A composition suitable for use in an oil-in-water sunscreen system and uses thereof

Abstract

The present application relates to a kind of compositions suitable for oil-in-water sunscreen system and its application.The composition includes polysorbate, polyethylene glycol methyl ether dimethicone, dextrin palmitate and hydrolyzed royal jelly protein.The composition formula is safe and non-irritating, has excellent sunscreen performance, and is easier to prepare stable oil-in-water sunscreen product, without cleaning product removal, and water washable.

Description

Technical Field

[0001] This invention belongs to the field of cosmetic technology, specifically relating to a composition suitable for water-in-oil sunscreen systems and its application. Background Technology

[0002] Ultraviolet (UV) rays damage skin cells, leading to sunburn, photoaging (wrinkles, age spots), and long-term exposure may increase the risk of skin cancer. Children's skin is thinner and more sensitive, making it more susceptible to UV damage, and this damage can accumulate and have lifelong effects. Children's pure physical sunscreens contain no chemical sunscreens, reducing the risk of allergies and irritation; they are not easily absorbed by the skin, making them suitable for sensitive skin; they are also highly stable and do not easily break down; they take effect immediately after application, requiring no waiting time, making them suitable for active children.

[0003] Water-in-oil physical sunscreens have a lighter texture and a refreshing feel compared to oil-in-water physical sunscreens; they are also easier to wash off, reducing the risk of adverse reactions during makeup removal; and they are more compatible and less likely to pill. However, to meet SPF requirements, they generally contain more physical sunscreen powder, and to enhance stability, they often contain large amounts of oil dispersants and emulsifiers, which can lead to a heavy feel and difficulty in washing off.

[0004] Therefore, developing a composition suitable for water-in-oil sunscreen systems that can improve sun protection while enhancing skin feel and reducing wash-off difficulty has become one of the urgent technical problems to be solved. Summary of the Invention

[0005] To address the shortcomings of existing technologies, the present invention aims to provide a composition suitable for water-in-oil sunscreen systems and its application. This composition exhibits excellent sun protection properties, facilitates the preparation of stable water-in-oil sunscreen products, and is washable with water without the need for product removal.

[0006] To achieve this objective, the present invention adopts the following technical solution:

[0007] In a first aspect, the present invention provides a composition suitable for an oil-in-water sunscreen system, the composition comprising polysorbate, polyethylene glycol methyl ether polydimethylsiloxane, dextrin palmitate and hydrolyzed royal jelly protein.

[0008] Polysorbate has a good balance of hydrophilicity and lipophilicity, which enhances the solubility of the system in water and facilitates post-use cleanup. Polyethylene glycol methyl ether (PEG-DME) combines the hydrophobicity of silicone oil with the hydrophilicity of polyethylene glycol, improving the skin feel of sunscreen products and making them easier to remove with water. It also works synergistically with polysorbate to further enhance the washability of the system. This invention creatively discovers that the combined use of polysorbate and PEG-DME results in a better water-washability than either polysorbate or PEG-DME alone, indicating a significant synergistic effect in improving the water-washability of sunscreen products.

[0009] Dextrin palmitate is a fatty acid ester extracted from palm oil. It can form a network gel structure, acting as a thickener for oils and improving the adhesion of sunscreen agents to the skin surface. Hydrolyzed royal jelly protein is a mixture of small-molecule peptides or amino acids obtained from royal jelly through hydrolysis processes (such as enzymatic hydrolysis). It retains the active ingredients of royal jelly, has a small molecular weight, and exhibits good water solubility and skin permeability. This invention creatively discovers that the combined use of dextrin palmitate and hydrolyzed royal jelly protein significantly enhances the sun protection effect of sunscreen products compared to either dextrin palmitate or hydrolyzed royal jelly protein alone, indicating a significant synergistic effect between the two in improving sun protection efficacy.

[0010] Preferably, in the polysorbate, the fatty acids esterified with sorbitol are selected from dodecanoic acid, hexadecanoic acid, octadecanoic acid, or octadecenoic acid.

[0011] Preferably, the polysorbate is polysorbate-60.

[0012] Preferably, the number of repeating units of polyethylene glycol in the polyethylene glycol methyl ether polydimethylsiloxane is 8-15, for example, 8, 10, 11, 15, etc.

[0013] Preferably, the polyethylene glycol methyl ether polydimethylsiloxane is PEG-11 methyl ether polydimethylsiloxane.

[0014] Preferably, the composition comprises, by weight parts, 0.3-0.8 parts of polysorbate, 0.05-0.3 parts of polyethylene glycol methyl ether polydimethylsiloxane, 0.1-0.5 parts of dextrin palmitate and 0.05-0.3 parts of hydrolyzed royal jelly protein.

[0015] Specifically, the specific point values ​​for 0.3-0.8 parts can be 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, etc.; the specific point values ​​for 0.05-0.3 parts can be 0.05, 0.1, 0.15, 0.2, 0.25, 0.3, etc.; the specific point values ​​for 0.1-0.5 parts can be 0.1, 0.15, 0.2, 0.25, 0.3, 0.35, 0.4, 0.45, 0.5, etc.; and the specific point values ​​for 0.05-0.3 parts can be 0.05, 0.1, 0.15, 0.2, 0.25, 0.3, etc.

[0016] Preferably, the composition further includes glyceryl behenate.

[0017] Glyceryl behenate is an ester compound formed by the esterification reaction of behenic acid and glycerol. Its molecule simultaneously contains the hydrophilic polyhydroxyl segments from the glycerol structure and the hydrophobic structure of the long carbon chain of behenic acid. This invention creatively discovers that the combined use of glyceryl behenate and polyethylene glycol methyl ether polydimethylsiloxane significantly improves the refreshing feel of sunscreen products compared to using either glyceryl behenate or polyethylene glycol methyl ether polydimethylsiloxane alone, indicating a significant synergistic effect in enhancing the refreshing feel of sunscreen products.

[0018] Preferably, the composition comprises, by weight parts, 0.3-0.8 parts of polysorbate, 0.05-0.3 parts of polyethylene glycol methyl ether polydimethylsiloxane, 0.1-0.5 parts of dextrin palmitate, 0.05-0.3 parts of hydrolyzed royal jelly protein, and 0.1-0.8 parts of glyceryl behenate.

[0019] Specifically, for the 0.3-0.8 parts range, the specific point values ​​can be 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, etc.; for the 0.05-0.3 parts range, the specific point values ​​can be 0.05, 0.1, 0.15, 0.2, 0.25, 0.3, etc.; and for the 0.1-0.5 parts range, the specific point values ​​can be 0.1, 0.15, 0.2, 0.2, etc. 5 parts, 0.3 parts, 0.35 parts, 0.4 parts, 0.45 parts, 0.5 parts, etc. Specific point values ​​in the range of 0.05-0.3 parts can be 0.05 parts, 0.1 parts, 0.15 parts, 0.2 parts, 0.25 parts, 0.3 parts, etc. Specific point values ​​in the range of 0.1-0.8 parts can be 0.1 parts, 0.2 parts, 0.3 parts, 0.4 parts, 0.5 parts, 0.6 parts, 0.7 parts, 0.8 parts, etc.

[0020] Preferably, the hydrolyzed royal jelly protein is prepared using a method comprising the following steps:

[0021] (1) Mix royal jelly with water and microwave it. After microwave treatment, filter and collect the filtrate to obtain the pretreated solution.

[0022] (2) The pretreatment solution is mixed with the compound enzyme and enzymatic hydrolysis is carried out to obtain the enzymatic hydrolysate. The enzymatic hydrolysate is filtered and the filtrate is collected to obtain hydrolyzed royal jelly protein.

[0023] The complex enzyme in step (2) includes papain, trypsin and neutral protease.

[0024] In the preparation process of hydrolyzed royal jelly protein, this invention first microwaves the royal jelly and then enzymatically hydrolyzes the pretreated liquid obtained after microwave treatment. This allows for better hydrolysis of the royal jelly raw material, resulting in a mixture of small molecule peptides with superior sun protection and enhancement effects.

[0025] This invention utilizes a complex enzyme to enzymatically hydrolyze the pretreatment solution. Papain, a cysteine ​​protease, can hydrolyze various protein substrates and exhibits relatively broad peptide bond specificity, favoring the hydrolysis of peptide bonds containing aromatic amino acids such as phenylalanine, tyrosine, and tryptophan, or hydrophobic amino acids such as leucine and valine. Trypsin, a serine protease, can hydrolyze peptide bonds at the carboxyl terminus of basic amino acids such as lysine and arginine in proteins. Meanwhile, neutral protease possesses high catalytic efficiency and broad substrate adaptability. This invention creatively discovers that the combined use of papain, trypsin, and neutral protease in the enzymatic hydrolysis of royal jelly pretreatment solution not only retains the active components of royal jelly protein but also demonstrates better compatibility with physical sunscreens such as titanium dioxide, further enhancing the sun protection effect of the prepared hydrolyzed royal jelly protein.

[0026] Preferably, the ratio of royal jelly to water in step (1) is 1:5-1:20 g / mL, for example, it can be 1:5 g / mL, 1:10 g / mL, 1:15 g / mL, 1:20 g / mL, etc.

[0027] Preferably, the microwave treatment temperature in step (1) is 50-80℃, the microwave treatment power is 200-500 W, and the microwave treatment time is 10-30 min.

[0028] Among them, the specific point values ​​in 50-80℃ can be 50℃, 60℃, 70℃, 80℃, etc.; the specific point values ​​in 200-500 W can be 200 W, 250 W, 300 W, 350 W, 400 W, 450 W, 500 W, etc.; and the specific point values ​​in 10-30 min can be 10 min, 15 min, 20 min, 25 min, 30 min, etc.

[0029] Preferably, the mass ratio of the pretreatment solution to the compound enzyme in step (2) is 100:1-100:5, the temperature of the enzymatic hydrolysis reaction is 30-50℃, and the time of the enzymatic hydrolysis reaction is 0.5-2 h.

[0030] Among them, the specific point values ​​in the range of 100:1-100:5 can be 100:1, 100:2, 100:3, 100:4, 100:5, etc.; the specific point values ​​in the range of 30-50℃ can be 30℃, 35℃, 40℃, 45℃, 50℃, etc.; and the specific point values ​​in the range of 0.5-2 h can be 0.5 h, 1 h, 1.5 h, 2 h, etc.

[0031] Preferably, the mass ratio of papain, trypsin and neutral protease in step (2) is (1-3):(0.5-1):(0.1-0.5).

[0032] Among them, the specific point values ​​in 1-3 can be 1, 1.5, 2, 2.5, 3, etc.; the specific point values ​​in 0.5-1 can be 0.5, 0.6, 0.7, 0.8, 0.9, 1, etc.; and the specific point values ​​in 0.1-0.5 can be 0.1, 0.2, 0.3, 0.4, 0.5, etc.

[0033] In a second aspect, the present invention provides a water-in-oil type sunscreen, wherein the water-in-oil type sunscreen comprises the composition described in the first aspect, a physical sunscreen agent, a stabilizer, an emulsifier, a thickener, an antioxidant, water, an optional humectant, and an optional dispersant.

[0034] Preferably, the physical sunscreen agent comprises titanium dioxide modified with a surface treatment agent.

[0035] Preferably, the surface treatment agent comprises any one or a combination of at least two of silica, aluminum hydroxide, or triethoxyoctylsilane.

[0036] Preferably, the stabilizer comprises octyl polymethylsiloxane and isononyl isononanoate.

[0037] Octyl polymethylsiloxane possesses characteristics such as low surface tension, good lubricity, and strong hydrophobicity. It exhibits good compatibility with titanium dioxide surfaces, allowing it to adsorb onto particle surfaces, reducing inter-particle attraction and preventing agglomeration. Isonononyl isononanoate, a branched fatty acid ester formed by the esterification reaction of isononanoic acid and isononol, possesses strong solubility, excellent powder dispersibility, and excellent compatibility with other ingredients in sunscreens. This invention creatively discovers that octyl polymethylsiloxane and isonononyl isononanoate have a significant synergistic effect in improving the stability of the water-in-oil sunscreen involved in this invention.

[0038] Preferably, the mass ratio of octyl polymethylsiloxane to isononyl isononanoate is 1:1 to 1:4, for example, it can be 1:1, 1:1.5, 1:2, 1:2.5, 1:3.5, 1:4.5, 1:4, etc.

[0039] Preferably, the emulsifier comprises cocoyl glucoside-cocoyl alcohol complex and / or cetearyl alcohol.

[0040] Preferably, the thickener includes polyacrylamide, lauryl alcohol polyether, C13-14 isoparaffin, water complex and / or xanthan gum.

[0041] Preferably, the antioxidant includes p-hydroxyacetophenone.

[0042] Preferably, the moisturizer includes any one or a combination of at least two of glycerin, 1,3-propanediol, and 1,2-hexanediol.

[0043] Preferably, the dispersant comprises polyhydroxystearic acid.

[0044] Preferably, by weight, the water-in-oil sunscreen comprises 0.5-2.5 parts of the composition described in the first aspect, 5-10 parts of physical sunscreen agent, 5-10 parts of stabilizer, 2-4 parts of emulsifier, 0.3-2 parts of thickener, 0.2-0.8 parts of antioxidant, 5-10 parts of moisturizer, and 60-85 parts of water.

[0045] Specifically, for the range of 0.5-2.5 parts, the specific point values ​​can be 0.5 parts, 1 part, 1.5 parts, 2 parts, 2.5 parts, etc.; for the range of 5-10 parts, the specific point values ​​can be 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, etc.; for the range of 2-4 parts, the specific point values ​​can be 2 parts, 2.5 parts, 3 parts, 3.5 parts, 4 parts, etc.; and for the range of 0.3-2 parts, the specific point values ​​can be 0.3 parts, 0.6 parts, 0.9 parts, 1 part, etc. 2 parts, 1.5 parts, 1.8 parts, 2 parts, etc.; for 0.2-0.8 parts, specific point values ​​can be 0.2 parts, 0.4 parts, 0.6 parts, 0.8 parts, etc.; for 0.2-0.4 parts, specific point values ​​can be 0.2 parts, 0.25 parts, 0.3 parts, 0.35 parts, 0.4 parts, etc.; for 60-85 parts, specific point values ​​can be 60 parts, 65 parts, 70 parts, 75 parts, 80 parts, 85 parts, etc.

[0046] The water-in-oil type sunscreen of the present invention does not require the addition of a large amount of physical sunscreen agents. Excellent sun protection effect can be achieved by adding the composition suitable for water-in-oil sunscreen system described in the first aspect. At the same time, the sunscreen does not require the addition of a large amount of surfactants. The addition of a small amount of stabilizer greatly improves the stability of the product. At the same time, it does not cause a heavy feeling on the skin and is easy to wash off.

[0047] The numerical range described in this invention includes not only the point values ​​listed above, but also any point values ​​within the numerical ranges not listed above. Due to space limitations and for the sake of brevity, this invention will not exhaustively list all the specific point values ​​included in the range.

[0048] Compared with the prior art, the present invention has the following beneficial effects:

[0049] The composition of the present invention applicable to the water-in-oil sunscreen system has excellent sun protection performance and is easier to prepare stable water-in-oil sunscreen products. At the same time, it does not require cleaning product removal and can be washed with water.

[0050] Furthermore, glyceryl behenate is added to the composition, which has a significant synergistic effect with polyethylene glycol methyl ether polydimethylsiloxane in improving the refreshing feel of sunscreen products.

[0051] Furthermore, in the preparation process of hydrolyzed royal jelly protein, this invention first microwaves the royal jelly, then enzymatically hydrolyzes the pretreated solution obtained after microwave treatment. This allows for better hydrolysis of the royal jelly, resulting in a mixture of small molecule peptides with superior sun protection and enhancement effects. In addition, controlling the microwave treatment power to 200-500W, or setting the complex as a combination of papain, trypsin, and neutral protease, can further enhance the sun protection and enhancement effects of hydrolyzed royal jelly protein.

[0052] Furthermore, the composition of the water-in-oil sunscreen system involved in this invention can be added to water-in-oil sunscreens, requiring only a small amount of sunscreen agent to give the sunscreen product excellent sun protection performance; at the same time, the addition of a stabilizer composed of octyl polymethylsiloxane and isononyl isononanoate to the water-in-oil sunscreen can further improve the powder stability and heat and cold resistance of the sunscreen product. Detailed Implementation

[0053] To further illustrate the technical means and effects of the present invention, the following describes the technical solution of the present invention in conjunction with preferred embodiments of the present invention. However, the present invention is not limited to the scope of the embodiments.

[0054] The sources of each component / raw material in the following embodiments are shown in Table 1.

[0055] Table 1

[0056]

[0057] Preparation Example 1

[0058] This preparation example provides a hydrolyzed royal jelly protein, prepared using the following method:

[0059] (1) Mix royal jelly and water at a ratio of 1:10 g / mL and microwave treat it (the temperature of microwave treatment is 70℃, the power is 300 W, and the time is 20 min). Filter the product of microwave treatment and collect the filtrate to obtain the pretreated solution.

[0060] (2) Add 3% of the mass of the pretreatment solution of the compound enzyme (the compound enzyme is papain, trypsin and neutral protease in a mass ratio of 2:0.8:0.3) to the pretreatment solution and carry out the enzymatic hydrolysis reaction (the temperature of the enzymatic hydrolysis reaction is 40℃ and the time is 1 h) to obtain the enzymatic hydrolysate. Filter the enzymatic hydrolysate and collect the filtrate. Concentrate the filtrate to 20% (v / v) and freeze-dry the concentrate to obtain hydrolyzed royal jelly protein.

[0061] Preparation Example 2

[0062] This preparation example provides a hydrolyzed royal jelly protein, prepared using the following method:

[0063] (1) Mix royal jelly and water at a ratio of 1:5 g / mL and microwave treat (microwave treatment temperature is 50℃, power is 200 W, time is 30 min). Filter the product of microwave treatment and collect the filtrate to obtain the pretreated solution.

[0064] (2) Add 5% of the mass of the pretreatment solution of the compound enzyme (the compound enzyme is papain, trypsin and neutral protease in a mass ratio of 1:1:0.1) to the pretreatment solution and carry out the enzymatic hydrolysis reaction (the temperature of the enzymatic hydrolysis reaction is 30℃ and the time is 2 h) to obtain the enzymatic hydrolysate. Filter the enzymatic hydrolysate and collect the filtrate. Concentrate the filtrate to 20% (v / v) and freeze-dry the concentrate to obtain hydrolyzed royal jelly protein.

[0065] Preparation Example 3

[0066] This preparation example provides a hydrolyzed royal jelly protein, prepared using the following method:

[0067] (1) Mix royal jelly and water at a ratio of 1:20 g / mL and microwave treat it (the temperature of microwave treatment is 80℃, the power is 500 W, and the time is 10 min). Filter the product of microwave treatment and collect the filtrate to obtain the pretreated solution.

[0068] (2) Add 1% of the mass of the pretreatment solution of the compound enzyme (the compound enzyme is papain, trypsin and neutral protease in a mass ratio of 3:0.5:0.5) to the pretreatment solution and carry out the enzymatic hydrolysis reaction (the temperature of the enzymatic hydrolysis reaction is 50℃ and the time is 0.5h) to obtain the enzymatic hydrolysate. Filter the enzymatic hydrolysate and take the filtrate. Concentrate the filtrate to 20% (v / v) and freeze-dry the concentrate to obtain hydrolyzed royal jelly protein.

[0069] Preparation Example 4

[0070] This preparation example provides a hydrolyzed royal jelly protein, which differs from Preparation Example 1 only in that the power of the microwave treatment in step (1) is adjusted to 600 W, while the rest of the steps are the same as those in Preparation Example 1.

[0071] Preparation Example 5

[0072] This preparation example provides a hydrolyzed royal jelly protein, which differs from Preparation Example 1 only in that the power of the microwave treatment in step (1) is adjusted to 150 W, while the other steps are the same as those in Preparation Example 1.

[0073] Preparation Example 6

[0074] This preparation example provides a hydrolyzed royal jelly protein, which differs from preparation example 1 only in that the total mass of the complex enzyme is kept constant in step (2), and the complex enzyme is adjusted to papain and trypsin with a mass ratio of 2:0.8. The remaining steps are consistent with preparation example 1.

[0075] Preparation Example 7

[0076] This preparation example provides a hydrolyzed royal jelly protein, which differs from preparation example 1 only in that the total mass of the complex enzyme remains unchanged in step (2), and the complex enzyme is adjusted to a mass ratio of papain and neutral protease of 2:0.3. The remaining steps are consistent with preparation example 1.

[0077] Preparation Example 8

[0078] This preparation example provides a hydrolyzed royal jelly protein, which differs from preparation example 1 only in that the total mass of the complex enzyme is kept constant in step (2), and the complex enzyme is adjusted to trypsin and neutral protease with a mass ratio of 0.8:0.3. The remaining steps are consistent with preparation example 1.

[0079] Example 1

[0080] This embodiment provides a composition comprising, in parts by weight:

[0081] 0.5 parts of polysorbate-60, 0.1 parts of PEG-11 methyl ether polydimethylsiloxane, 0.2 parts of dextrin palmitate, 0.1 parts of hydrolyzed royal jelly protein obtained in Preparation Example 1, and 0.2 parts of glyceryl behenate.

[0082] Example 2

[0083] This embodiment provides a composition comprising, in parts by weight:

[0084] 0.3 parts of polysorbate-60, 0.3 parts of PEG-11 methyl ether polydimethylsiloxane, 0.1 parts of dextrin palmitate, 0.2 parts of hydrolyzed royal jelly protein obtained in Preparation Example 2, and 0.1 parts of glyceryl behenate.

[0085] Example 3

[0086] This embodiment provides a composition comprising, in parts by weight:

[0087] 0.8 parts of polysorbate-60, 0.05 parts of PEG-11 methyl ether polydimethylsiloxane, 0.3 parts of dextrin palmitate, 0.05 parts of hydrolyzed royal jelly protein obtained in Preparation Example 3, and 0.3 parts of glyceryl behenate.

[0088] Examples 4-8

[0089] Examples 4-8 each provide a composition, which differs from Example 1 only in that the hydrolyzed royal jelly protein obtained in Preparation Example 1 is replaced with the hydrolyzed royal jelly protein obtained in Preparation Examples 4-8 respectively, while the composition and amount of other raw materials are the same as in Example 1.

[0090] Example 9

[0091] This embodiment provides a composition that differs from Example 1 only in that it does not contain glycerol behenate. The reduced mass fraction is made up by PEG-11 methyl ether polydimethylsiloxane, while the composition and amount of other raw materials remain the same as in Example 1.

[0092] Comparative Example 1

[0093] This comparative example provides a composition that differs from Example 1 only in that it does not include polysorbate-60. The reduced mass fraction is made up by PEG-11 methyl ether polydimethylsiloxane, while the composition and amount of other raw materials remain the same as in Example 1.

[0094] Comparative Example 2

[0095] This comparative example provides a composition that differs from Example 1 only in that it does not contain PEG-11 methyl ether polydimethylsiloxane, and the reduced mass fraction is made up by polysorbate-60. The composition and amount of other raw materials are the same as in Example 1.

[0096] Comparative Example 3

[0097] This comparative example provides a composition that differs from Example 1 only in that it does not contain dextrin palmitate, and the reduced mass fraction is made up by hydrolyzed royal jelly protein. The composition and amount of other raw materials are the same as in Example 1.

[0098] Comparative Example 4

[0099] This comparative example provides a composition that differs from Example 1 only in that it does not contain hydrolyzed royal jelly protein, and the reduced mass fraction is made up by dextrin palmitate. The composition and amount of other raw materials are the same as in Example 1.

[0100] Comparative Example 5

[0101] This comparative example provides a composition that differs from Example 1 only in that it does not contain PEG-11 methyl ether polydimethylsiloxane, and the reduced mass fraction is made up by glyceryl behenate. The composition and amount of other raw materials are the same as in Example 1.

[0102] Application Example 1

[0103] This application example provides a water-in-oil type sunscreen, comprising the components shown in Table 2.

[0104] Table 2

[0105]

[0106] The preparation method is as follows:

[0107] (1) Dissolve and mix all components in phase A at 80℃ to achieve homogeneous dispersion; dissolve and mix all components in phase B at 80℃ to achieve homogeneous dispersion; dissolve and mix all components in phase C at 60℃ to achieve homogeneous dispersion, and then cool to 25℃ for later use.

[0108] (3) Add phase A to phase B under stirring, then homogenize at 2500 rpm for 5 min, stir and cool down to 40℃, add phase C to the mixture of phase A and phase B, stir evenly and cool down to 25℃.

[0109] Application Example 2

[0110] This application example provides a water-in-oil type sunscreen, comprising the components shown in Table 3.

[0111] Table 3

[0112]

[0113] The preparation method is as follows:

[0114] (1) Dissolve and mix all components in phase A at 85℃ to achieve homogeneous dispersion; dissolve and mix all components in phase B at 85℃ to achieve homogeneous dispersion; dissolve and mix all components in phase C at 65℃ to achieve homogeneous dispersion, and then cool to 25℃ for later use.

[0115] (3) Add phase A to phase B under stirring, then homogenize at 2000 rpm for 10 min, stir and cool down to 35℃, add phase C to the mixture of phase A and phase B, stir evenly and cool down to 25℃.

[0116] Application Example 3

[0117] This application example provides a water-in-oil type sunscreen, comprising the components shown in Table 4.

[0118] Table 4

[0119]

[0120] The preparation method is as follows:

[0121] (1) Dissolve and mix all components in phase A at 75℃ to achieve homogeneous dispersion; dissolve and mix all components in phase B at 75℃; dissolve and mix all components in phase C at 55℃ and then cool to 25℃ for later use.

[0122] (3) Add phase A to phase B under stirring, then homogenize at 3000 rpm for 5 min, stir and cool down to 35℃, add phase C to the mixture of phase A and phase B, stir evenly and cool down to 25℃.

[0123] Application Examples 4-9

[0124] Application Examples 4-9 each provide a water-in-oil type sunscreen. The only difference between them and Application Example 1 is that the composition of Example 1 in Phase A is replaced by an equal mass of the compositions of Examples 4-9, respectively. The rest of the formulation and preparation method are the same as those of Application Example 1.

[0125] Application Example 10

[0126] This application example provides a water-in-oil type sunscreen, which differs from Application Example 1 only in that the total mass of the stabilizer remains unchanged, and the stabilizer is adjusted to 8 parts of octyl polymethylsiloxane. The rest of the formulation and preparation method are consistent with Application Example 1.

[0127] Application Example 11

[0128] This application example provides a water-in-oil type sunscreen, which differs from Application Example 1 only in that the total mass of the stabilizer remains unchanged, and the stabilizer is adjusted to 8 parts of isononyl isononanoate. The rest of the formulation and preparation method are consistent with Application Example 1.

[0129] Comparative Application Examples 1-5

[0130] Comparative Application Examples 1-5 each provide a water-in-oil type sunscreen. The only difference between them and Application Example 1 is that the composition of Example 1 in Phase A is replaced by an equal mass of the compositions of Comparative Examples 1-5, respectively. The rest of the formulation and preparation method are the same as those of Application Example 1.

[0131] Comparative Application Example 6

[0132] This application example provides a water-in-oil type sunscreen, which differs from Application Example 1 only in that no stabilizer is added to the formula, and the reduced mass parts are made up by water to 100 parts. The rest of the formula and preparation method are consistent with Application Example 1.

[0133] Comparative Application Example 7

[0134] This application example provides a water-in-oil type sunscreen, which differs from Application Example 1 only in that the composition of Example 1 is not added to the formula, and the reduced mass parts are made up by water to 100 parts. The rest of the formula and preparation method are the same as Application Example 1.

[0135] Test Example 1

[0136] This test case evaluates the sun protection factor (SPF) of the water-in-oil sunscreens in the above application examples and comparative application examples.

[0137] (1) Test method:

[0138] Sixty healthy volunteers aged 18-60 years were selected and randomly divided into 6 groups of 10 each. Each volunteer was tested with 3 test samples (the test samples were the water-in-oil sunscreens used in the application examples and control examples mentioned above). Each group of volunteers was tested with the same 3 test samples. An irradiation area was selected on the back of the subject, and the lowest irradiation dose that caused erythema was defined as the minimum erythema dose (MED) for normal skin of that subject. The test product was also applied to the subject's skin at a dose of 2.00 ± 0.05 mg / cm². 2 Weigh out the sample and apply it evenly to the test area. After waiting 15-30 minutes, the lowest radiation dose at which erythema appears on the skin is taken as the MED of the subject's skin under the product's protection. The SPF value of the sample for a single subject is calculated using the following formula:

[0139] Individual SPF = MED of protected skin / MED of unprotected skin

[0140] (2) Test results:

[0141] Table 5 shows the SPF values ​​of the water-in-oil sunscreens in various application examples and comparative application examples. It is evident that the composition of the present invention, suitable for water-in-oil sunscreen systems, can significantly improve the SPF value of sunscreens.

[0142] Data from Application Example 1 and Comparative Application Examples 3-4 show that dextrin palmitate and hydrolyzed royal jelly protein have a significant synergistic effect in enhancing sun protection efficacy.

[0143] A comparison of the data from Application Example 1 and Application Examples 4-8 shows that controlling the microwave treatment power to 200-500 W during the preparation of hydrolyzed royal jelly protein can further enhance the sun protection effect of royal jelly protein. In addition, using papain, trypsin, and neutral protease as a complex enzyme to enzymatically hydrolyze the pretreated solution after microwave treatment during the preparation of hydrolyzed royal jelly protein can further increase the content of active ingredients in the product, thereby enabling hydrolyzed royal jelly protein to better exert its synergistic effect with dextrin palmitate.

[0144] Test Example 2

[0145] This test case examines the water washability of the above application examples and comparative application examples of water-in-oil sunscreens.

[0146] (1) Test method:

[0147] Ninety healthy volunteers aged 18-60 years were selected and divided into 18 groups of 5 people each. Each group used the water-in-oil type sunscreens mentioned in the above application examples and control examples, and the water wash-off performance was tested according to the test methods in the group standard "Test and Evaluation Method for Water Wash-off Performance of Sunscreen Cosmetics".

[0148] (1.1) T0 phase: Subjects cleaned their faces with cleansing products and sat quietly for 30 minutes in an independent environment with a temperature of 21±1℃ and a relative humidity of 50±10%. The baseline values ​​of the test sites of the subjects were measured using a skin colorimeter and a facial image analyzer. Under the guidance of the volunteers, each group of volunteers used the sunscreen products of the application case and the control application case respectively.

[0149] (1.2) T1 stage: 30 minutes after the sunscreen product was used, the test sites of the subjects were measured using a skin colorimeter and a facial image analyzer; each group of volunteers cleaned their face under guidance (half of the face was washed with water and a cleansing towel, and the other half of the face was cleaned with makeup remover and then washed with water and a cleansing towel).

[0150] (1.3) T2 phase: 30 minutes after cleansing the face, the test sites of the subjects were measured using a skin colorimeter and a facial image analyzer.

[0151] (2) Test results:

[0152] The cleanliness rate was calculated according to the method in "Evaluation Method for Washable Sunscreen Cosmetics". The test results of the cleanliness rate of each sunscreen product are shown in Table 5. If the cleanliness rate is >75%, it is considered washable with water, and if it is ≥90%, it is considered easy to wash with water.

[0153] As can be seen from the data in Table 5, the composition of the present invention applicable to the water-in-oil sunscreen system can significantly improve the water washability of sunscreen.

[0154] Furthermore, a comparison of the data from Application Example 1 and Comparative Application Examples 1-2 shows that polysorbate and polyethylene glycol methyl ether polydimethylsiloxane have a significant synergistic effect in terms of water washability.

[0155] Test Example 3

[0156] This test case examines the lightness of the water-in-oil sunscreens in the above application examples and comparative application examples.

[0157] (1) Test method: 90 subjects, the same as in test example 2, were selected and divided into 18 groups of 5 people each. In an independent environment with the same temperature of 21±1℃ and relative humidity of 50±10%, they sat quietly for 30 minutes and then used the water-in-oil sunscreens of the above application examples and the control application examples. The subjects rated the refreshing feeling of the sunscreens. The score was an integer from 1 to 10. After the scoring was completed, the average value of each sample was taken. The higher the score, the stronger the refreshing feeling.

[0158] (2) Test results:

[0159] The test results are shown in Table 5. The results show that the water-washable composition applicable to water-in-oil sunscreen systems involved in this invention can significantly improve the refreshing feel of sunscreen.

[0160] Meanwhile, a comparison of the data from Application Example 1, Application Example 9, and Comparative Application Example 5 shows that glyceryl behenate and polyethylene glycol methyl ether polydimethylsiloxane have a significant synergistic effect in improving the refreshing feel of sunscreen products.

[0161] Table 5

[0162]

[0163] Test Example 4

[0164] This test case examines the safety of the water-in-oil sunscreens in the above application examples and comparative application examples.

[0165] (1) Test method:

[0166] Sixty subjects, the same as in Test Example 1, were selected and divided into six groups of ten each. Each subject was tested with three samples (the samples were the water-in-oil sunscreens from the above application examples and control examples). Each group of volunteers tested the same three samples.

[0167] After the subject cleaned their back, a spot tester containing an equal mass of sunscreen sample was applied to a selected location on the back using non-irritating adhesive tape. After application, the tape was gently pressed onto the skin with fingers to ensure even distribution, and left on for 48 hours. During this 48-hour period, the subject was instructed to keep the patch area dry and avoid strenuous exercise, scratching, and prolonged sun exposure. After 48 hours, the tester was removed and marked. After 30 minutes, once the pressure marks had disappeared, the results were assessed under adequate lighting.

[0168] The grading criteria for adverse skin reactions are shown in Table 6.

[0169] Table 6

[0170]

[0171] (2) Test results:

[0172] The safety test results of the water-in-oil type sunscreens in various application examples and comparative application examples are shown in Table 7. The results show that the sunscreens involved in this invention are safe and non-irritating.

[0173] Table 7

[0174]

[0175] Test Example 5

[0176] This test case examines the stability of the water-in-oil sunscreens in the above application examples and comparative application examples.

[0177] (1) Test method:

[0178] (1.1) Appearance stability: The water-in-oil sunscreens of each application example and the comparative application example were placed under a standard light source at room temperature, and the appearance of the material was observed.

[0179] (1.2) Heat resistance: The water-in-oil sunscreens of each application example and the comparative application example were placed in an electric thermostatic incubator at 45℃ for 30 days. After returning to room temperature, the appearance of the material was observed.

[0180] (1.3) Cold resistance: The water-in-oil sunscreens of each application example and the comparative application example were placed in a -10℃ refrigerator for 30 days, and the appearance of the material was observed after the temperature returned to room temperature.

[0181] (1.4) Cyclic thermal stability: Within 72 h, the water-in-oil sunscreens of each application example and the control application example were repeatedly changed between 10℃ and 45℃. This operation was repeated for 3 cycles. After returning to room temperature, the appearance of the material was observed.

[0182] (2) Test results:

[0183] The stability test results of the water-in-oil sunscreens in various application examples and comparative application examples are shown in Table 8. It can be seen that the water-in-oil sunscreens of the present invention have excellent storage stability and are less restricted by the storage environment.

[0184] Furthermore, a comparison of the data from Application Example 1 with Application Examples 10-11 and Comparative Application Example 6 shows that octyl polymethylsiloxane and isononyl isononanoate have a significant synergistic effect in improving the stability of the composition. The addition of stabilizers can improve the stability of sunscreen products, thereby achieving excellent effects such as refreshing washability and enhanced sun protection.

[0185] Table 8

[0186]

[0187] The applicant declares that the technical solution of this invention is illustrated by the above embodiments, but this invention is not limited to the above embodiments, that is, it does not mean that this invention must rely on the above embodiments to be implemented. Those skilled in the art should understand that any improvements to this invention, equivalent substitutions of raw materials for the products of this invention, addition of auxiliary components, selection of specific methods, etc., all fall within the protection scope and disclosure scope of this invention.

[0188] The preferred embodiments of the present invention have been described in detail above. However, the present invention is not limited to the specific details in the above embodiments. Within the scope of the technical concept of the present invention, various simple modifications can be made to the technical solution of the present invention, and these simple modifications all fall within the protection scope of the present invention.

[0189] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any suitable manner without contradiction. In order to avoid unnecessary repetition, the present invention will not describe the various possible combinations separately.

Claims

1. An oil-in-water sunscreen characterized in that, The oil-in-water sunscreen cream comprises, in parts by mass, 0.5-2.5 parts of a composition suitable for an oil-in-water sunscreen system, 5-10 parts of a physical sunscreen agent, 5-10 parts of a stabilizer, 2-4 parts of an emulsifier, 0.3-2 parts of a thickening agent, 0.2-0.8 parts of an antioxidant, 5-10 parts of a humectant, 0.2-0.4 parts of a dispersing agent, and 60-85 parts of water; The stabilizer comprises octylpolymethylsiloxane and isononyl isononanoate; The mass ratio of the octylpolymethylsiloxane and the isononyl isononanoate is 1:1-1:4; The composition suitable for the oil-in-water sunscreen system comprises, in parts by mass, 0.3-0.5 parts of polysorbate, 0.1-0.2 parts of polyethylene glycol methyl ether dimethicone, 0.2-0.4 parts of dextrin palmitate, 0.1-0.3 parts of hydrolyzed royal jelly protein, and 0.2-0.6 parts of glyceryl behenate; The hydrolyzed royal jelly protein is prepared by a preparation method comprising the following steps: (1) mixing royal jelly with water, performing microwave treatment, filtering and collecting the filtrate after the microwave treatment to obtain a pretreatment liquid; (2) mixing the pretreatment liquid with a composite enzyme to perform enzymolysis to obtain an enzymolysis liquid, filtering and collecting the filtrate of the enzymolysis liquid to obtain the hydrolyzed royal jelly protein; The composite enzyme in step (2) comprises papain, trypsin and neutral protease; The ratio of the royal jelly to water in step (1) is 1:5-1:20 g / mL; The temperature of the microwave treatment in step (1) is 50-80℃, the power of the microwave treatment is 200-500 W, and the time of the microwave treatment is 10-30 min.

2. The oil-in-water sunscreen according to claim 1, characterized in that The mass ratio of the pretreatment liquid to the composite enzyme in step (2) is 100:1-100:5, the temperature of the enzymolysis is 30-50℃, and the time of the enzymolysis is 0.5-2 h; The mass ratio of the papain, the trypsin and the neutral protease in step (2) is (1-3):(0.5-1):(0.1-0.5).

3. The oil-in-water sunscreen of claim 1, wherein, The physical sunscreen agent comprises titanium dioxide modified by a surface treatment agent; The surface treatment agent comprises any one or a combination of at least two of silica, aluminum hydroxide or triethoxysilane.

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