Sunscreen composition, sunscreen product as well as preparation method and application of sunscreen product

Abstract

The invention relates to the technical field of cosmetics, in particular to a sunscreen composition and a preparation method and application thereof. The sunscreen composition disclosed by the invention is prepared by adopting a specific emulsifier and a D-phase emulsification process, obtained particles are fine and uniform in granularity, and not only have excellent stability, but also can effectively improve the sunscreen efficiency of a sunscreen product, and has an obvious synergistic effect on the sunscreen effect; in addition, the use amount of a chemical sun-screening agent in a sun-screening product can be reduced, then the problem that the skin feeling of a high-magnification sun-screening product is greasy is solved, and the composition is suitable for preparing cosmetics with the sun-screening or light protection effect and has a good application prospect in the field of cosmetics.

Description

Technical Field

[0001] This invention relates to the field of cosmetic technology, and in particular to sunscreen compositions, sunscreen products, their preparation methods and applications. Background Technology

[0002] The spectral distribution of sunlight includes 3%–7% ultraviolet radiation (290–400 nm), 44% visible light (400–700 nm), and 53% infrared radiation (700–1440 nm). Ultraviolet, visible, and infrared light can all cause photoaging of the skin, inducing free radical production and oxidative stress, leading to photodamage. In recent years, ozone layer depletion has resulted in excessive global sun exposure, leading to a significant increase in skin diseases, and making sun protection a widespread concern.

[0003] The ultraviolet (UV) spectrum in sunlight ranges from 200 to 400 nm and can be divided into three bands: short-wave UVC (200-290 nm), medium-wave UVB (290-320 nm), and long-wave UVA (320-400 nm). UVA has strong penetrating power, reaching the dermis and damaging elastic and collagen fibers, causing tanning and wrinkles. UVB causes erythema; prolonged or excessive exposure leads to tanning, redness, and peeling. UVC has poor penetrating power, is almost completely absorbed by the ozone layer, and does not reach the ground, posing little harm to humans. Currently, sunscreens primarily protect against UVA and UVB rays, with SPF and PFA values ​​used to measure their effectiveness. Meeting high SPF requirements often requires layering multiple organic sunscreens, resulting in high concentrations and increasing the risk of skin irritation. Therefore, there is an urgent need to provide a sunscreen product that offers good sun protection while using a small amount of organic sunscreen agents.

[0004] The D-phase (surfactant phase) is a special phase state formed by surfactants, separating the oil phase (O) and the water phase (W). When the external conditions change, it easily undergoes a phase transition, forming a micro-O / W or W / O emulsion system. The key technical factor of D-phase emulsification is the special self-assembly structure of the D-phase and its emulsifying ability for the oil phase, because the surfactant arrangement in the D-phase is conducive to the formation of small oil droplets in the O / D phase. The rapid migration of surfactants to the oil-water interface is crucial for the preparation of nanoemulsions. Currently, this technology has been applied to skin care products, such as those for skin aging. For example, Chinese patent application 202410997359.4 discloses an anti-skin aging efficacy composition and its application in D-phase emulsified products. This composition is a blend of brown algae probiotic fermentation broth, collagen, adenosine, 1,3-butanediol, polysorbate-80, and fermentation products of *Candida beemannii* / glucose / rapeseed oleate. Experiments have shown that the components in the effective composition work synergistically to increase the content of type VII collagen, type XVI collagen, laminin 5, integrin a6, and antimicrobial peptides, thus exhibiting anti-wrinkle effects. Furthermore, this composition further promotes its penetration and absorption in D-phase emulsions, resulting in a stronger anti-aging effect. For example, Chinese patent application 202111169543.2 discloses a nanoemulsion with anti-wrinkle effects prepared using a D-phase emulsification method and its application. The nanoemulsion prepared by the D-phase emulsification method comprises the following components in the following mass percentages: PEG-55 propylene glycol oleate 0.5%–1.5%, C12-16 alkyl glucoside 0.5%–1.5%, oil 5%–15%, polyol 20%–30%, and water 55%–70%. This composition, obtained using modern extraction technology, inhibits matrix metalloproteinase activity, enhances skin elasticity, and prevents or even reduces the formation of fine lines.

[0005] There are currently no reports of applying D-phase emulsification technology to sunscreen formulations. This technological gap presents several unresolved challenges: Firstly, the photostability of sunscreens (especially organic sunscreens) and whether D-phase light exposure leads to emulsion demulsification or sunscreen degradation are not yet clear. Secondly, the precise control of SPF / PFA values ​​in sunscreen formulations and the matching mechanism between the amount of sunscreen encapsulated and the release rate in D-phase emulsification technology still require systematic exploration. These technological bottlenecks restrict the application and expansion of D-phase emulsification in the field of sunscreen. Summary of the Invention

[0006] In view of this, the present invention provides sunscreen compositions, sunscreen products, preparation methods thereof, and applications. The present invention utilizes D-phase emulsification combined with specific emulsifiers to prepare D-phase sunscreen formulations. Sunscreen products prepared using these D-phase sunscreen formulations exhibit good sun protection effects, require less chemical sunscreen agent, have high stability, are non-irritating to the skin, and have good safety.

[0007] The sunscreen composition, by weight, comprises the following ingredients:

[0008] Polyglycerol emulsifier: 5 to 15 parts;

[0009] Polyols: 10 to 20 parts;

[0010] Organic sunscreen agent: 24 to 40 parts;

[0011] The polyglycerol emulsifier comprises polyglycerol-10 oleate, or comprises polyglycerol-10 oleate and at least one of the following:

[0012] Polyglycerol-10 oleate and at least one of the following:

[0013] Polyglycerol-10 myristate, polyglycerol-10 stearate;

[0014] The organic sunscreen agent includes at least one of the following: cinnamic acid ester derivatives, salicylic acid ester derivatives, triazine derivatives, siloxane derivatives, benzoazole derivatives, dibenzoylmethane derivatives, p-aminobenzoic acid ester derivatives, benzo(methyl) ketone derivatives, and camphor derivatives.

[0015] The sunscreen composition of the present invention is prepared by a D-phase emulsification process.

[0016] In this invention, the polyglycerol emulsifier is either a single polyglycerol-10 oleate or a composite emulsifier containing polyglycerol-10 oleate. The composite emulsifier, in addition to polyglycerol-10 oleate, also includes polyglycerol-10 myristate and / or polyglycerol-10 stearate.

[0017] This invention is the first to utilize D-phase emulsification to readily formulate organic sunscreen agents into D-phase sunscreen compositions, which are then used as raw materials to prepare sunscreen products. This invention explored various types and combinations of emulsifiers, and the results showed that different emulsifiers directly affect the particle size and stability of the D-phase sunscreen composition. Specifically, polyglycerol-10 oleate alone or composite emulsifiers containing polyglycerol-10 oleate effectively improved the stability of the sunscreen composition. The combination of polyglycerol-10 oleate and polyglycerol-10 myristate, using less emulsifier, effectively improved the particle stability of the sunscreen composition, achieving the best results.

[0018] In the sunscreen composition of the present invention, the polyglycerol emulsifier is preferably 6 to 10 parts by weight, more preferably 7 to 10 parts. In some specific embodiments, it is specifically 7 parts, 8 parts, 9 parts, or 10 parts.

[0019] In the sunscreen composition of the present invention, the polyol is preferably 15 to 18 parts by mass, more preferably 16.5 to 18 parts by mass, and specifically 16.5, 17, 17.5 or 18 parts.

[0020] In the sunscreen composition of the present invention, the organic sunscreen agent is preferably 24 to 30 parts or 30 to 40 parts by weight; some specific embodiments may contain 24 parts, 26 parts, 28 parts, 30 parts, 32 parts or 34 parts.

[0021] In some embodiments, the polyglycerol emulsifier is composed of polyglycerol-10 oleate and polyglycerol-10 myristate. Further, the mass ratio of polyglycerol-10 oleate to polyglycerol-10 myristate is (5–10):(0.5–3), preferably (5–7.5):(0.5–3). In some specific embodiments, the mass ratio is 7.5:0.5 or 5:3.

[0022] In some embodiments, the polyglycerol emulsifier is polyglycerol-10 oleate. In some specific embodiments, the polyglycerol-10 oleate is present in parts by weight of 10 parts.

[0023] In some embodiments, the polyglycerol emulsifier is composed of polyglycerol-10 oleate and polyglycerol-10 stearate. In some specific embodiments, the mass ratio of polyglycerol-10 oleate to polyglycerol-10 stearate is 7.5:2.5.

[0024] In some embodiments, the cinnamic ester derivative is at least one of ethylhexyl methoxycinnamate, isoamyl p-methoxycinnamate, and octocrylene.

[0025] In some embodiments, the salicylate derivative is at least one of ethylhexyl salicylate and homosalate;

[0026] In some embodiments, the triazine derivative is at least one of bis-ethylhexyloxyphenol methoxyphenyl triazine, diethylhexylbutamidotriazinone, and ethylhexyltriazinone.

[0027] In some embodiments, the siloxane is at least one of polysiloxane-15 and cresoltrazol trisiloxane.

[0028] In some embodiments, the benzoazole derivative is at least one of methylene bis-benzotriazolyl tetramethylbutylphenol, phenylbenzimidazole sulfonic acid, and disodium phenyl dibenzimidazole tetrasulfonate.

[0029] In some embodiments, the benzoylmethane derivative is at least one of butylmethoxybenzoylmethane and diethylaminohydroxybenzoylhexyl benzoate;

[0030] In some embodiments, the para-aminobenzoic acid ester derivative is at least one of PEG-25 para-aminobenzoic acid and dimethyl PABA ethylhexyl ester.

[0031] In some embodiments, the benzophenone derivative is at least one of benzophenone-3 and benzophenone-4;

[0032] In some embodiments, the camphor derivative is at least one of terephthalimide dicamphor sulfonic acid, 4-methylbenzyl camphor, and camphor benzalkonium methyl sulfate.

[0033] In some embodiments, the organic sunscreen agent is composed of cinnamic acid ester derivatives, dibenzoylmethane derivatives, and triazine derivatives. In some specific embodiments of the present invention, the cinnamic acid ester derivative is ethylhexyl methoxycinnamate; the dibenzoylmethane derivative is diethylaminohydroxybenzoylhexyl benzoate; the triazine derivative is composed of ethylhexyl triazine ketone and bis-ethylhexyloxyphenol methoxyphenyl triazine; the preferred mass ratio of ethylhexyl triazine ketone to bis-ethylhexyloxyphenol methoxyphenyl triazine is 3:4. In a specific embodiment of the present invention, the mass ratio of the cinnamic acid ester derivative, dibenzoylmethane derivative, and triazine derivative is 17:7:8.

[0034] In some embodiments, the organic sunscreen agent is composed of cinnamic acid ester derivatives, salicylic acid ester derivatives, benzoylmethane derivatives, triazine derivatives, and silane derivatives. In some specific embodiments of the present invention, the cinnamic acid ester derivative is composed of ethylhexyl methoxycinnamate and octocrylene; the salicylic acid ester derivative is ethylhexyl salicylate; the benzoylmethane derivative is diethylaminohydroxybenzoylhexyl benzoate; the triazine derivative is composed of ethylhexyl triazine ketone, bis-ethylhexyloxyphenol methoxyphenyl triazine, and diethylhexylbutamidotriazine ketone, wherein the mass ratio of ethylhexyl triazine ketone, bis-ethylhexyloxyphenol methoxyphenyl triazine, and diethylhexylbutamidotriazine ketone is 2:3:3; and the siloxane is cresoltrazol trisiloxane. In a specific embodiment of the present invention, the mass ratio of the cinnamic acid ester derivative, salicylic acid ester derivative, dibenzoylmethane derivative, triazine derivative and silane derivative is 14:5:5:8:2.

[0035] In some specific embodiments, the organic sunscreen agent is selected from any combination shown in (1) to (3) below:

[0036] (1) Ethylhexyl methoxycinnamate, hexyl diethylamino hydroxybenzoyl benzoate, ethylhexyl triazine ketone and bis-ethylhexyloxyphenol methoxyphenyl triazine.

[0037] (2) Ethylhexyl methoxycinnamate, octocrylene, ethylhexyl salicylate, diethylamino hydroxybenzoyl benzoate, ethylhexyl triazine, bis-ethylhexyloxyphenol methoxyphenyl triazine, diethylhexylbutamidotriazine, cresoltrazol trisiloxane.

[0038] (3) Ethylhexyl methoxycinnamate, octocrylene, diethylamino hydroxybenzoyl benzoate, ethylhexyl triazine, bis-ethylhexyloxyphenol methoxyphenyl triazine, diethylhexylbutamidotriazine.

[0039] In this invention, the polyol used is preferably selected from, but not limited to, at least one of the following groups: glycerol, propylene glycol, butanediol, 1,2-pentanediol, and 1,2-hexanediol. During the D-phase emulsification process, the presence of the polyol raises the cloud point of the surfactant, improves the miscibility between the surfactant and the aqueous phase, and makes it easier for the surfactant to adsorb onto the oil-water interface.

[0040] In this invention, the raw materials of the sunscreen composition further include synthetic ester oil. In some embodiments, the synthetic ester oil is 8 to 20 parts by weight, preferably 8 to 12 parts. The synthetic ester oil includes at least one selected from C12-15 alcohol benzoate, butyl octyl salicylate, caprylic / capric triglyceride, coconut oil alcohol-caprylate / capric acid ester, diisopropyl sebacate, diisopropyl adipate, dibutyl adipate, isoamyl laurate, diethylhexyl carbonate, dioctyl carbonate, heptadecyl undecanoate, and propylene glycol dibenzoate. More preferably, it includes at least one selected from diisopropyl sebacate, C12-15 alcohol benzoate, and diisopropyl adipate.

[0041] In this invention, the sunscreen composition further includes an oil-soluble film-forming agent. In some embodiments, the oil-soluble film-forming agent is present in parts by weight of 1 to 4 parts, preferably 3 to 3.5 parts. The film-forming agent includes at least one of VP / hexadecene copolymer, VP / eicosene copolymer, triacontyl PVP, trimethylsiloxysilicate, acrylate / polydimethylsiloxane copolymer, and polymethylsilsesquioxane. In some specific embodiments, the oil-soluble film-forming agent includes VP / hexadecene copolymer and / or triacontyl PVP.

[0042] In this invention, the sunscreen composition further includes a preservative. In some embodiments, the preservative is 0.1 to 1 part by weight, and the preservative includes at least one selected from caprylyl glycol, 1,2-pentanediol, ethylhexylglycerin, 1,2-hexanediol, chlorophenoxyethanol, phenoxyethanol, methylparaben, p-hydroxyacetophenone, capryloyl hydroxamic acid, and glyceryl caprylate.

[0043] The sunscreen composition of the present invention also includes water as a raw material. In some embodiments, the water is preferably 10 to 35 parts by weight. In some specific embodiments, the water is 12.5 to 30.4 parts by weight.

[0044] In this invention, the particle size of the sunscreen composition is 100-500 nm.

[0045] The present invention also provides a method for preparing the sunscreen composition, comprising the following steps:

[0046] S1. Heat and stir the organic sunscreen agent until it is completely dissolved and homogeneous, forming an oil phase;

[0047] S2. Mix the polyglycerol emulsifier with the polyol, heat and stir until homogeneous to form phase D;

[0048] S3. Under stirring conditions, the oil phase and the D phase are mixed and homogenized to obtain a material.

[0049] S4. Add water to the material and stir until homogeneous to obtain the D-phase sunscreen composition.

[0050] In the preparation method of the present invention, steps S1 and S2 are not sequential.

[0051] In step S1 of this invention, the oil phase heating condition is 80-85℃.

[0052] In step S2 of this invention, the heating condition of phase D is 75-80℃.

[0053] In step S2 of this invention, water may or may not be added after heating and stirring until homogeneous. There are no special requirements regarding the specific amount of water added; it can be selected based on actual conditions, but typically should not exceed 5% of the total water volume.

[0054] In step S3 of this invention, the homogenization is performed at 5000-9000 rpm for 3-5 minutes.

[0055] The present invention also provides the use of the sunscreen composition described herein or the sunscreen composition prepared by the method described herein in the preparation of sunscreen products.

[0056] The present invention also provides a sun protection product comprising sun protection ingredients and cosmetically acceptable adjuvants;

[0057] The sunscreen ingredients are as shown in (1) or (2):

[0058] (1) The sunscreen composition according to any one of claims 1 to 7 or the sunscreen composition prepared by the preparation method according to any one of claims 8 to 9

[0059] (2) The sunscreen composition described in (1) and other sunscreen agents; the other sunscreen agents include inorganic sunscreen agents and / or organic sunscreen agents;

[0060] The organic sunscreen agent includes at least one of the following: cinnamic acid ester derivatives, salicylic acid ester derivatives, triazine derivatives, siloxanes, benzoazole derivatives, dibenzoylmethane derivatives, p-aminobenzoic acid ester derivatives, benzo(methyl)ketone derivatives, and camphor derivatives;

[0061] The inorganic sunscreen agent includes titanium dioxide and / or zinc oxide;

[0062] The cosmetic-acceptable additives include at least one of the following: solvents, pH adjusters, thickeners, preservatives, synthetic ester oils, oil-soluble film-forming agents, polyol moisturizers, and emulsifiers.

[0063] The sunscreen composition described in this invention can be used to prepare sunscreen products or cosmetics.

[0064] Furthermore, the cosmetic product is a cosmetic product with photoprotective properties.

[0065] In some embodiments, the cosmetic includes creams, lotions, gels, or aqueous solutions. Those skilled in the art can prepare the traditional Chinese medicine composition of the present invention according to the method described above, and then add pharmaceutically acceptable conventional excipients and formulate it into a clinically acceptable dosage form using conventional processes.

[0066] The sunscreen composition of this invention is prepared using a specific emulsifier and a D-phase emulsification process, resulting in fine and uniform particles. It not only possesses excellent stability but also effectively improves the sun protection efficiency of sunscreen products, exhibiting a significant synergistic effect in sun protection. Furthermore, it can reduce the amount of chemical sunscreen agents used in sunscreen products, thereby improving the oily feel of high-SPF sunscreens. This composition is suitable for preparing cosmetics with sun protection or photoprotection functions and has promising application prospects in the cosmetics field. Attached Figure Description

[0067] Figure 1 The material properties of each sample are shown after being placed at room temperature (25°C) for three months; from left to right, they are the results of sample 1 of Example 1, sample 2 of Example 2, sample 2 of Comparative Example 1, and sample 1 of Comparative Example 2.

[0068] Figure 2 The material properties of each sample after being placed at 55°C for one month are shown; from left to right, they are the results of sample 1 of Example 1, sample 2 of Example 2, sample 2 of Comparative Example 2, and sample 1 of Comparative Example 1. Detailed Implementation

[0069] This invention provides sunscreen compositions, sunscreen products, their preparation methods, and applications. Those skilled in the art can refer to the content herein and appropriately modify the process parameters to achieve the desired results. It should be particularly noted that all similar substitutions and modifications are obvious to those skilled in the art and are considered to be included in this invention. The methods and applications of this invention have been described through preferred embodiments. Those skilled in the art can clearly modify or appropriately change and combine the methods and applications described herein without departing from the content, spirit, and scope of this invention to realize and apply the technology of this invention.

[0070] In this invention, "D-phase sunscreen preparation", "D-phase sunscreen composition" and "sunscreen composition" have the same meaning, all referring to sunscreen raw materials made by using the D-phase emulsification process with specific emulsifiers, and they can be used interchangeably.

[0071] In this invention, the terms "comprising," "including," and "having" are used interchangeably to indicate the inclusiveness of a solution, meaning that the solution may contain elements other than those listed. It should also be understood that the use of "comprising," "including," and "having" herein also provides for solutions "consisting of...".

[0072] In this invention, "and / or" as used herein includes the meaning of "and", "or", and "all or any other combination of elements linked by the term".

[0073] In this invention, "at least one" means one or more, and "more than one" means two or more. "At least one," "at least one item," or similar expressions refer to any combination of these items, including any combination of single or multiple items.

[0074] In this document, numerical ranges are referred to as continuous unless otherwise specified, and include the minimum and maximum values ​​of the range, as well as every point value between the minimum and maximum values. Furthermore, when a range refers to an integer, it includes every integer between the minimum and maximum values ​​of the range. Additionally, when multiple ranges are provided to describe a feature or characteristic, the ranges may be merged. Unless otherwise specified, all ranges disclosed herein should be understood to include any and all subranges to which they are incorporated.

[0075] This invention does not impose any special restrictions on the source of any of the raw materials. Unless otherwise specified, all test materials used in this invention are common commercial products and can be purchased from the market.

[0076] The present invention will be further illustrated below with reference to the embodiments:

[0077] Examples 1-4

[0078] The D-phase formulations of Examples 1-4 and the sunscreen cream of Example 7 were prepared according to the formulations in Table 1 using the following steps:

[0079] (1) Weigh the raw material of the B phase formula, i.e. the oil phase, and put it into a constant temperature water bath at 80-85℃ and heat it. Keep it warm and stir for 15-20 minutes until the oil phase is completely dissolved and there are no particles, and obtain the B phase.

[0080] (2) Weigh the raw material of the A1 phase formula, i.e. the D phase, and put it into a constant temperature water bath at 75-80℃ and heat it. Keep it warm and stir for 15-20 minutes until the D phase is completely dissolved and there are no particles. Then add a small amount of water (A2) to the A1 phase and stir evenly to obtain the A mixed phase.

[0081] (3) Under stirring, the B phase is slowly added dropwise into the A mixed phase, stirred evenly, and then the homogenizer is turned on for about 3-5 minutes at a speed of 5000-9000 rpm.

[0082] (4) Stir and cool the mixture at an ambient temperature of 28°C. When the temperature drops to 40-45°C, slowly add the C phase raw material and stir until it is evenly mixed to finally obtain the D phase sunscreen formulation.

[0083] The raw material formulations used in Examples 1-4 and Example 7 are as follows:

[0084] Table 1

[0085]

[0086] Preparation of comparative 1-3D phase sunscreen formulations

[0087] The D-phase sunscreen formulations of Comparative Examples 1-3 were prepared according to the preparation methods of Examples 1-4.

[0088] The raw material formulations used in Comparative Examples 1-3 are as follows:

[0089] Table 2

[0090]

[0091] Examples 5-6: Preparation of the sunscreen cream of the present invention

[0092] Using the D-phase sunscreen formulations of Examples 1-2 as raw materials, the sunscreen creams containing the D-phase sunscreen formulations of Examples 5-6 were prepared according to the following steps based on the formulation in Table 3:

[0093] (1) Weigh the raw material of phase A, i.e. the aqueous phase, and put it into a constant temperature water bath at 85℃ and heat it for 10 minutes. Then homogenize the aqueous phase for 2-3 minutes at a speed of 6500-7500 rpm.

[0094] (2) Weigh out the amount of raw material in phase B, i.e., the oil phase, and heat it in a constant temperature water bath at 85°C until the oil phase is completely dissolved and there are no particles.

[0095] (3) Under the condition of constant temperature water bath at 85℃, pour phase B into phase A, stir evenly, and then turn on homogenization for about 2-4 minutes at a speed of 6500-7500 rpm to obtain emulsion.

[0096] (4) Remove the homogenized emulsion from the constant temperature water bath and cool it down by stirring at an ambient temperature of 28℃ and a rotation speed of 500-1000 rpm / min. Add phase C when the temperature drops to 40-45℃, and finally stir until homogeneous.

[0097] The raw material formula used in the sunscreen creams in Examples 5-6 is as follows:

[0098] Table 3

[0099]

[0100]

[0101] Preparation of Comparative Examples 4-5: Sunscreen Cream

[0102] The cream of this comparative example was prepared using a preparation method that was basically the same as that used in Examples 5-6.

[0103] The raw material formulations used in Comparative Examples 4 and 5 are as follows:

[0104] Table 4

[0105]

[0106]

[0107] Test Experiment

[0108] 1. Security Testing

[0109] Test samples: Example 5, Comparative Example 4;

[0110] Test method: Safety was tested by a third-party testing agency. Areas not exceeding 50mm² were selected. 2 A suitable patch applicator with a depth of approximately 1 mm is used, and approximately 0.02-0.025 ml (g) of the test substance is added into the patch applicator using a closed patch test method.

[0111] An experimental group and a control group were set up. The experimental group was given the samples of Example 5 and Comparative Example 4, respectively, while the control group was given an empty white spot tester without the test substance. The spot tester was applied to the flexor side of the subject's forearm, and the test substance was removed after 24 hours. Skin reactions were observed at 0.5 hours, 24 hours, and 48 hours after removal.

[0112] The results were recorded according to the skin reaction grading standards in the "Cosmetic Safety Technical Regulations 2015".

[0113] Table 5 Results of patch test

[0114]

[0115] Note: Skin reaction grading standards;

[0116] Grade 0: Negative reaction;

[0117] Grade 1: Suspicious reaction; only slight erythema;

[0118] Grade 2: Weak positive reaction (erythema reaction); erythema, infiltration, edema, and papules may be present;

[0119] Grade 3: Strong positive reaction (herpes reaction); erythema, infiltration, edema, papules, vesicles; the reaction may extend beyond the tested area;

[0120] Grade 4: Extremely strong reaction (confluent herpes simplex reaction): obvious erythema, severe infiltration, edema, confluent herpes simplex, reaction extending beyond the test area.

[0121] As shown in Table 5 above, the cream prepared in Example 5 showed no irritation and passed the safety test.

[0122] 2. Stability Test:

[0123] The initial particle size of the D-phase sunscreens prepared in Examples 1 and 2, the D-phase sunscreens prepared in Comparative Examples 1, 2 and 5, and the cream in Example 7 was determined using a Zetasizer nanoZS nanoparticle size analyzer. The experimental results are summarized in Table 6.

[0124] The D-phase sunscreen formulations prepared in Examples 1-4 were subjected to stability evaluation for three months at room temperature, -16°C, 45°C, and 55°C, respectively. The results are summarized in Table 7. The D-phase sunscreen formulations prepared in Comparative Examples 1, 2, and 3 were subjected to stability evaluation for one month at room temperature, -16°C, 45°C, and 55°C, respectively. The results are summarized in Table 8. The properties of the material at room temperature (25°C) are shown in Table 8. Figure 1 The material properties at 55℃ are shown below. Figure 2 .

[0125] Table 6 Initial particle size test reports of D-phase sunscreen formulations in each example and comparative example.

[0126] serial number Particle size (nm) Particle Size Polydispersity Index (PDI) Example 1 141.8 0.248 Example 2 190.1 0.220 Comparative Example 1 220.2 0.237 Comparative Example 2 190.1 0.393 Example 7 297.4 0.347 Comparative Example 5 1286 0.551

[0127] Table 7. Stability test reports of the D-phase sunscreen formulations for each embodiment.

[0128]

[0129]

[0130] Table 8. Stability test reports of D-phase sunscreen formulations for each comparative example.

[0131]

[0132] As can be seen from the table above, Examples 1, 2, and 3 exhibit superior stability, while Example 4 shows stratification under high-temperature conditions. This indicates that, compared to other polyglycerol emulsifiers, polyglycerol-10 oleate has a superior emulsifying effect on the organic sunscreen agent described in this invention, resulting in a more stable product.

[0133] Although D-phase sunscreen formulations can be prepared by using polyether emulsifiers alone or Tween emulsifiers alone in Comparative Examples 1-3, their stability is poor.

[0134] 3. Comparison of SPF and PA values ​​in in vitro testing:

[0135] (1) Test samples: sunscreen creams containing D-phase sunscreen agents provided in Examples 5-6 and sunscreen creams without D-phase sunscreen agents provided in Comparative Examples 4-5;

[0136] (2) Testing instrument: UV2000S ultraviolet transmittance analyzer;

[0137] (3) Test method: The sunscreen cream or control sample was tested at 1.3 mg / cm³. 2 The coating density was uniformly applied to the PMMA board, and four parallel tests were conducted. The solar irradiance value was referenced to the ISO 2021 standard. The UV2000S ultraviolet transmittance analyzer was used for scanning and testing. Nine points were selected for testing each test board. The SPF average value was rounded up to obtain the final SPF value, and the PA average value was rounded up to obtain the final PA value.

[0138] The specific test results are shown in Table 9 below:

[0139] Table 9. Test reports on SPF and PA values ​​of sunscreens from various examples and comparative examples.

[0140] Test Project SPF value PA value Example 5 38 12 Example 6 38 13 Comparative Example 4 32 10 Example 7 31.19 12.28 Comparative Example 5 27.87 8.37

[0141] Using DSM's sunscreen simulator, the SPF value for Examples 5 and 6 was 32.9, and the PA value was 9.6. As shown in Table 9, the components in the D-phase sunscreen formulation of this invention work synergistically to enhance both SPF and PA protection capabilities. It significantly improves absorption across a broad and strong 280-400nm wavelength range, achieving an SPF value of around 38. Furthermore, it is stable, non-irritating to the skin, and has good safety, making it an ideal sunscreen composition.

[0142] Comparative Example 5 and Example 7 used the same type and amount of chemical sunscreen agents. Comparative Example 5 did not use the D-phase emulsification process, while Comparative Example 7 used the D-phase emulsification process to prepare the sunscreen cream. Compared with Comparative Example 5, Example 7 had smaller particle size and a higher SPF value. This shows that the components in the D-phase sunscreen formulation of the present invention work synergistically with the D-phase emulsification process, resulting in a synergistic effect in terms of SPF and PA sun protection capabilities. An ideal SPF value can be obtained using a small amount of chemical sunscreen agent. Without the D-phase emulsification process of the present invention (such as Comparative Example 5), it is difficult to obtain an ideal SPF value; one must increase the amount of chemical sunscreen agent to achieve the desired SPF value.

[0143] The above are merely preferred embodiments of the present invention. It should be noted that those skilled in the art can make various improvements and modifications without departing from the principle of the present invention, and these improvements and modifications should also be considered within the scope of protection of the present invention.

Claims

1. A sunscreen composition, characterized in that, It is prepared by emulsifying the following raw materials in parts by weight using the D phase: Polyglycerol emulsifier: 5-15 parts; Polyols: 10-20 parts; Organic sunscreen agents: 24-40 parts; The polyglycerol emulsifier comprises polyglycerol-10 oleate, or comprises polyglycerol-10 oleate and at least one of the following: Polyglycerol-10 myristate, polyglycerol-10 stearate; The organic sunscreen agent includes at least one of the following: cinnamic acid ester derivatives, salicylic acid ester derivatives, triazine derivatives, siloxane derivatives, benzoazole derivatives, dibenzoylmethane derivatives, p-aminobenzoic acid ester derivatives, benzo(methyl) ketone derivatives, and camphor derivatives.

2. The sunscreen composition according to claim 1, characterized in that, The polyglycerol emulsifier is composed of polyglycerol-10 oleate and polyglycerol-10 myristate.

3. The sunscreen composition according to claim 2, characterized in that, The mass ratio of polyglycerol-10 oleate to polyglycerol-10 myristate is (5-10):(0.5-3).

4. The sunscreen composition according to claim 1, characterized in that, The cinnamic acid ester derivatives mentioned above are at least one of ethylhexyl methoxycinnamate, isoamyl p-methoxycinnamate, and octocrylene. The salicylate derivatives mentioned are at least one of ethylhexyl salicylate and homosalate; The triazine derivatives mentioned are at least one of bis-ethylhexyloxyphenol methoxyphenyl triazine, diethylhexylbutamidotriazinone, and ethylhexyltriazinone; The siloxanes mentioned are at least one of polysiloxane-15 and cresoltrazol trisiloxane; The benzoazole derivatives mentioned are at least one of methylene bis-benzotriazolyl tetramethylbutylphenol, phenylbenzimidazole sulfonic acid, and disodium phenyl dibenzimidazole tetrasulfonate. The benzoylmethane derivatives mentioned above are at least one of butyl methoxybenzoylmethane and diethylamino hydroxybenzoyl hexyl benzoate; The para-aminobenzoic acid ester derivatives mentioned above are at least one of PEG-25 para-aminobenzoic acid and dimethyl PABA ethylhexyl ester; The benzophenone derivatives mentioned are at least one of benzophenone-3 and benzophenone-4; The camphor derivatives mentioned are at least one of terephthalimide dicamphor sulfonic acid, 4-methylbenzyl camphor, and camphor benzalkonium methyl sulfate.

5. The sunscreen composition according to claim 1, characterized in that, The organic sunscreen agent is composed of cinnamic acid ester derivatives and triazine derivatives, preferably, the mass ratio of the cinnamic acid ester derivatives to the triazine derivatives is 17:15; Alternatively, the organic sunscreen agent is composed of cinnamic acid ester derivatives, salicylic acid ester derivatives, dibenzoylmethane derivatives, triazine derivatives, and silane derivatives. Preferably, the mass ratio of the cinnamic acid ester derivatives, salicylic acid ester derivatives, dibenzoylmethane derivatives, triazine derivatives, and silane derivatives is 14:5:5:8:

2.

6. The sunscreen composition according to claim 1, characterized in that, The polyol includes at least one of glycerol, propylene glycol, butylene glycol, 1,2-pentanediol, and 1,2-hexanediol.

7. The sunscreen composition according to claim 1, characterized in that, It also includes at least one of water, preservatives, oil-soluble film-forming agents, and synthetic ester oils; The synthetic ester oil has a mass fraction of 8 to 20 parts, and the synthetic ester oil includes at least one of C12-15 alcohol benzoate, butyl octyl salicylate, caprylic / capric triglyceride, coconut oil alcohol-caprylate / capric acid ester, diisopropyl sebacate, diisopropyl adipate, dibutyl adipate, isoamyl laurate, diethylhexyl carbonate, dioctyl carbonate, heptadecyl undecenoate, and propylene glycol dibenzoate. The oil-soluble film-forming agent has a mass fraction of 1 to 4 parts, and the film-forming agent includes at least one of VP / hexadecene copolymer, VP / eicosene copolymer, triacontyl PVP, trimethylsiloxysilicate, acrylate / polydimethylsiloxane copolymer, and polymethylsilsesquioxane. The preservative is present in a fraction of 0.1 to 1 part by weight, and the preservative includes at least one of the following: caprylyl glycol, 1,2-pentanediol, ethylhexylglycerin, 1,2-hexanediol, chlorphenesin, phenoxyethanol, methylparaben, p-hydroxyacetophenone, capryloyl hydroxamic acid, and glyceryl caprylate.

8. The sunscreen composition according to any one of claims 1 to 7, characterized in that, The particle size of the sunscreen composition is 100-500 nm.

9. A method for preparing the sunscreen composition according to any one of claims 1 to 8, characterized in that, Includes the following steps: S1. Heat and stir the organic sunscreen agent until it is completely dissolved and homogeneous, forming an oil phase; S2. Mix the polyglycerol emulsifier with the polyol, heat and stir until homogeneous to form phase D; S3. Under stirring conditions, the oil phase and the D phase are mixed and homogenized to obtain a lio body; S4. Add the remaining water to the material and stir evenly to obtain the D-phase sunscreen composition.

10. The preparation method according to claim 9, characterized in that, There is no specific order between steps S1 and S2; In step S1, the oil phase heating condition is 80-85℃; In step S2, the heating condition for phase D is 75-80℃; In step S3, the mixing involves slowly adding the oil phase into the D phase. The homogenization process involves homogenizing at 5000-9000 rpm for 3-5 minutes.

11. The use of the sunscreen composition according to any one of claims 1 to 8 or the sunscreen composition prepared by the preparation method according to any one of claims 9 to 10 in the preparation of sunscreen products.

12. A sunscreen product, characterized in that, This includes sunscreen ingredients and cosmetically acceptable additives; The sunscreen ingredients are as shown in (1) or (2): (1) The sunscreen composition according to any one of claims 1 to 8 or the sunscreen composition prepared by the preparation method according to any one of claims 9 to 10 (2) The sunscreen composition described in (1) and other sunscreen agents; the other sunscreen agents include inorganic sunscreen agents and / or organic sunscreen agents; The organic sunscreen agent includes at least one of the following: cinnamic acid ester derivatives, salicylic acid ester derivatives, triazine derivatives, siloxanes, benzoazole derivatives, dibenzoylmethane derivatives, p-aminobenzoic acid ester derivatives, benzo(methyl)ketone derivatives, and camphor derivatives; The inorganic sunscreen agent includes titanium dioxide and / or zinc oxide; The cosmetic-acceptable additives include at least one of the following: solvents, pH adjusters, thickeners, preservatives, synthetic ester oils, oil-soluble film-forming agents, polyol moisturizers, and emulsifiers.

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