunscreen composition may further include phase D and / or more phase components (e.g., but not limited to fragrances, pigments, antioxidants, active extracts, etc.). Those skilled in the art can independently separate the corresponding components into phases according to actual formulation needs and add them in any suitable step of the preparation method. For example, phase D can be added to the liquid and stirred evenly after cooling to below 40°C in step S4. The number of phases involved in the preparation steps of the sunscreen composition and the order of addition of the corresponding components can be adaptively adjusted according to the actual formulation composition and are not particularly limited.
[0043] A third aspect of the present invention provides an application of a sunscreen composition, said sunscreen composition being used in creams, lotions, foundations, gels, sprays or mousses.
[0044] The following describes embodiments of this application. The embodiments described below are exemplary and are only used to explain this application, and should not be construed as limiting this application. Where specific techniques or conditions are not specified in the embodiments, they are performed according to the techniques or conditions described in the literature in this field or according to the product instructions. Reagents or instruments used, unless otherwise specified, are all conventional products that can be obtained commercially.
[0045] The diethylhexyl sebacate used in the following implementation examples is all from ZSI, model ZETEMOL OSB.
[0046] Example 1 This embodiment provides a sunscreen composition and its preparation method. The formulation of the sunscreen composition by mass percentage is shown in Table 1.
[0047] Table 1
[0048] The emulsifier is a mixture of glyceryl stearate, cetearyl alcohol, sodium lauroyl glutamate, and sodium stearoyl lactylate, which is derived from ZSI and is designated as PROTELAN NMF. The formula of this raw material by mass percentage is: 45-75% glyceryl stearate, 30-50% cetearyl alcohol, 5-15% sodium lauroyl glutamate, and 5-10% sodium stearoyl lactylate.
[0049] The preservative is a mixture of phenoxyethanol and octyl glycol, derived from Roelmi, and is marketed as BioscontrolSynergy PCG.
[0050] The preparation steps of the sunscreen composition include: S1. Weigh the raw material of phase A, stir until completely dissolved, and heat to 80°C to obtain liquid one; S2. Weigh the B phase raw material, heat it to 80℃, and stir until it is completely dissolved to obtain liquid two; S3. Add liquid 2 to liquid 1, stir and homogenize, and cool to 65℃ to obtain liquid 3; S4. Add the C phase raw material to the third solution (where pH adjuster is added sequentially to adjust to the target pH), cool to room temperature, stir evenly, and obtain the sunscreen composition (the dosage form is a cream).
[0051] Examples 2-4 Examples 2-4 each provide a sunscreen composition, with the specific implementation method being the same as in Example 1; the difference lies in the different oil synergists, as detailed in Table 2.
[0052] Table 2
[0053] Example 5 This embodiment provides a sunscreen composition and its preparation method. The formulation of the sunscreen composition by mass percentage is shown in Table 3.
[0054] Table 3
[0055] The emulsifier is a mixture of glyceryl stearate, cetearyl alcohol, sodium lauroyl glutamate, and sodium stearoyl lactylate, which is derived from ZSI and is designated as PROTELAN NMF. The formula of this raw material by mass percentage is: 45-75% glyceryl stearate, 30-50% cetearyl alcohol, 5-15% sodium lauroyl glutamate, and 5-10% sodium stearoyl lactylate.
[0056] The preservative is a mixture of phenoxyethanol and octyl glycol, derived from Roelmi, and is marketed as BioscontrolSynergy PCG.
[0057] The softener, polydimethylsiloxane, is sourced from Evonik and is designated Abil 350.
[0058] The preparation steps of the sunscreen composition include: S1. Weigh the A phase raw material, heat it to 75°C with slow stirring until it is dissolved and homogeneous to obtain liquid one; S2. Weigh the B phase raw material, heat it to 75℃ and stir until completely dissolved to obtain liquid two; S3. Add liquid 2 to liquid 1 and homogenize under vacuum for 5 minutes to obtain liquid 3; S4. Cool the third liquid to 45°C, add the C phase raw material to the third liquid, and homogenize under vacuum for 2 minutes to obtain the fourth liquid. S5. Cool the fourth liquid to 40°C, add the D phase raw material to the fourth liquid, homogenize under vacuum for 2 minutes, stir slowly and cool to room temperature to obtain the sunscreen composition.
[0059] Example 6 This embodiment provides a sunscreen composition and its preparation method. The formulation of the sunscreen composition by mass percentage is shown in Table 5.
[0060] Table 5
[0061] The emulsifier is a mixture of glyceryl stearate, cetearyl alcohol, sodium lauroyl glutamate, and sodium stearoyl lactylate, which is derived from ZSI and is designated as PROTELAN NMF. The formula of this raw material by mass percentage is: 45-75% glyceryl stearate, 30-50% cetearyl alcohol, 5-15% sodium lauroyl glutamate, and 5-10% sodium stearoyl lactylate.
[0062] The preparation steps of the sunscreen composition include: S1. Weigh the A phase raw material, heat it to 75°C with slow stirring until it is dissolved and homogeneous to obtain liquid one; S2. Weigh the B phase raw material, heat it to 75℃ and stir until completely dissolved to obtain liquid two; S3. Add liquid 2 to liquid 1 and homogenize under vacuum for 5 minutes to obtain liquid 3; S4. Weigh the C phase raw material, heat it to 75°C with slow stirring to dissolve it evenly, and obtain liquid four; S5. Add liquid four to liquid three, and homogenize under vacuum for 2 minutes to obtain liquid five; S6. Cool liquid five to 30°C, add phase D raw material to liquid five, stir slowly and cool to room temperature to obtain sunscreen composition.
[0063] Comparative Example 1 The specific implementation method is the same as in Example 5; the difference is that diethylhexyl sebacate (ZETEMOL OSB) is replaced with dibutyl adipate (CETIOL B) of the same concentration.
[0064] Comparative Example 2 The specific implementation method is the same as in Example 5; the difference is that diethylhexyl sebacate ZETEMOL OSB is replaced with phenethyl benzoate X-TEND 226 of the same concentration.
[0065] Comparative Example 3 The specific implementation method is the same as in Example 6; the difference is that diethylhexyl sebacate (ZETEMOL OSB) is replaced with dibutyl adipate (CETIOL B) of the same concentration.
[0066] Comparative Example 4 The specific implementation method is the same as in Example 6; the difference is that diethylhexyl sebacate ZETEMOL OSB is replaced with phenethyl benzoate X-TEND 226 of the same concentration.
[0067] Performance testing 1. Oil and fat dissolving ability Various oils (ZETEMOL 99 isononanoate, ZETEMOL 2IS isostearate, ZETEMOL OSB diethylhexyl sebacate, CETIOL B dibutyl adipate, CETIOL AB C12-15 benzoate, X-TEND 226 phenoxyethyl octanoate, TEGOSOFT XC, and MINERAL OIL) were tested for their solubility in different sunscreen agents (Tinosorb S bis-ethylhexyloxyphenol methoxyphenyl triazine, Uvinul A Plus diethylaminohydroxybenzoyl hexyl benzoate, Uvinul T 150 ethylhexyl triazine, and BMDM butyl methoxydibenzoylmethane). The test temperature was 25℃, and three parallel samples were set up for each sample, and the average value was taken. The test results are shown in […]. Figure 1 .
[0068] Figure 1 The results showed that ester oils exhibited varying degrees of solubility for several chemical sunscreens. Among them, diethylhexyl sebacate (ZETEMOL OSB), dibutyl adipate (CETIOL B), C12-15 benzoate (CETIOL AB), and phenethyl benzoate (X-TEND 226) showed better solubility for sunscreens. In particular, diethylhexyl sebacate (ZETEMOL OSB) and dibutyl adipate (CETIOL B) demonstrated excellent solubility for all four sunscreens.
[0069] 2. Sun protection performance The sunscreens from Examples 1-7 were used for sun protection factor (SPF) testing. The tests were conducted according to European Commission Technical Recommendation 2006 / 647 / EC, using standardized in vitro testing methods to accurately characterize the product's UV protection capability and photostability. The specific testing procedure is as follows: (1) Preparation of test carrier: Polymethyl methacrylate (PMMA) plate with a specific surface roughness (e.g., 6μm) is selected as the test substrate to simulate human skin. The texture of real human skin is simulated by a special roughness plate surface to ensure that the test environment is consistent with the actual use scenario and to avoid the interference of substrate differences on the test results. (2) Quantitative coating of the test samples: The quantitative sunscreen product was uniformly coated on the surface of the PMMA plate using an automatic precision coating device. The coating amount of the sample was controlled at 1.0mg / cm²-1.2mg / cm² to simulate the actual state of consumers applying sunscreen products in daily life, and to ensure that the coating thickness and amount of each sample were uniform. (3) Detecting initial UV absorbance and calculating initial sun protection factor: The PMMA plate coated with sun protection film was tested for full-band UV absorbance using a spectrophotometer. The detection bands covered UVB (290nm-320nm) and UVA (320nm-400nm). The initial in vitro SPF value of the product was calculated by collecting the initial absorbance data. (4) Simulated solar irradiation treatment: Based on the initial in vitro SPF value of the product under test, the matching exclusive ultraviolet irradiation dose is calculated, and then the sun protection film on the surface of the PMMA plate is irradiated in a directional manner through a solar simulator to accurately simulate the natural light environment during the actual use of the product, thereby assessing the photostability of the sun protection product and the sun protection agent system. (5) Testing and comprehensive evaluation of performance after irradiation: After the irradiation is completed, the ultraviolet absorbance of the sunscreen film is tested again using a spectrophotometer. By comparing the absorbance data of the whole band before and after irradiation, the final in vitro SPF value of the product can be accurately calculated. At the same time, based on the data change pattern, it can be determined whether the sunscreen agent in the formula has photodegradation phenomenon, and the comprehensive evaluation of the sun protection performance and photostability of the product can be completed.
[0070] This testing method uses the coefficient of variation (CoV) to evaluate the repeatability and reliability of the test data. The formula for calculating the coefficient of variation is: CoV = standard deviation / mean × 100% (n=5). In the in vitro sunscreen testing system, CoV is used to quantify the consistency of test results for the same formula on different PMMA test plates. A lower CoV value indicates smaller differences between parallel test samples, better test repeatability, and higher reliability of the test data; a higher CoV value indicates greater fluctuations in test data across different test plates, and poorer test stability and data accuracy. The coefficients of variation for all test samples in this invention are at a low level, indicating that the test data in this group has low dispersion, excellent repeatability, and high stability and reliability, effectively and objectively reflecting the true sunscreen performance of the formula; the test results are shown in Table 6.
[0071] The EU standard (2006 / 647 / CE) stipulates that the SPF label value / UVA protection factor must be less than 3 and the critical wavelength must be greater than 370nm.
[0072] Table 6
[0073] As shown in Table 6, in the SPF 30 system, the sunscreen composition containing only ZETEMOL OSB had an SPF label value / UVA protection factor ratio of less than 3 before and after light exposure, fully meeting EU standards (2006 / 647 / CE). In contrast, the CETIOLB, CETIOL AB, and X-TEND 226 formulations in Examples 2-4 all failed one of these tests before or after light exposure. Furthermore, the in vitro SPF value (52.47 before light exposure, 48.62 after light exposure) and retention rate (92.7%) of the ZETEMOLOSB formulation were significantly better than the other three oils (Examples 2-4). In the SPF 10 and SPF 50 systems, its measured SPF value was also the highest in its group and exhibited the least degradation after light exposure. In addition, its excellent solubility and microdispersibility against various chemical sunscreens indicate that ZETEMOL... OSB (diethylhexyl sebacate) is a preferred oil-based carrier for ensuring that sunscreen compositions have high sun protection efficiency, excellent photostability, and compliance with EU regulations.
[0074] 3. Stability The sunscreen compositions of Examples 1-6 were placed at 4°C, 45°C, and room temperature (25°C) for 3 months respectively, and their stability was evaluated. The results showed that none of the samples in each example exhibited unstable phenomena such as stratification, precipitation, or discoloration after long-term storage, indicating that the sunscreen compositions of the present invention have good stability under the above temperature conditions.
[0075] Table 7
[0076] Figure 2 The results shown are those of Examples 1-4 after being stored at room temperature for 3 months, observed under an optical microscope at 40x magnification. The results show that no sunscreen crystallization, oil droplet aggregation, or phase separation was observed in any of the four oil systems. The dispersed phase was uniformly distributed, exhibiting good microscopic stability. Among them, the formulation using Zetemol OSB (diethylhexyl sebacate) had smaller droplet size and a more delicate and uniform distribution, resulting in the best overall dispersion effect.
Claims
1. A sunscreen composition, characterized in that, The raw materials for preparing the sunscreen composition, by weight percentage, include: 0.5-15% oil synergist, 1-30% sunscreen agent, 1-10% moisturizer, 0.5-12% emollient, 1-5% emulsifier, and the balance being solvent; The oil synergist is selected from at least one of the following: diethylhexyl sebacate, dibutyl adipate, diisopropyl sebacate, dibutyl sebacate, diethyl sebacate, dibutyloctyl sebacate, dibutyloctyl sebacate, diisopropyl adipate, diisooctyl adipate, diisobutyl adipate, dibutyl adipate, butanediol dioctanoate / didecanoate, C12-15 alcohol benzoate, and phenethyl benzoate.
2. The sunscreen composition according to claim 1, characterized in that, The oil synergist is selected from diethylhexyl sebacate; the amount of diethylhexyl sebacate added to the sunscreen composition is 0.8-13%.
3. The sunscreen composition according to claim 1, characterized in that, The raw materials for preparing the sunscreen composition, by weight percentage, include: Phase A: Chelating agent 0-0.2%, humectant 1-10%, thickener 0-0.5%, solvent replenishment balance; Phase B: Oil enhancer 0.5-15%, sunscreen 1-30%, emollient 0.5-2%, emulsifier 1-5%; Phase C: pH adjuster 0.1-2%, preservative 0.1-1%.
4. The sunscreen composition according to claim 1, characterized in that, The sunscreen agent comprises at least two of the following: bis-ethylhexyloxyphenol methoxyphenyl triazine, diethylaminohydroxybenzoyl hexyl benzoate, ethylhexyl methoxycinnamate, ethylhexyl triazine ketone, ethylhexyl salicylate, butyl methoxydibenzoylmethane, benzophenone-3, bis-ethylhexyloxyphenol methoxyphenyl triazine, butyl methoxydibenzoylmethane, diethylaminohydroxybenzoyl hexyl benzoate, diethylhexylbutamidotriazine ketone, ethylhexyl triazine ketone, and methylene bis-benzotriazolyltetramethylbutylphenol.
5. The sunscreen composition according to claim 3, characterized in that, The softener includes at least one of cetearyl alcohol ethylhexanoate, ethylhexyl palmitate, polydimethylsiloxane, and cetearyl alcohol.
6. The sunscreen composition according to claim 1, characterized in that, The emulsifiers include glyceryl stearate, cetearyl alcohol, sodium lauroyl glutamate, and sodium stearoyl lactylate.
7. The sunscreen composition according to claim 1, characterized in that, The moisturizer includes one or more of the following: glycerin, propylene glycol, 1,3-butanediol, dipropylene glycol, sorbitol, sodium PCA, sodium lactate, sodium hyaluronate, hydrolyzed hyaluronic acid, acetylated hyaluronic acid, trehalose, betaine, panthenol, erythritol, xylitol, mannitol, fructose, glucose, sucrose, maltitol, polyethylene glycol, tremella polysaccharide, β-glucan, hydroxyethyl urea, ceramide, and allantoin.
8. The sunscreen composition according to claim 1, characterized in that, The thickener includes one or more of the following: carbomer, acrylate / C10-30 alkanol acrylate crosspolymer, polyacrylate, ammonium acryloyl dimethyl taurate / VP copolymer, hydroxyethyl acrylate / sodium acryloyl dimethyl taurate copolymer, sodium polyacrylate, xanthan gum, hydroxyethyl cellulose, hydroxypropyl methyl cellulose, sodium carboxymethyl cellulose, microcrystalline cellulose, cellulose gum, hydroxypropyl starch phosphate, aluminum octenyl succinate of starch, sodium alginate, carrageenan, gellan gum, pectin, gum arabic, and guar gum.
9. A method for preparing a sunscreen composition according to any one of claims 1-8, characterized in that, The preparation steps of the sunscreen composition include: mixing the raw materials for preparing the sunscreen composition evenly to obtain the final product.
10. The application of a sunscreen composition according to any one of claims 1-8, characterized in that, The sunscreen composition is applied in creams, lotions, foundations, gels, sprays, or mousses.
Citation Information
Patent Citations
Sunscreen composition and preparation method thereof
CN115463054A
Safe and mild sunscreen composition and application thereof
CN117064781A
