Water-resistant oil-in-water sunscreen lotion capable of reducing percutaneous penetration of chemical sunscreen agent, and preparation method therefor

By using an emulsifier composed of C20-40 alcohol and C20-40 acid in an oil-in-water sunscreen, a crystalline water-oil interface is formed, solving the problem of easy penetration of chemical sunscreens and achieving a highly safe and water-resistant sunscreen effect, suitable for sensitive skin and children.

WO2025255985A1PCT designated stage Publication Date: 2025-12-18AOYUAN NEW MATERIAL (GUANGZHOU) LTD +1
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Patent Information

Application Number
PCT/CN2024/119103
Authority / Receiving Office
WO · WO
Patent Type
Applications
Current Assignee / Owner
Priority Date
2024-06-14
Filing Date
2024-09-14
Publication Date
2025-12-18

AI Technical Summary

Technical Problem

In existing water-in-oil sunscreen systems, chemical sunscreen agents are easily penetrated through the skin, leading to high sensitization rates and insufficient water resistance and durability, making it difficult to meet the needs of sensitive skin and children.

Method used

Emulsifiers, which are a combination of C20-40 alcohols and C20-40 acids or a combination of long-carbon alcohol co-emulsifiers, form a crystalline water-oil interface, which stably encapsulates chemical sunscreens, reduces their permeability, and improves film-forming properties and water resistance through the combination of highly polar chemical sunscreens and crystalline emulsifiers.

Benefits of technology

It significantly reduces the transdermal penetration of chemical sunscreens, improves the safety and water resistance of sunscreen products, is suitable for sensitive skin and children, has good film-forming properties, is long-lasting and does not peel off, and has a light and comfortable feel on the skin.

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Abstract

A water-resistant oil-in-water sunscreen lotion capable of reducing percutaneous penetration of a chemical sunscreen agent, and a preparation method therefor. The components of the sunscreen lotion include, in mass percent: 1-35 parts of a sunscreen agent and 0.5-10 parts of an emulsifier, wherein the emulsifier contains C20-40 acid and further contains C20-40 alcohol and / or a long-chain alcohol co-emulsifier, and the sunscreen agent contains a chemical sunscreen agent and a physical sunscreen agent. The prepared water-resistant oil-in-water sunscreen lotion has an SPF value exceeding 30, exhibits excellent sun-protection efficacy, and contains a system with a special crystalline-type emulsification structure, endowing the obtained oil-in-water emulsification system with excellent stability, water resistance, friction resistance and anti-shedding properties, so that the possibility of direct contact between the chemical sunscreen agent in the sunscreen lotion and the skin is greatly reduced, and the percutaneous penetration of the chemical sunscreen agent is significantly reduced, thereby improving the safety of sunscreen products. In addition, the water-resistant oil-in-water sunscreen lotion is mild and non-irritating, provides a comfortable skin feel, and is suitable for use by individuals with sensitive skin and children.
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Description

An anti-water oil-in-water sunscreen emulsion capable of reducing the percutaneous penetration of chemical sunscreen agents and a preparation method thereof TECHNICAL FIELD

[0001] The present application belongs to the technical field of cosmetics, and particularly relates to an anti-water oil-in-water sunscreen emulsion capable of reducing the percutaneous penetration of chemical sunscreen agents and a preparation method thereof. BACKGROUND

[0002] With the continuous improvement of people's living standards and the continuous enhancement of personal protection awareness, the domestic sunscreen market has grown significantly in recent years, not limited to adult sunscreens, but also significantly in children's sunscreens. Sunscreen products are currently defined as special cosmetics under the laws and regulations in China, and the safety of sunscreen products is the focus of general concern.

[0003] At present, the state allows the use of 25 chemical sunscreen agents and 2 physical sunscreen agents, most of which can only be oil-soluble. Most of the sunscreen products currently sold on the market are water-in-oil sunscreen systems and full oil wax-based systems. In these two systems, the chemical sunscreen agents are in the external phase, directly contacting the skin and more likely to cause percutaneous penetration, raising concerns about safety. Therefore, in order to reduce the greater skin problems such as sensitization and swelling caused by chemical sunscreen agents in the external phase, the oil-in-water system is a good choice. The oil-in-water system has the advantages of a relatively light skin feel, high moisturizing and permeability, and does not cause a large burden on the skin after long-term use. In the oil-in-water system, although the chemical sunscreen agents are in the internal phase, the extremely fine emulsion droplets can also cause percutaneous penetration, bringing the unfriendly ingredients such as chemical sunscreen agents into the deep layer of the skin. Therefore, how to reduce the penetration of chemical sunscreen agents is a big problem. In addition, the oil-in-water system has poor durability and water resistance, so the application of the oil-in-water system in sunscreen products that require water resistance and durability needs to overcome a series of hydrophilic problems of the oil-in-water system. Therefore, improving the water resistance and durability of the oil-in-water system for skin sunscreen products and how to improve the water resistance of the product while considering the good use performance of the product are extremely difficult problems in the oil-in-water system. CN115300417A discloses a sunscreen cream suitable for children and sensitive skin and a preparation method thereof. The sunscreen cream uses water-based thickeners and emulsion thickeners, as well as water-soluble emulsifiers and oil-soluble emulsifiers, etc. By wrapping the organic sunscreen agents, the penetration of the organic sunscreen agents into the skin is reduced, achieving a mild and safe sunscreen effect. However, the sunscreen cream has poor water resistance and durability, and is prone to falling off. CN109833214A discloses a mild oil-in-water pickering sunscreen and skin care product. By using polyacryloyl dimethyl sodium taurate, the sunscreen powder such as zinc oxide and titanium dioxide is wrapped to prepare a mild oil-in-water pickering sunscreen and skin care product, which has good waterproof and sweat-proof effects. However, the sunscreen and skin care product has poor durability after film formation and is prone to falling off.

[0004] In summary, reducing the sensitization of sunscreen skin care products and reducing the skin penetration of sunscreen agents is an important part of sunscreen skin care products, and improving the water resistance and durability of sunscreen skin care products of oil-in-water system, and improving the water resistance of the product while considering the good use performance of the product are the key problems to be solved for sunscreen skin care products of oil-in-water system.

[0005] SUMMARY

[0006] In view of the problems in the prior art, the present application provides an anti-water type oil-in-water sunscreen cream capable of reducing the percutaneous penetration of chemical sunscreen agents and a preparation method thereof. The anti-water type oil-in-water sunscreen cream can significantly reduce the percutaneous penetration of chemical sunscreen agents, reduce the sensitization of chemical sunscreen agents, improve the safety of sunscreen skin care products, and is suitable for sensitive skin, children and other populations.

[0007] In a first aspect, the present application provides an anti-water type oil-in-water sunscreen cream capable of reducing the percutaneous penetration of chemical sunscreen agents. The sunscreen cream ingredients include moisturizing agents, thickening agents, emollients, emulsifiers, sunscreen agents, anti-allergic agents, pH regulators, skin feel regulators, preservatives and water.

[0008] Further, the sunscreen cream ingredients include 1-25 parts of moisturizing agents, 0.1-15 parts of thickening agents, 1-50 parts of emollients, 0.5-10 parts of emulsifiers, 1-35 parts of sunscreen agents, 0.1-5 parts of anti-allergic agents, 0.1-3 parts of pH regulators, 1-10 parts of skin feel regulators, 0.1-5 parts of preservatives and 20-80 parts of water, by mass percentage of the total mass of the sunscreen cream.

[0009] Further, the emulsifier contains 0.1-5 parts of C20-40 acid, and the emulsifier also contains 0.1-5 parts of C20-40 alcohol and / or 0.1-5 parts of long carbon alcohol co-emulsifier, by mass percentage.

[0010] Further, the long carbon alcohol co-emulsifier is selected from one or more of lauryl alcohol, cetyl alcohol, stearyl alcohol, cetearyl alcohol, behenyl alcohol.

[0011] Preferably, the emulsifier contains 0.1-5 parts of C20-40 alcohol and 0.1-5 parts of C20-40 acid.

[0012] More preferably, the mass ratio of the C20-40 alcohol and the C20-40 acid is 1:(0.5-5).

[0013] Further, the emulsifier can also add one or more of ceteareth-20, glyceryl stearate, PEG-100 stearate, sucrose ester oil-in-water emulsifier, PEG-containing oil-in-water emulsifier.

[0014] Preferably, the mass ratio of C20-40 alcohol, C20-40 acid, ceteareth-20 in the emulsifier is 1: (0.5-5): (0.1-3);

[0015] Further, the thickening agent is selected from one or more of xanthan gum, sodium magnesium lithium silicate, carbomer, sodium polyacryloyldimethyl taurate;

[0016] Preferably, the thickening agent is a complex of xanthan gum and sodium magnesium lithium silicate;

[0017] More preferably, the mass ratio of xanthan gum and sodium magnesium lithium silicate is 1:1-6.

[0018] Further, the humectant is selected from one or more of glycerin, propylene glycol, erythritol, butylene glycol, pentylene glycol, sodium hyaluronate, ceramide, polysaccharide.

[0019] Still further, the humectant is any combination of propylene glycol, sodium hyaluronate and erythritol;

[0020] Preferably, the mass ratio of sodium hyaluronate, propylene glycol, erythritol is 0-1:5-15:5.

[0021] Still further, the humectant is selected from one or more of glycerin 1-10 parts, propylene glycol 1-10 parts, erythritol 1-10 parts, butylene glycol 1-10 parts, pentylene glycol 1-10 parts, sodium hyaluronate 0.01-5 parts, ceramide 0.1-5 parts, polysaccharide 1-10 parts, in terms of total mass of sunscreen cream;

[0022] Further, the emollient is selected from one or more of dioctyl ether, ethylhexyl palmitate, caprylic / capric triglyceride, isononyl isononanoate, propylene glycol dicaprylate / dicaprate, dicaprylyl carbonate, coco-caprylate / caprate, mineral oil, octyldodecanol, isohexadecane, isododecane, cyclopentasiloxane, dimethicone, squalane, hydrogenated polyisobutene, phenyl dimethicone, PRUNUS DOMESTICA seed extract, a complex of JUNIPERUS VIRGINIANA CALLUS EXTRACT (and) PADINA PAVONICA THALLUS EXTRACT (mass ratio 99:1), a complex of CAPRYLIC / CAPRIC TRIGLYCERIDE (and) TIPROFEN (mass ratio 98:2), a complex of HELIANTHUS ANNUUS (SUNFLOWER) SEED OIL (and) LUPINUS ALBUS SEED EXTRACT (and) TOCOPHEROL (mass ratio 95.4-96.4%:3.5-4.5%:0.1%), HELIANTHUS ANNUUS (SUNFLOWER) SEED OIL UNSAPONIFIABLES, PASSIFLORA EDULIS SEED OIL, MAURITIA FLEXUOSA FRUIT OIL.

[0023] Further, the emollient is selected from one or more of dioctyl ether 1-20 parts, ethylhexyl palmitate 1-10 parts, caprylic / capric triglyceride 1-10 parts, isononyl isononanoate 1-15 parts, propylene glycol dicaprylate / dicaprate 1-10 parts, dicaprylyl carbonate 1-10 parts, coco-caprylate / caprate 1-10 parts, mineral oil 1-20 parts, octyldodecanol 1-10 parts, isohexadecane 1-20 parts, isododecane 1-15 parts, cyclopentasiloxane 1-15 parts, dimethicone 1-15 parts, squalane 1-10 parts, hydrogenated polyisobutene 1-5 parts, phenyl dimethicone 1-15 parts, PRUNUS DOMESTICA seed extract 0.1-1 part, a complex of JUNIPERUS VIRGINIANA CALLUS EXTRACT (and) PADINA PAVONICA THALLUS EXTRACT 0.1-1 part, a complex of CAPRYLIC / CAPRIC TRIGLYCERIDE (and) TIPROFEN 0.1-1 part, a complex of HELIANTHUS ANNUUS (SUNFLOWER) SEED OIL (and) LUPINUS ALBUS SEED EXTRACT (and) TOCOPHEROL 0.1-1 part, HELIANTHUS ANNUUS (SUNFLOWER) SEED OIL UNSAPONIFIABLES 0.1-1 part, PASSIFLORA EDULIS SEED OIL 0.1-1 part, MAURITIA FLEXUOSA FRUIT OIL 0.1-1 part, by total mass of the sunscreen emulsion.

[0024] Further, the sunscreen agent includes 1 to 20 parts of a chemical sunscreen agent and 1 to 5 parts of a physical sunscreen agent, based on the total mass of the sunscreen cream.

[0025] Preferably, the mass ratio of the chemical sunscreen agent to the physical sunscreen agent is 1 to 20:1.

[0026] Further, the chemical sunscreen agent is selected from one or more of ethylhexyl methoxy cinnamate, ethylhexyl triazone, diethylamino hydroxybenzoyl hexyl benzoate, bis-ethylhexyloxyphenol methoxyphenyl triazine, homosalate, benzophenone-3, butyl methoxydibenzoylmethane, ethylhexyl salicylate, octocrylene, benzylidene camphor sulfonic acid and salts thereof, diethylhexyl butamido triazone, drometrizole trisiloxane, and ethylhexyl salicylate.

[0027] Further, the chemical sunscreen agent is selected from one or more of ethylhexyl methoxy cinnamate 1 to 10 parts, ethylhexyl triazone 1 to 10 parts, diethylamino hydroxybenzoyl hexyl benzoate 1 to 5 parts, bis-ethylhexyloxyphenol methoxyphenyl triazine 1 to 5 parts, homosalate 1 to 5 parts, benzophenone-3 1 to 5 parts, butyl methoxydibenzoylmethane 1 to 5 parts, ethylhexyl salicylate 1 to 5 parts, octocrylene 1 to 10 parts, benzylidene camphor sulfonic acid and salts thereof 1 to 4 parts, diethylhexyl butamido triazone 1 to 10 parts, drometrizole trisiloxane 1 to 15 parts, and ethylhexyl salicylate 1 to 5 parts, based on the total mass of the sunscreen cream.

[0028] Further, the physical sunscreen agent is selected from titanium dioxide and / or zinc oxide.

[0029] Further, the physical sunscreen agent is selected from titanium dioxide 1 to 10 parts and / or zinc oxide 1 to 10 parts, based on the total mass of the sunscreen cream.

[0030] Further, the anti-allergic agent is selected from one or more of dipotassium glycyrrhizinate, a complex of glycerin (and) water (and) glycerylphosphorylpopcitol choline salt (trade name: NP GPI Choline, glycerin: water: glycerylphosphorylpopcitol choline salt = 8:1:1), and a complex of Schisandra sphenanthera extract (and) maltodextrin (trade name: Sweetone Bio, Schisandra sphenanthera extract: maltodextrin = 50:50).

[0031] Preferably, based on the total mass percentage of the sunscreen lotion, the anti-allergy agent is selected from one or more of the following: 0.1-2 parts of dipotassium glycyrrhizate, 0.1-1 parts of a complex of glycerol (and) water (and) glycerophosphate inositol choline salt, and 0.1-1 parts of a complex of Schisandra spp. extract (and) maltodextrin.

[0032] Furthermore, the skin feel modifier is selected from one or more of silica, polymethylsilsesquioxane, and starch.

[0033] Furthermore, the preservative is selected from one or more of bis(hydroxymethyl)imidazolidinyl urea, iodopropynyl butylcarbamate, phenoxyethanol, and methylparaben.

[0034] Furthermore, based on the total mass percentage of the sunscreen lotion, the skin feel modifier is selected from one or more of the following: 1-5 parts silica, 1-5 parts polymethylsilsesquioxane, and 1-5 parts starch.

[0035] Furthermore, the pH adjuster includes an alkaline pH adjuster and an acidic pH adjuster, wherein the alkaline pH adjuster is selected from one or more of triethanolamine, sodium hydroxide, and potassium hydroxide, and the acidic pH adjuster is selected from citric acid and / or succinic acid.

[0036] Furthermore, chelating agents and / or colorants may be added to the sunscreen lotion;

[0037] Furthermore, based on the total mass percentage of the sunscreen lotion, the added chelating agent is 0.1 to 5 parts and / or colorant is 0.1 to 20 parts.

[0038] Further, based on the total mass percentage of the sunscreen lotion, the chelating agent is selected from disodium EDTA and / or tetrasodium EDTA; preferably, the chelating agent is selected from 0.01 to 0.2 parts of disodium EDTA and / or 0.01 to 0.2 parts of tetrasodium EDTA.

[0039] Furthermore, the colorant is selected from one or more of iron oxide black, iron oxide red, iron oxide yellow, titanium dioxide, and synthetic fluorophlogopite.

[0040] Secondly, this application also provides a method for preparing the water-resistant oil-in-water sunscreen lotion that reduces the transdermal penetration of chemical sunscreen agents, comprising the following steps:

[0041] S1. Mix the humectant, thickener, alkaline pH adjuster and water, heat, and stir thoroughly until completely transparent; set aside.

[0042] S2. Mix the emollient, emulsifier, sunscreen, and skin feel modifier evenly and heat until completely dissolved. Stir homogenously and set aside.

[0043] S3, heating the material prepared in step S1 to 80-95℃, slowly adding the material in step S2 under homogenization, and continuing homogenization after the addition is completed to obtain a premix;

[0044] S4, stirring the premix at a rotation speed of 500-1200 r / min, adding the anti-allergic agent, preservative, and acid pH regulator, mixing uniformly, and then reducing to room temperature to obtain the water-resistant oil-in-water sunscreen cream capable of reducing the penetration of chemical sunscreen agents through the skin.

[0045] Further, step S4 is replaced by: S4, stirring the premix at a rotation speed of 500-1200 r / min, reducing the temperature to 45-50℃, adding the anti-allergic agent, preservative, and acid pH regulator, mixing uniformly, and then reducing to room temperature to obtain the water-resistant oil-in-water sunscreen cream capable of reducing the penetration of chemical sunscreen agents through the skin.

[0046] Wherein, the mass percentage is based on 100 parts of the total mass of the water-resistant oil-in-water sunscreen cream capable of reducing the penetration of chemical sunscreen agents through the skin.

[0047] The water-resistant oil-in-water sunscreen cream capable of reducing the penetration of chemical sunscreen agents through the skin prepared in the present application uses C20-40 alcohol (Performacol 350 Alcohol) and C20-40 acid (Performacid 350 Acid) complex, or C20-40 acid (Performacid 350 Acid) and long carbon alcohol emulsifier complex as emulsifiers or one of the emulsifier components of the oil-in-water system, which can form a crystalline water-oil interface emulsion structure. Compared with the ordinary liquid type water-oil interface emulsion structure, it has large emulsion particle size and high interface structure strength, which can greatly improve the anti-migration property of the oil-in-water system, improve the stability of the oil-in-water emulsion particles, stably wrap the sunscreen agents in the emulsion particles, reduce the release of sunscreen agents from the oil-in-water system, thereby penetrating into the skin, reducing the irritation to the skin, improving the safety and anti-sensitivity of the sunscreen product of the oil-in-water system, and at the same time not affecting the penetration of water-soluble active substances through the skin, so as to achieve an intelligent penetration selectivity (separating substances that irritate the human body, such as chemical sunscreen agents, from the skin surface as much as possible, while not affecting the penetration of active substances beneficial to the human body, such as anti-allergic ingredients).

[0048] The application uses C20-40 alcohol (Performacol 350 Alcohol) and C20-40 acid (Performacid 350 Acid) to compound, or C20-40 acid (Performacid 350 Acid) and long carbon alcohol emulsifiers to compound, so that the emulsion has stronger film-forming property on the skin surface, realizes that the water resistance and friction resistance of the oil-in-water system can be greatly improved without adding a film-forming agent, realizes good adhesion, anti-shedding and sliding, persistent film-forming property, waterproof and sweat-proof, anti-friction and other effects, and has a light and moist skin feel without stickiness.

[0049] Further, the application preferably uses C20-40 alcohol (Performacol 350 Alcohol) and C20-40 acid (Performacid 350 Acid) which have relatively low polarity, which can significantly enhance the crystallinity of C20-40 alcohol (Performacol 350 Alcohol) and C20-40 acid (Performacid 350 Acid) during compounding with high-polarity sunscreen agents and oils, and form a crystalline emulsion interface by C20-40 alcohol and C20-40 acid and high-polarity chemical sunscreen agents or oils, forming a large-particle-size crystalline emulsion structure, while compounding with conventional non-polar oils can only form a small spherical conventional emulsion structure. Therefore, the application uses a compound of chemical sunscreen agents methoxy cinnamic acid ethylhexyl ester, ethylhexyl triazone, diethyl amino hydroxy benzoyl hexyl benzoate, and bis-ethylhexyloxyphenol methoxyphenyl triazine as high-polarity oils and sunscreen agents, and the compound of C20-40 alcohol (Performacol 350 Alcohol) and C20-40 acid (Performacid 350 Acid) together realizes the emulsification and film-forming effect of the water-resistant oil-in-water sunscreen emulsion that can reduce the percutaneous penetration of chemical sunscreen agents, improves the film-forming property of the emulsion, obtains good oil-in-water film-forming property in a non-film-forming agent addition system, and significantly improves the water resistance and friction resistance of the oil-in-water system. At the same time, since the added chemical sunscreen agent is an oil-soluble component, the chemical sunscreen agent is wrapped in the crystalline structure in the emulsion structure of the application, thereby reducing the possibility of direct contact between the chemical sunscreen agent and the skin during use, and thus significantly reducing the percutaneous penetration of the chemical sunscreen agent and significantly improving the safety of the sunscreen product.

[0050] The anti-allergic agent used in the low-permeable sunscreen emulsion prepared in the present application is selected from one or more of dipotassium glycyrrhizinate, a complex of glycerin (and) water (and) glycerylphosphorylcholine salt, and a complex of Schisandra sphenanthera extract (and) maltodextrin, wherein the complex of glycerin (and) water (and) glycerylphosphorylcholine salt and the complex of Schisandra sphenanthera extract (and) maltodextrin can significantly reduce the sensitization of chemical sunscreens and improve the sun protection factor and comfort of skin care sunscreen products.

[0051] Compared with the prior art, the present application has the following advantages:

[0052] The present application develops an anti-water type oil-in-water sunscreen emulsion containing a C20-40 alcohol (Performacol 350 Alcohol) and C20-40 acid (Performacid 350 Acid) complex, or a C20-40 acid (Performacid 350 Acid) and long carbon alcohol co-emulsifier complex, an oil-in-water emulsion with a large particle size crystalline emulsion structure, excellent stability, water resistance, anti-friction, and anti-falling, which can achieve the stability effect of a water-in-oil sunscreen emulsion, and has better waterproof performance than the oil-in-water emulsion in the prior art.

[0053] The anti-water type oil-in-water sunscreen emulsion of the present application uses a high-polarity chemical sunscreen or oil and a C20-40 alcohol (Performacol 350 Alcohol) and C20-40 acid (Performacid 350 Acid) complex, or a C20-40 acid (Performacid 350 Acid) and long carbon alcohol co-emulsifier complex, which greatly reduces the possibility of direct contact between chemical sunscreens and the skin, significantly reduces the transdermal penetration of chemical sunscreens, improves the safety of sunscreen products, has a mild and non-irritating use effect, and can be used for skin sensitive people and children.

[0054] (1) The anti-water type oil-in-water sunscreen emulsion of the present application can reduce the transdermal penetration of chemical sunscreens by adding chemical sunscreens and physical sunscreens, significantly improving the sunscreen performance of the sunscreen emulsion, further improving the sunscreen effect under the action of the emulsifier component containing a C20-40 alcohol (Performacol 350 Alcohol) and C20-40 acid (Performacid 350 Acid) complex, or a C20-40 acid (Performacid 350 Acid) and long carbon alcohol co-emulsifier complex, and the SPF value is more than 30.

[0055] (4) The water-resistant oil-in-water sunscreen emulsion of the present application can reduce the percutaneous penetration of chemical sunscreen agents, and has better spreadability, slight stickiness, a relatively dry skin, and an overall comfortable skin feel. BRIEF DESCRIPTION OF DRAWINGS

[0056] Figure 1 is a microstructure diagram of the oil-in-water sunscreen emulsion prepared in Example 1 of the present application under a microscope magnification of 200 times;

[0057] Figure 2 is a microstructure diagram of the oil-in-water sunscreen emulsion prepared in Example 1 of the present application under a microscope magnification of 500 times;

[0058] Figure 3 is a microstructure diagram of the oil-in-water sunscreen emulsion prepared in Example 1 of the present application under a polarized light microscope magnification of 500 times;

[0059] Figure 4 is a microstructure diagram of the oil-in-water sunscreen emulsion prepared in Example 5 of the present application under a microscope magnification of 500 times;

[0060] Figure 5 is a microstructure diagram of the oil-in-water sunscreen emulsion prepared in Comparative Example 1 under a microscope magnification of 200 times;

[0061] Figure 6 is a microstructure diagram of the oil-in-water sunscreen emulsion prepared in Comparative Example 1 under a polarized light microscope magnification of 500 times;

[0062] Figure 7 is a microstructure diagram of the oil-in-water sunscreen emulsion prepared in Comparative Example 6 under a polarized light microscope magnification of 500 times;

[0063] Figure 8 is the mouse skin penetration amount of the oil-in-water sunscreen emulsion prepared in Example 1 (Sample A in the figure) and Comparative Example 1 (Sample B in the figure);

[0064] Figure 9 is the mouse skin residence amount of the oil-in-water sunscreen emulsion prepared in Example 1 (Sample A in the figure) and Comparative Example 1 (Sample B in the figure). DETAILED DESCRIPTION

[0065] The experimental methods not specified in the following examples of the present application are generally carried out under conventional conditions, or under the conditions recommended by the manufacturers. The various common chemical reagents used in the examples are commercially available products.

[0066] Unless otherwise defined, all technical and scientific terms used in the present application have the same meaning as commonly understood by one of ordinary skill in the art to which the present application belongs. The terminology used in the specification of the present application is only for the purpose of describing specific embodiments and is not intended to limit the present application.

[0067] For the purposes of the present application, the technical solutions and advantages are made more clear, in the following detailed description, the description is only exemplary, and is not intended to limit the scope of the present application. In addition, in the following description, the description of the known structure and technology is omitted to avoid unnecessary confusion of the concept of the present application.

[0068] The following examples further describe the present application, but the examples are not intended to limit the scope of protection of the present application.

[0069] The source and model of the reagents, raw materials and other ingredients used in the embodiments of the present application are shown in Table 1.

[0070] Table 1 Source and model of reagents and raw materials

[0071] Preparation of water-resistant oil-in-water sunscreen emulsion capable of reducing percutaneous penetration of chemical sunscreen agents

[0072] The formula of the water-resistant oil-in-water sunscreen emulsion capable of reducing percutaneous penetration of chemical sunscreen agents of the present embodiment is shown in Table 2.

[0073] Table 2 Formula of water-resistant oil-in-water sunscreen emulsion capable of reducing percutaneous penetration

[0074] According to the formula in Table 2, the specific preparation steps of the water-resistant oil-in-water sunscreen emulsion capable of reducing percutaneous penetration of chemical sunscreen agents of the present embodiment are as follows:

[0075] S1, mix sodium magnesium lithium silicate and water, heat to 98-100℃, mix well at a stirring speed of 1000r / min, then cool to 80℃, add xanthan gum, mix well and make completely transparent, and reserve;

[0076] S2, gradually add propylene glycol, erythritol, and alkaline pH adjuster to step S1, mix well and make completely transparent, cool to room temperature, and reserve;

[0077] S3, mix the emollient, sunscreen agent, and skin feel modifier, heat to completely dissolve, and homogenize at a high speed of 12000r / min for 5min, and reserve;

[0078] S4, add the emulsifier to step S3, mix until completely dissolved, and heat to 80-95℃, and reserve;

[0079] S5, heat the mixture of step S2 to 80-95℃, slowly add the mixture of step S4 to the mixture of step S2 under homogenization (speed 12000r / min), continue homogenization for 2min after the addition is completed, and obtain a premix.

[0080] S6. Stir the premixed material with a stirring paddle at a speed of about 800 r / min and lower the temperature to 45℃. Then add the preservative, anti-allergen and acid pH adjuster, mix evenly and cool to room temperature to obtain a water-in-oil sunscreen lotion that can reduce the percutaneous penetration of chemical sunscreens.

[0081] Example 2: Preparation of a water-in-oil sunscreen emulsion that reduces the transdermal penetration of chemical sunscreens.

[0082] The water-resistant oil-in-water sunscreen formula of this embodiment, which can reduce the transdermal penetration of chemical sunscreens, is shown in Table 3.

[0083] Table 3. Formulas of water-in-oil sunscreens with low transdermal penetration.

[0084] According to the formula in Table 3, the specific preparation steps of the low transdermal penetration water-repellent oil-in-water sunscreen emulsion in this embodiment are as follows:

[0085] S1. Mix sodium magnesium lithium silicate and water, heat to 98-100℃, stir at 1000r / min until homogeneous, then cool to 80℃, add xanthan gum, stir thoroughly until completely transparent, and set aside.

[0086] S2. Gradually add propylene glycol, erythritol, and alkaline pH adjuster to step S1, stir thoroughly until completely transparent, cool to room temperature, and set aside.

[0087] S3. Mix the emollient, sunscreen, and skin feel modifier evenly, heat until completely dissolved, and homogenize at 12000r / min for 5 minutes. Set aside.

[0088] S4. Add the emulsifier to step S3, stir until completely dissolved, and heat to 80-95°C for later use;

[0089] S5. Heat the mixture from step S2 to 80-95°C. Under homogenization conditions (speed 12000 r / min), slowly add the mixture from step S4 to the mixture from step S2. After the addition is complete, continue homogenization for 2 minutes to obtain the premixed material.

[0090] S6. Stir the premixed material with a stirring paddle at a speed of about 800 r / min and lower the temperature to 45℃. Then add the preservative, anti-allergen and acid pH adjuster, mix evenly and cool to room temperature to obtain a water-in-oil sunscreen lotion that can reduce the percutaneous penetration of chemical sunscreens.

[0091] Example 3: Preparation of a water-resistant oil-in-water sunscreen emulsion that reduces the transdermal penetration of chemical sunscreens

[0092] The anti-water type oil-in-water sunscreen emulsion formula of the present embodiment which can reduce the percutaneous penetration of chemical sunscreen agents is shown in Table 4;

[0093] Table 4 Anti-water type oil-in-water sunscreen emulsion formula with low percutaneous penetration

[0094] According to the formula in Table 4, the specific preparation steps of the anti-water type oil-in-water sunscreen emulsion of the present embodiment which can reduce the percutaneous penetration of chemical sunscreen agents are as follows:

[0095] S1, mix sodium magnesium lithium silicate and water, heat to 98-100°C, mix uniformly at a stirring speed of 1000 r / min, then cool to 80°C, add xanthan gum, fully stir until completely transparent, and reserve;

[0096] S2, gradually add propylene glycol, erythritol, and alkaline pH adjuster to step S1, fully stir until completely transparent, cool to room temperature, and reserve;

[0097] S3, mix the emollients, sunscreen agents, and skin feel adjusters uniformly, heat to completely dissolve, and homogenize at 12000 r / min for 5 min, and reserve;

[0098] S4, add the emulsifiers to step S3, stir until completely dissolved, and heat to 80-95°C, and reserve;

[0099] S5, heat the mixture of step S2 to 0-95°C, slowly add the mixture of step S4 to the mixture of step S2 under homogenization (speed 12000 r / min), continue homogenizing for 2 min after the addition is complete, and obtain a premix;

[0100] S6, stir the premix with a stirring paddle at a stirring speed of about 800 r / min, and reduce the temperature to 45°C, then add the preservatives, anti-allergic agents, and acidic pH adjuster, mix uniformly, and cool to room temperature to obtain the anti-water type oil-in-water sunscreen emulsion which can reduce the percutaneous penetration of chemical sunscreen agents.

[0101] Preparation of the anti-water type oil-in-water sunscreen emulsion of the present embodiment which can reduce the percutaneous penetration of chemical sunscreen agents

[0102] The anti-water type oil-in-water sunscreen emulsion formula of the present embodiment which can reduce the percutaneous penetration of chemical sunscreen agents is shown in Table 5;

[0103] Table 5 Anti-water type oil-in-water sunscreen emulsion formula with low percutaneous penetration

[0104] According to the formula in Table 5, the specific preparation steps of the anti-water type oil-in-water sunscreen emulsion of the present embodiment which can reduce the percutaneous penetration of chemical sunscreen agents are as follows:

[0105] S1, sodium magnesium lithium silicate and water were mixed, heated to 98-100℃, mixed at a stirring speed of 1000 r / min, then cooled to 80℃, sodium hyaluronate was added, fully stirred until completely transparent, and reserved;

[0106] S2, propylene glycol, erythritol, and alkaline pH adjuster were gradually added to step S1, fully stirred until completely transparent, and cooled to room temperature, and reserved;

[0107] S3, emollients, sunscreens, and skin feel adjusters were mixed and heated until completely dissolved, and homogenized at 12000 r / min for 5 min, and reserved;

[0108] S4, emulsifiers were added to step S3, stirred until completely dissolved, and heated to 80-95℃, and reserved;

[0109] S5, the mixture of step S2 was heated to 80-95℃, and the mixture of step S4 was slowly added to the mixture of step S2 under homogenization (12000 r / min), and homogenized for another 2 min after the addition was completed, to obtain a premix;

[0110] S6, the premix was stirred with a stirring paddle at a stirring speed of about 800 r / min, and the temperature was reduced to 45℃, then preservatives, anti-allergic agents, and acidic pH adjusters were added, mixed uniformly, and cooled to room temperature to obtain the water-resistant oil-in-water sunscreen emulsion with reduced percutaneous penetration of chemical sunscreens.

[0111] Preparation of the water-resistant oil-in-water sunscreen emulsion with reduced percutaneous penetration of chemical sunscreens of Example 5

[0112] The formula of the water-resistant oil-in-water sunscreen emulsion with reduced percutaneous penetration of chemical sunscreens of this example is shown in Table 6;

[0113] Table 6 Formula of the water-resistant oil-in-water sunscreen emulsion with reduced percutaneous penetration

[0114] According to the formula in Table 6, the specific preparation steps of the water-resistant oil-in-water sunscreen emulsion with reduced percutaneous penetration of chemical sunscreens of this example are as follows:

[0115] S1, sodium magnesium lithium silicate and water were mixed, heated to 98-100℃, mixed at a stirring speed of 1000 r / min, then cooled to 80℃, sodium hyaluronate was added, fully stirred until completely transparent, and reserved;

[0116] S2, propylene glycol, erythritol, and alkaline pH adjuster were gradually added to step S1, fully stirred until completely transparent, and cooled to room temperature, and reserved;

[0117] S3, the emollient, sunscreen, skin feel modifier are mixed evenly and heated to complete dissolution, and high-speed homogenized at 12000 r / min for 5 min, ready for use;

[0118] S4, the emulsifier is added to step S3, stirred to complete dissolution, and heated to 80-95°C, ready for use;

[0119] S5, the mixture of step S2 is heated to 80-95°C, and the mixture of step S4 is slowly added to the mixture of step S2 under the condition of homogenization (speed 12000 r / min), and homogenized for 2 min after the addition is completed, to obtain a premix body;

[0120] S6, the premix body is stirred with a stirring paddle at a stirring speed of about 800 r / min, and the temperature is reduced to 45°C, then the preservative and the anti-allergic agent and the acidic pH adjuster are added, mixed evenly, and cooled to room temperature to obtain the water-resistant oil-in-water sunscreen cream capable of reducing the percutaneous penetration of chemical sunscreen agents.

[0121] Preparation of the oil-in-water sunscreen cream of Comparative Example 1

[0122] The main difference between the oil-in-water sunscreen cream formula of this comparative example and Example 1 is the emulsifier composition and content. In the oil-in-water sunscreen cream of this comparative example, the emulsifier composition is: C20-40 alcohol (Performacol 350 Alcohol) 1 part, cetyl stearyl alcohol polyether-20 (ALKONAT CE 200F) 2.3 parts, no alkaline pH adjuster and acidic pH adjuster is added, and water is added to make up the amount.

[0123] The preparation steps of the oil-in-water sunscreen cream of this comparative example are basically the same as those of Example 1.

[0124] Preparation of the oil-in-water sunscreen cream of Comparative Example 2

[0125] The main difference between the oil-in-water sunscreen cream formula of this comparative example and Example 1 is the emulsifier composition and content. In the oil-in-water sunscreen cream of this comparative example, C20-40 alcohol (Performacol 350 Alcohol) and C20-40 acid (Performacid 350 Acid) are not added in the emulsifier composition, cetyl stearyl alcohol polyether-20 (ALKONAT CE 200F) 3.3 parts, no alkaline pH adjuster and acidic pH adjuster is added, and water is added to make up the amount.

[0126] The preparation steps of the oil-in-water sunscreen cream of this comparative example are basically the same as those of Example 1.

[0127] Preparation of the oil-in-water sunscreen cream of Comparative Example 3

[0128] The sunscreen emulsion of the present comparative example is different from that of Example 1 in that the thickening agent component is different. In the sunscreen emulsion of the present comparative example, sodium magnesium lithium silicate is replaced by magnesium lithium silicate, and other components and preparation methods are the same as those of Example 1.

[0129] The preparation steps of the sunscreen emulsion of the present comparative example are basically the same as those of Example 1.

[0130] Preparation of the sunscreen emulsion of Comparative Example 4

[0131] The sunscreen emulsion of the present comparative example is different from that of Example 1 in that the thickening agent component is different. In the sunscreen emulsion of the present comparative example, the thickening agent is xanthan gum 0.52 parts, and sodium magnesium lithium silicate (Laponite-XLG XR) 0.25 parts, and other components and preparation methods are the same as those of Example 1.

[0132] The preparation steps of the sunscreen emulsion of the present comparative example are basically the same as those of Example 1.

[0133] Comparative Example 5

[0134] The sunscreen emulsion of the present comparative example is different from that of Example 4 in that the anti-allergic agent component and content are different. In the sunscreen emulsion of the present comparative example, the anti-allergic agent component (water (and) glycerin phosphatidylcholine salt (NP GPI Choline), Schisandra sphenanthera extract (and) maltodextrin compound (trade name Sweetone Bio, Schisandra sphenanthera, reduced amount supplemented with water) is not added, and other components and preparation methods are the same as those of Example 4.

[0135] The preparation steps of the sunscreen emulsion of the present comparative example are basically the same as those of Example 4.

[0136] Comparative Example 6

[0137] The sunscreen emulsion of the present comparative example is different from that of Example 1 in that the sunscreen agent component and content are different. In the sunscreen emulsion of the present comparative example, the chemical sunscreen agent component is not added, only the physical sunscreen component is added, and the emollient is supplemented, and other components are the same as those of Example 1.

[0138] The preparation steps of the sunscreen emulsion of the present comparative example are basically the same as those of Example 1.

[0139] Comparative Example 7

[0140] The sunscreen emulsion of the present comparative example is different from that of Example 1 in that the sunscreen agent component and content are different. In the sunscreen emulsion of the present comparative example, the sunscreen agent is composed of titanium dioxide 7.5 parts, zinc oxide 7 parts, and other components are the same as those of Example 1.

[0141] The preparation steps of the oil-in-water sunscreen emulsion of the present comparative example are basically consistent with those of Example 1.

[0142] Test Example One, Microstructure of Oil-in-Water Sunscreen Emulsion

[0143] The sunscreen emulsions prepared in Example 1, Example 5, Comparative Example 1 and Comparative Example 6 were observed under a microscope and a polarizing microscope, and the results are shown in Figures 1 to 7. As can be seen from the microstructure, the microstructure of the sunscreen emulsion prepared in Example 1 and Example 5 is an irregular rice grain type structure, and under the scale contrast, the emulsion particle size is mostly more than 10 μm. Under the polarizing microscope, it is found that the interface film has a clear bright light, which confirms the crystalline interface, large particle size and crystalline interface structure, and thus it is easier to adhere to the skin surface to form a film. The microstructure of the sunscreen emulsion prepared in Comparative Example 1 is a uniform spherical droplet, and the particle size is much smaller than 10 μm. Under the polarizing microscope, the oil-water interface is a circular shadow, which does not have crystallinity and is a liquid type interface film. The microstructure of the sunscreen emulsion prepared in Comparative Example 6 is a uniform spherical droplet, and the particle size is much smaller than 10 μm, indicating that C20-40 alcohol and C20-40 acid can form a unique large particle crystalline structure only when they are compounded with high-polarity sunscreen agents or oils, and cannot form a unique large particle crystalline structure with physical sunscreen agents or sunscreen powders alone, and thus it is difficult to form a stable emulsion to achieve water resistance, friction resistance and other effects.

[0144] Test Example Two, Sunscreen Performance Test of Oil-in-Water Sunscreen Emulsion

[0145] The sunscreen emulsions prepared in Examples 1 to 5 and Comparative Examples 1 to 2 and Comparative Examples 6 to 7 were tested for sunscreen effect, and the test method referred to the detection method of cosmetic sunscreen SPF in the 2015 edition of “Cosmetic Safety Specification”. The test results are shown in Table 7.

[0146] Table 7 Sunscreen Test Results

[0147] As can be seen from the test results in Table 7, the water-resistant oil-in-water sunscreen emulsion prepared in the present application, which can reduce the percutaneous penetration of chemical sunscreen agents, has good sunscreen performance. Compared with the physical sunscreen agent alone (Comparative Examples 6 to 7), the chemical sunscreen agent and the physical sunscreen agent are combined in Examples 1 to 3 and 5 to achieve better sunscreen effect, and the SPF value is more than 30.

[0148] Test Example Three, Water Resistance Test of Oil-in-Water Sunscreen Emulsion

[0149] The water resistance test was performed on the oil-in-water sunscreen emulsions prepared in Examples 1-5 and Comparative Examples 1-2 and 6-7 according to the General Water Resistance Test Method in Chapter 8, Section 3 of the 2015 edition of the Cosmetics Safety Standard. The SPF value of the test sample was determined after the following 40-minute water resistance test to evaluate the water resistance of the test sample:

[0150] (1) Apply the sunscreen emulsion sample to the skin test site and wait for 15-30 minutes or as required by the label instructions.

[0151] (2) The subject performs equal amount of activity in water or the water flow rotates at a moderate level for 20 minutes.

[0152] (3) Rest for 20 minutes after getting out of the water (do not use a towel to wipe the test site).

[0153] (4) Perform equal amount of activity in water for another 20 minutes.

[0154] (5) End the water activity and wait for the skin to dry (do not use a towel to wipe the test site).

[0155] (6) Perform ultraviolet irradiation and measurement according to the SPF measurement method specified in the standard.

[0156] Water resistance requirement: Refer to the SPF value indicated on the product label or the predicted SPF value before the water resistance test. If the measured value decreases by more than 50% after bathing, the product cannot be labeled as water-resistant. The application of the Cosmetics Hygiene Standard 2007 edition is based on the industry basis.

[0157] The water resistance test was performed on the sunscreen emulsions prepared in Examples 1-5 and Comparative Examples 1-2 and 6-7 according to the above method, and the test results are shown in Table 8.

[0158] Table 8 Water resistance test results

[0159] From the water resistance test results of the sunscreen emulsions in Table 8, it can be seen that the SPF values of the oil-in-water sunscreen emulsions prepared in Examples 1-5 do not decrease by more than 50% after 40 minutes of bathing, and have water resistance. The SPF values of the sunscreen emulsions prepared in Comparative Examples 1-2 decrease by more than 50% after 40 minutes of bathing, and have no water resistance at all. Therefore, it can be seen that the oil-in-water emulsifier composition prepared by compounding C20-40 alcohol (Performacol 350 Alcohol) and C20-40 acid (Performacid 350 Acid), or by compounding C20-40 acid (Performacid 350 Acid) and long-chain alcohol emulsifier (cetylstearyl alcohol) as one of the emulsifier components can significantly improve the water resistance of the oil-in-water sunscreen emulsion.

[0160] Secondly, the comparative example 6 basically loses water resistance after water resistance test, indicating that even if the oil-in-water emulsifier composition of C20-40 alcohol (Performacol 350 Alcohol) and C20-40 acid (Performacid 350 Acid) is used in the sunscreen cream, and the physical sunscreen agent is compounded alone, the good water resistance of the sunscreen cream cannot be achieved, which is due to the unique emulsion structure formed by C20-40 alcohol (Performacol 350 Alcohol) and C20-40 acid (Performacid 350 Acid) and the chemical sunscreen agent. Comparative example 7 still loses water resistance by using the same amount of physical sunscreen agent, which further verifies the technical scheme.

[0161] Test example four, sensory test of oil-in-water sunscreen cream

[0162] The sunscreen creams prepared in examples 1-5 and comparative examples 1-7 are subjected to sensory test in this test example, which specifically includes test of application feeling and skin feeling, and the test method is as follows:

[0163] Five volunteers are selected to apply the same amount of sample on the inner arm of the hand in a circular manner, and the extensibility, absorption speed, sticky feeling during absorption, skin feeling after complete absorption, and irritation and sensitivity of the cream are felt.

[0164] The test results according to the above test method are shown in Table 9.

[0165] Table 9 Sensory test results

[0166] As can be seen from the results in Table 9, the cream prepared in example 2 is thick due to excessive addition of C20-40 alcohol (Performacol 350 Alcohol) and C20-40 acid (Performacid 350 Acid), resulting in heavy skin feeling, but it can be made into a stable sunscreen cream, and only the skin feeling is slightly thick. The sunscreen creams prepared in examples 1, 3, 4, 5 and comparative examples 1-2 have high average extensibility, slight stickiness, dry skin, and comfortable overall skin feeling. The skin feeling of comparative examples 6-7 is refreshing and not sticky, mainly because of the absence of chemical sunscreen agent. The powder content of comparative example 7 is relatively high, and the application is obviously whitish, slightly muddy, and the use experience is poor. The sunscreen creams prepared in comparative examples 3-4 have thick and heavy skin feeling, and the use experience is relatively poor in sunscreen products which require refreshing texture.

[0167] Test example five, stability test of oil-in-water sunscreen agent

[0168] The stability of the oil-in-water sunscreen emulsion prepared in Examples 1-4, Comparative Examples 1-2 and Comparative Examples 6-7 was tested according to the following method.

[0169] (1) Centrifugal test at 2000 r / 30 min;

[0170] (2) Heat resistance test at 45°C / 30 days;

[0171] (3) Cold resistance test at -5°C / 30 days;

[0172] (4) Normal temperature / 30 days;

[0173] According to the above stability test method, the oil-in-water sunscreen emulsion prepared in Examples 1-4 and Comparative Examples 1-6 of the present application had excellent stability

[0174] The test results are shown in Table 10.

[0175] Table 10 Stability test results

[0176] As can be seen from the stability test data in Table 10, the oil-in-water sunscreen emulsion prepared in Examples 1-4 has excellent stability, can maintain the stability of the emulsion under external force, and has excellent heat resistance, cold resistance and storage stability at normal temperature. Comparative Examples 5-7 also have good stability, while the sunscreen emulsion prepared in Comparative Examples 1-4 shows stratification under centrifugation, indicating that the emulsification effect, molding property and emulsion uniformity of the emulsion are not good, the emulsion system is prone to separation under external force, and the emulsifier and thickening agent have certain influence on the heat resistance and cold resistance of the sunscreen emulsion, which cannot be stored for a long time at normal temperature.

[0177] Test Example Six, Transdermal Penetration Test of Oil-in-Water Sunscreen

[0178] In this test example, the transdermal penetration test of the oil-in-water sunscreen emulsion prepared in Example 1 and Comparative Example 1 was carried out, and the specific test method and experimental results are as follows.

[0179] First Part, Test Method

[0180] (1) Test method: determined by using a transdermal test instrument: transdermal diffusion cell, total volume 8.0 (V0) mL.

[0181] (2) Liquid chromatograph: quantitatively determined by using Agilent 1260 (with diode array detector).

[0182] (3) Animal test:

[0183] Mice: purchased from Southern Medical University, and the abdominal skin of isolated mice was selected for transdermal diffusion test.

[0184] Pre-treatment: the sample solution was prepared by taking about 2 g / 3.14 cm2 Standby.

[0185] Preparation of ex vivo mouse skin: Take 2 white mice and divide them into 2 groups: blank group, sample group. The mice were sacrificed by dislocation method. After the mice died, the back of the mouse was repeatedly wiped with depilatory agent. After 15 minutes, the back was rinsed with normal saline. Then the undamaged skin (area greater than diffusion cell) was removed by blunt separation method. The skin was soaked in normal saline for standby.

[0186] Selection of transdermal absorption solution: Fix the skin on the diffusion cell with the stratum corneum facing the supply chamber. Clamp it with a clamp. Fill the receiving chamber with the receiving solution. Remove the air under the skin so that the liquid surface is in contact with the mouse skin. Then apply the sample at 2g / 3.14cm 2 Uniformly apply the sample to the mouse skin. Take samples at 30min, 60min, 90min, 120min, 150min, and 180min, respectively. Each time take 2mL, and add an equal volume of receiving solution at the same temperature. The removed receiving solution is immediately filtered with a 0.22μm microporous filter. The skin residence amount is taken after 180min. The skin is removed, wiped 5 times with normal saline, and then washed 5 times with isopropyl alcohol. Then cut it into small pieces, shake it with 2mL isopropyl alcohol, and ultrasonicate it for 1h. Then filter and test.

[0187] (4) Verification basis: According to the literature (Guo Li, Xiong Wei, Lu Yubin, He Mei, Li Lei. In vitro release and transdermal comparison of different polar drugs in musk bone paste. Chinese pharmacist, 2022, 25(09): 1667-1671.)

[0188] Second part: Test results

[0189] The sunscreen emulsion prepared in Example 1 and Comparative Example 1 was subjected to a sunscreen transdermal penetration test according to the test method of the first part. The test results are as follows: see FIG. 8 and FIG. 9.

[0190] The transdermal absorption results of diethylaminohydroxybenzoyl hexyl benzoate (DHHB) in Example 1 (sample A) were as follows: the cumulative penetration amount was 0.537μg, the skin residence amount after 180min was 6.46μg, and the total penetration amount was 7.00μg. The transdermal absorption results of methoxyethylhexyl cinnamate (OMC) were as follows: the cumulative penetration amount was 0.91μg, the skin residence amount after 180min was 24.90μg, and the total penetration amount was 25.81μg. The transdermal absorption results of ethylhexyl triazone (T150) were as follows: the cumulative penetration amount was 0.00μg, the skin residence amount after 180min was 2.71μg, and the total penetration amount was 2.71μg. The transdermal absorption results of bis-ethylhexyloxyphenol methoxyphenyl triazine (BEMT) were as follows: the cumulative penetration amount was 0.00μg, the skin residence amount after 180min was 3.62μg, and the total penetration amount was 3.62μg.

[0191] The results of the transdermal absorption of diethylaminohydroxybenzoyl hexyl benzoate (DHHB) in Comparative Example 1 (Sample B) were a cumulative permeation amount of 1.35 μg, a skin resident amount of 15.33 μg after 180 min, and a total permeation amount of 16.68 μg; the results of the transdermal absorption of ethylhexyl methoxycinnamate (OMC) were a cumulative permeation amount of 3.958 μg, a skin resident amount of 42.87 μg after 180 min, and a total permeation amount of 46.83 μg; the results of the transdermal absorption of ethylhexyl triazone (T150) were a cumulative permeation amount of 0.14 μg, a skin resident amount of 6.79 μg after 180 min, and a total permeation amount of 6.93 μg; and the results of the transdermal absorption of bis-ethylhexyloxyphenol methoxyphenyl triazine (BEMT) were a cumulative permeation amount of 0.0000 μg, a skin resident amount of 5.27 μg after 180 min, and a total permeation amount of 5.27 μg.

[0192] As can be seen from FIG. 9 and the results of FIG. 9, by comparing the data of Example 1 (Sample A) and Example 2 (Sample B), Example 1 (Sample A) can significantly reduce the transdermal penetration of OMC, DHHB, T150, and BEMT chemical sunscreens.

[0193] For the sake of brevity, the above description of examples is quite specific and detailed to illustrate certain embodiments of the application, but it is not to be construed as limiting the scope of the patent. Those skilled in the art can combine and combine the features of different embodiments and features of different embodiments described in the specification without contradiction.

Claims

1. An oil-in-water sunscreen emulsion of water-resistant type which can reduce the percutaneous penetration of chemical sunscreen agents, characterized by, The sunscreen cream comprises 1-35 parts of sunscreen agent and 0.5-10 parts of emulsifier by mass percentage, the emulsifier comprises a first emulsifying component and a second emulsifying component, the first emulsifying component is C20-40 acid, the second emulsifying component is C20-40 alcohol and / or long carbon alcohol co-emulsifier, and the long carbon alcohol co-emulsifier is selected from one or more of lauryl alcohol, cetyl alcohol, stearyl alcohol, cetearyl alcohol and behenyl alcohol.

2. The water-resistant oil-in-water sunscreen emulsion capable of reducing percutaneous penetration of chemical sunscreen agents according to claim 1, wherein The emulsifier comprises 0.1-5 parts of C20-40 acid by mass percentage, and further comprises 0.1-5 parts of C20-40 alcohol and / or 0.1-5 parts of long carbon alcohol co-emulsifier.

3. The water-resistant oil-in-water sunscreen emulsion capable of reducing percutaneous penetration of chemical sunscreen agents according to claim 2, characterized by, The emulsifier comprises 0.1-5 parts of C20-40 alcohol and 0.1-5 parts of C20-40 acid.

4. The water-resistant oil-in-water sunscreen emulsion capable of reducing percutaneous penetration of chemical sunscreen agents according to claim 3, characterized by, The mass ratio of the C20-40 alcohol to the C20-40 acid is 1:(0.5-5).

5. The water-resistant oil-in-water sunscreen emulsion capable of reducing percutaneous penetration of chemical sunscreen agents according to claim 1, wherein The emulsifier further comprises one or more of ceteareth-20, glyceryl stearate, PEG-100 stearate, sucrose ester oil-in-water emulsifier, and PEG-containing oil-in-water emulsifier.

6. The water-resistant oil-in-water sunscreen emulsion capable of reducing percutaneous penetration of chemical sunscreen agents according to claim 1, wherein The mass ratio of the C20-40 alcohol, the C20-40 acid and the ceteareth-20 in the emulsifier is 1:(0.5-5):(0.1-3).

7. The water-resistant, oil-in-water sunscreen emulsion with reduced percutaneous penetration of chemical sunscreen agent according to claim 1, wherein, The sunscreen agent comprises a chemical sunscreen agent and a physical sunscreen agent.

8. The water-resistant, oil-in-water sunscreen emulsion with reduced percutaneous penetration of chemical sunscreen agent according to claim 7, wherein, The sunscreen agent comprises 1-20 parts of chemical sunscreen agent and 1-5 parts of physical sunscreen agent by mass percentage of the total mass of the sunscreen cream.

9. The water-resistant oil-in-water sunscreen emulsion capable of reducing percutaneous penetration of chemical sunscreen agents according to claim 7 or 8, characterized by, The chemical sunscreen agent is selected from one or more of ethylhexyl methoxy cinnamate, ethylhexyl triazone, diethylamino hydroxybenzoyl hexyl benzoate, bis-ethylhexyloxyphenol methoxyphenyl triazine, homosalate, benzophenone-3, butyl methoxydibenzoylmethane, ethylhexyl salicylate, octocrylene, benzylidene camphor sulfonic acid and salts thereof, diethylhexyl butamido triazone, phenylbenzimidazole sulfonic acid, and ethylhexyl salicylate.

10. The water-resistant, oil-in-water sunscreen emulsion that reduces percutaneous penetration of chemical sunscreens according to claim 9, wherein, The chemical sunscreen agent is selected from one or more of ethylhexyl methoxy cinnamate 1-10 parts, ethylhexyl triazone 1-10 parts, diethylamino hydroxybenzoyl hexyl benzoate 1-5 parts, bis-ethylhexyloxyphenol methoxyphenyl triazine 1-5 parts, homosalate 1-5 parts, benzophenone-3 1-5 parts, butyl methoxydibenzoylmethane 1-5 parts, ethylhexyl salicylate 1-5 parts, octocrylene 1-10 parts, benzylidene camphor sulfonic acid and salts thereof 1-4 parts, diethylhexyl butamido triazone 1-10 parts, phenylbenzimidazole sulfonic acid 1-15 parts, and ethylhexyl salicylate 1-5 parts by mass percentage of the total mass of the sunscreen cream.

11. The water-resistant oil-in-water sunscreen emulsion capable of reducing percutaneous penetration of chemical sunscreen agents according to claim 7 or 8, characterized by, The physical sunscreen agent is selected from titanium dioxide and / or zinc oxide.

12. The water-resistant, oil-in-water sunscreen emulsion that reduces percutaneous penetration of chemical sunscreens according to claim 11, wherein, The physical sunscreen agent is selected from titanium dioxide 1-10 parts and / or zinc oxide 1-10 parts by mass percentage of the total mass of the sunscreen cream.

13. The water-resistant, oil-in-water sunscreen emulsion capable of reducing percutaneous penetration of chemical sunscreen agents according to claim 7 or 8, characterized by, The mass ratio of the chemical sunscreen agent to the physical sunscreen agent is 1-20:

1.

14. The water-resistant, oil-in-water sunscreen emulsion with reduced percutaneous penetration of chemical sunscreen agent according to claim 1, wherein, The sunscreen cream further comprises a combination of one or more of humectant, thickening agent, emollient, anti-allergic agent, pH adjusting agent, skin feel modifier, preservative, chelating agent, coloring agent, and water.

15. The water-resistant, oil-in-water sunscreen emulsion that reduces percutaneous penetration of chemical sunscreens according to claim 14, wherein, The sunscreen cream further comprises a humectant, a thickening agent, an emollient, an emulsifier, a sunscreen agent, an anti-allergic agent, a pH adjusting agent, a skin feel adjusting agent, a preservative and water.

16. The water-resistant, oil-in-water sunscreen emulsion that reduces percutaneous penetration of chemical sunscreens according to claim 15, wherein, The sunscreen cream comprises, by mass percentage, 1-25 parts of a humectant, 0.1-15 parts of a thickening agent, 1-50 parts of an emollient, 0.5-10 parts of an emulsifier, 1-35 parts of a sunscreen agent, 0.1-5 parts of an anti-allergic agent, 0.1-3 parts of a pH adjusting agent, 1-10 parts of a skin feel adjusting agent, 0.1-5 parts of a preservative and 20-80 parts of water.

17. The water-resistant, oil-in-water sunscreen emulsion that reduces percutaneous penetration of chemical sunscreen agents according to any one of claims 14 to 16, characterized in that, The thickening agent comprises one or more of xanthan gum, sodium magnesium lithium silicate, carbomer, sodium polyacryloyldimethyl taurate; the humectant is selected from one or more of glycerin, propylene glycol, erythritol, butylene glycol, pentylene glycol, sodium hyaluronate, ceramide, polysaccharide; the emollient is selected from one or more of dicaprylyl ether, ethylhexyl palmitate, caprylic / capric triglyceride, isononyl isononanoate, propylene glycol dicaprylate / dicaprate, dicaprylyl carbonate, coco-caprylate / caprate, mineral oil, octyldodecanol, isohexadecane, isododecane, cyclopentasiloxane, dimethicone, squalane, hydrogenated polyisobutene, phenyl dimethicone, a complex of European buckthorn seed extract, jojoba seed oil and Phormidium faveloides thallus extract, caprylic / capric triglyceride and teprenone, a complex of sunflower seed oil and Lupinusalbus seed extract and tocopherol, sunflower seed oil unsaponifiables, physalis peruviana seed oil, moringa oleifera seed oil; the anti-allergic agent is selected from one or more of dipotassium glycyrrhizinate, a complex of glycerin and water and glycerophosphoinositol choline salt, a complex of Schisandra sphenanthera extract and maltodextrin; the pH adjusting agent is selected from a basic pH adjusting agent and / or an acidic pH adjusting agent, the basic pH adjusting agent is selected from one or more of triethanolamine, sodium hydroxide, potassium hydroxide, the acidic pH adjusting agent is selected from citric acid and / or succinic acid; the skin feel adjusting agent is selected from one or more of silica, polymethylsilsesquioxane, starch; the preservative is selected from one or more of bis(hydroxymethyl)imidazolinyl urea, iodopropynyl butylcarbamate, phenoxyethanol, hydroxybenzoic acid ester.

18. The water-resistant, oil-in-water sunscreen emulsion that reduces percutaneous penetration of chemical sunscreens according to claim 14, wherein, The sunscreen cream further comprises a chelating agent and / or a coloring agent, the chelating agent is selected from disodium EDTA and / or tetrasodium EDTA; the coloring agent is selected from one or more of black iron oxide, red iron oxide, yellow iron oxide, titanium dioxide, synthetic fluorphlogopite.

19. The water-resistant, oil-in-water sunscreen emulsion that reduces percutaneous penetration of chemical sunscreens according to claim 18, wherein, The chelating agent is added in an amount of 0.1-5 parts and / or the coloring agent is added in an amount of 0.1-20 parts, by mass percentage of the total mass of the sunscreen cream.

20. The water-resistant, oil-in-water sunscreen emulsion that reduces percutaneous penetration of chemical sunscreens according to claim 18, wherein, The chelating agent is selected from disodium EDTA in an amount of 0.01-0.2 parts and / or tetrasodium EDTA in an amount of 0.01-0.2 parts, by mass percentage of the total mass of the sunscreen cream.

21. The water-resistant, oil-in-water sunscreen emulsion that reduces percutaneous penetration of chemical sunscreens according to claim 17, wherein, The thickening agent is selected from a complex of xanthan gum and sodium magnesium lithium silicate; the mass ratio of the xanthan gum to the sodium magnesium lithium silicate is 1:1-6.

22. The water-resistant, oil-in-water sunscreen emulsion that reduces percutaneous penetration of chemical sunscreens according to claim 17, wherein, The humectant is any combination of propylene glycol, sodium hyaluronate and erythritol; the mass ratio of the sodium hyaluronate to the propylene glycol to the erythritol is 0-1:5-15:

5.

23. The water-resistant, oil-in-water sunscreen emulsion with reduced percutaneous penetration of chemical sunscreen agent according to claim 17, wherein, The humectant is selected from one or more of glycerin 1-10 parts, propylene glycol 1-10 parts, erythritol 1-10 parts, butylene glycol 1-10 parts, pentylene glycol 1-10 parts, sodium hyaluronate 0.01-5 parts, ceramide 0.1-5 parts, polysaccharide 1-10 parts, by 100% of the total mass of the sunscreen cream.

24. The water-resistant, oil-in-water sunscreen emulsion with reduced percutaneous penetration of chemical sunscreen agent according to claim 17, wherein, The emollient is selected from one or more of dioctyl ether 1-20 parts, ethylhexyl palmitate 1-10 parts, caprylic / capric triglyceride 1-10 parts, isononyl isononanoate 1-15 parts, propylene glycol dicaprylate / dicaprate 1-10 parts, dicapryl carbonate 1-10 parts, coco- caprylate / caprate 1-10 parts, mineral oil 1-20 parts, octyldodecanol 1-10 parts, isohexadecane 1-20 parts, isododecane 1-15 parts, cyclomethicone 1-15 parts, dimethicone 1-15 parts, squalane 1-10 parts, hydrogenated polyisobutene 1-5 parts, phenyl dimethicone 1-15 parts, European plum seed extract 0.1-1 parts, a complex of jojoba seed oil and powdery funaria hygrometric leaf thallus extract 0.1-1 parts, a complex of caprylic / capric triglyceride and teprenone 0.1-1 parts, a complex of sunflower seed oil and white lupine seed extract and tocopherol 0.1-1 parts, sunflower seed oil unsaponifiables 0.1-1 parts, passion fruit seed oil 0.1-1 parts, moringa oleifera seed oil 0.1-1 parts, by parts of the total mass of the sunscreen cream.

25. The water-resistant, oil-in-water sunscreen emulsion with reduced percutaneous penetration of chemical sunscreen agent according to claim 17, wherein, The anti-allergic agent is selected from one or more of dipotassium glycyrrhizate 0.1-2 parts, a complex of glycerin and water and glycerophosphoinositol choline salt 0.1-1 parts, a complex of kadsura japonica extract and maltodextrin 0.1-1 parts, by parts of the total mass of the sunscreen cream.

26. The water-resistant, oil-in-water sunscreen emulsion with reduced percutaneous penetration of chemical sunscreen agent according to claim 17, wherein, The skin feel modifier is selected from one or more of silica 1-5 parts, polymethylsilsesquioxane 1-5 parts, starch 1-5 parts, by parts of the total mass of the sunscreen cream.

27. A method of preparing a water-resistant, oil-in-water sunscreen emulsion that reduces the percutaneous penetration of chemical sunscreens, comprising: The method comprises the following steps: S1, mix the humectant, thickening agent, alkaline pH regulator and water, heat, fully stir evenly to complete transparency, standby; S2, mix the emollient, emulsifier, sunscreen, skin feel modifier evenly, heat to complete dissolution, homogenize and stir evenly, standby; S3, heat the material prepared in step S1 to 80-95℃, slowly add the material obtained in step S2 under homogenization conditions, continue to homogenize evenly after adding, obtain a premix; S4, stir the premix at a speed of 500-1200 r / min, add the anti-allergic agent, preservative and acidic pH regulator, mix evenly, then cool to room temperature, obtain the water-resistant oil-in-water sunscreen cream capable of reducing the percutaneous penetration of chemical sunscreen agents.

28. The method of claim 27, wherein, S4 is replaced by: S4, stir the premix at a speed of 500-1200 r / min, cool to 45-50℃, add the anti-allergic agent, preservative and acidic pH regulator, mix evenly, then cool to room temperature, obtain the water-resistant oil-in-water sunscreen cream capable of reducing the percutaneous penetration of chemical sunscreen agents.

Citation Information

Patent Citations

  • Low irritation type multi-emulsifying sunscreen cosmetic and preparation method thereof

    CN109549859A

  • Sunscreen composition containing carboxylic acid functional group polyvinyl and polyvinyl mixture

    CN1316239A

  • Makeup composition

    CN1823705A

  • Cosmetic or dermatological light-protective formulation comprising a water-soluble UV filter substance and a benzoxazole derivative

    US20050048009A1

  • Cosmetic or dermatological light protection formulation with a benzoxazole derivative

    US20050142080A1