Efficient sunscreen composition as well as preparation method and application thereof

Abstract

The invention relates to the technical field of skin care products, and particularly discloses an efficient sunscreen composition as well as a preparation method and application thereof. The efficient sunscreen composition is prepared from the following raw materials in parts by weight: 20 to 25 parts of non-nano zinc oxide, 1 to 5 parts of silica, 0.2 to 0.8 part of tetrahydromethylpyrimidine carboxylic acid, 0.05 to 0.1 part of European cork oak bark extract, 20 to 24 parts of emollient and 0.2 to 0.8 part of water. The sunscreen composition can be used for sunscreen cream and has the advantages of being non-nanoscale, safe, free of irritation, high in sunscreen capacity, high in transparency and free of false white.

Description

Technical Field

[0001] The present application relates to the technical field of skin care products, and more specifically, to a high-efficiency sunscreen composition and a preparation method and application thereof. Background Art

[0002] Sunlight is an indispensable part of life, including X-rays, ultraviolet rays, visible light and infrared rays. Most of them are blocked by the atmosphere. If the ecological environment on which humans depend for survival is further damaged, especially if the ozone content in the ozone layer is further reduced, the intensity of ultraviolet rays entering the earth will increase day by day. A moderate amount of ultraviolet rays is good for human health, but when humans are exposed to ultraviolet rays for a long time and in large doses, it will cause great damage to the skin and even the entire body, and may cause skin problems such as sagging and aging, skin pigmentation, and spots. Severe cases may cause skin inflammation, burns, and even cancer. Therefore, in order to maintain healthy and beautiful skin, people should take good sun protection measures.

[0003] Common sunscreens mainly block or absorb long-wave ultraviolet rays (UVA) and medium-wave ultraviolet rays (UVB) that are more harmful to human skin. In recent years, many sunscreen cosmetics have appeared on the market. These products add physical sunscreens that can block, reflect or scatter ultraviolet rays, or chemical sunscreens that absorb ultraviolet rays, thereby protecting the skin from tanning, damage and aging.

[0004] In the process of sunscreen product development, the application of chemical sunscreens has generally increased, but for people with sensitive skin and children's skin, small molecule chemical sunscreens may cause skin irritation and allergies. Physical sunscreen ingredients have become a hot spot in the development of sunscreen products today due to their low irritation, fewer side effects, and greater safety. They have a broad market space and great research and development value.

[0005] In view of the above-mentioned related technologies, the inventors found that the particle size of nano zinc oxide as a physical sunscreen ingredient is relatively small, and there is a risk of penetrating into the skin, so nano physical sunscreens are not allowed to be added to children's sunscreen products. Non-nano physical sunscreens have a larger particle size, so the sunscreen products made of them are relatively white, which is easy to be fake white after application, and the SPF index is low, resulting in a high addition amount, a relatively thick skin feel, and difficult to spread. Summary of the invention

[0006] In order to provide better SPF value and PA value without false white and high transparency, the present application provides a high-efficiency sunscreen composition and a preparation method and application thereof.

[0007] In the first aspect, the present application provides a high-efficiency sunscreen composition, which adopts the following technical solution: A high-efficiency sunscreen composition comprises the following raw materials in parts by weight: 20-25 parts of non-nano zinc oxide, 1-5 parts of silica, 0.2-0.8 parts of ectoine, 0.05-0.1 parts of European cork oak bark extract, 20-24 parts of emollients, and 0.2-0.8 parts of water.

[0008] By adopting the above technical scheme and using non-nano zinc oxide as the raw material, a natural barrier with a white and refreshing texture is formed on the skin, which can block, reflect or scatter ultraviolet rays and is not easily absorbed by the skin. The ingredients are natural and safe, and the sunscreen is non-irritating. In addition, the use of components such as tetrahydromethylpyrimidine carboxylic acid and European cork oak bark extract can make the sunscreen composition lighter, easier to spread, easier to apply, with better transparency, no false whitening, and higher SPF value and PA value. At the same time, as a derivative of amino acids, tetrahydromethylpyrimidine carboxylic acid has good hydrophilicity, which is equivalent to adding a protective shield to the outer layer of the skin, strengthening and restoring cell function, stabilizing the skin barrier, restoring and regulating water content, and helping to lock in moisture, moisturizing the skin to keep it healthy and hydrated. It can not only effectively block the damage of sunlight and blue light, but also resist pollutants and allergens in the air, stimulate the skin's self-repair ability, and enhance the immune protection function of skin cells. European cork oak bark extract is rich in polyphenols, such as flavonoids and tannins, and has strong antioxidant and anti-free radical capabilities, helping to resist ultraviolet damage to the skin, prevent skin aging and sunburn, and is also anti-inflammatory and antibacterial, providing more comprehensive protection for the skin. It is used in combination with tetrahydromethylpyrimidine carboxylic acid and non-nano zinc oxide to make non-nano physical sunscreen ingredients, providing higher SPF and PA values, and has better transparency, improving the false white defects of pure physical non-nano sunscreen, and avoiding the risk of irritation to children's skin caused by small molecule chemical sunscreens. It not only has good stability, but also has good spreadability.

[0009] Optionally, the mass ratio of the ectoine to the European Quercus variabilis bark extract is 5:1.

[0010] By adopting the above technical scheme, the mass ratio of ectoine and European cork oak bark extract is adjusted to 5:1, and a sunscreen composition with higher transparency, better spreadability, skin adhesion and refreshing properties can be obtained.

[0011] Optionally, the silica is pretreated as follows: Dissolve 10-12 parts by weight of carboxymethyl chitosan to prepare a solution with a concentration of 1.5-2wt%, add 10-12 parts by weight of collagen peptide, 0.2-0.24 parts by weight of TG enzyme and 10-12 parts by weight of silica, adjust the pH value to 7, and stir at 28-30°C for 12-16h.

[0012] When silica is applied to the skin in a sunscreen composition, it may make it difficult to apply the product evenly, resulting in uneven sunscreen protection. By adopting the above technical solution, the silica is pretreated with a carboxymethyl chitosan solution, collagen peptides, and TG enzyme. The hydroxyl, carboxyl, and other polar groups in the carboxymethyl chitosan molecules can form hydrogen bonds with water molecules. The cross-linking effect of TG enzyme and the electrostatic interaction between carboxymethyl chitosan and collagen peptides can effectively improve the gel properties of the collagen peptide aggregates, thereby surface coating the silica and improving the adhesiveness of the gel, so that the silica can adhere to the skin more docilely, fill the skin pores, and make the skin more lubricated. TG enzyme can improve the ability of protein to bind water, or improve the protein gel network structure to improve the water retention of the gel, so that the skin is more hydrated, and the silica is smoother, easier to apply evenly, and has better spreadability. In addition, collagen peptides can remove DPPH free radicals, improve the normal growth of cells, and also have the function of repairing tissues, participate in the migration, differentiation and proliferation of cells, increase skin elasticity, and reduce skin aging caused by ultraviolet radiation.

[0013] Optionally, the collagen peptide is tilapia skin collagen peptide.

[0014] By adopting the above technical scheme, tilapia skin is the by-product of tilapia processing, and the extracted collagen peptide is the main active ingredient. When combined with carboxymethyl chitosan with good moisturizing properties, a complex with moisturizing, anti-aging and sun protection properties can be obtained. Moreover, the tilapia skin collagen peptide has good affinity, compatibility and permeability with the skin, and can be directly absorbed by the skin, making the skin more delicate and radiant, and increasing the glossiness and elasticity.

[0015] Optionally, the preparation method of the tilapia skin collagen peptide is: The skin of tilapia is washed, drained, boiled, and minced to obtain fish skin crumbs, deionized water 3-4 times the amount of the fish skin crumbs is added, the pH is adjusted to neutral, a composite enzyme is added, and enzymolysis is performed at 50-55° C. for 3.5-4 hours, the enzyme is inactivated, the mixture is cooled, filtered, and the filtrate is spray-dried to obtain a polypeptide powder; Add the polypeptide powder to deionized water, adjust the pH value to neutral, add inorganic zinc, heat to 70-80°C, stir for 30-40 minutes, concentrate and dry. The molar ratio of amino acids to zinc ions in the polypeptide powder is 2:1.

[0016] By adopting the above technical scheme, after the tilapia skin is hydrolyzed by the composite enzyme, the obtained polypeptide powder contains a variety of amino acids, which play an antioxidant and anti-aging role. After adding inorganic zinc, the zinc ions can form coordination bonds with the amino acid molecules and at the same time form ionic bonds with their carboxyl groups to finally form a chelate structure, which is easily absorbed by the matrix and has antioxidant properties. Zinc is an important trace element in the growth and repair of skin cells, which can help maintain skin health, accelerate skin self-repair, relieve skin inflammation, promote skin cell proliferation and differentiation, and regulate skin oil secretion. In addition, zinc is a component of many antioxidant enzymes, which can help protect the skin from damage by free radicals and ultraviolet rays and reduce the occurrence of skin aging.

[0017] Optionally, the emollient is selected from at least one of cyclopentasiloxane, cardamine extract, codonopsis oligosaccharide, and triethylhexanoin.

[0018] By adopting the above technical scheme, cyclopentasiloxane has good chemical stability, low surface tension and excellent waterproof performance, can form an oil-free film on the skin surface, can reduce water evaporation, help the skin stay hydrated, moisturize the skin, protect the skin mucosa, relieve skin dryness, fill and smooth the skin, make the skin younger and firmer, improve the skin texture, and make it softer and more delicate; triethylhexanoin can not only meet the light weight requirements, but also have a low molecular weight and branched structure, and a segmented carbon chain, giving it an excellent light skin feel and adjusting the consistency and texture of the product; Codonopsis oligosaccharides have the functions of improving skin oil secretion and maintaining normal skin tissue structure and morphology. The oil secreted by the sebaceous glands and the sweat secreted by the sweat glands form an emulsified film on the skin surface, which has the functions of softening the stratum corneum, preventing water loss, and maintaining normal skin tissue structure and morphology; skin elasticity refers to the skin stretching and recovery period The ability to restore the original form is usually related to the content of collagen and elastin in the skin. Codonopsis oligosaccharides can significantly increase the content of collagen and elastin in the skin, improve skin elasticity and tension, and reduce wrinkles; it can also increase the water content in the dermis of the skin, and then supply the stratum corneum, so Codonopsis oligosaccharides have the effect of moisturizing and nourishing the skin; Cardamine extract contains active ingredients such as polysaccharides, and cyclopentasiloxane can prevent the evaporation of water too quickly. Together with Codonopsis oligosaccharides, the three can work together to lock in moisture, moisturize, and balance water and oil, which can improve the content of elastin and collagen, and Cardamine has a strong antioxidant effect, which can slow down the oxidative damage of free radicals to fibroblasts and macromolecules such as collagen to a certain extent. The combined effects of moisturizing and water-oil balance will also increase the elasticity of the skin, thereby improving the skin condition and achieving certain anti-aging and anti-wrinkle effects.

[0019] Optionally, the emollient comprises cyclopentasiloxane, cardamine extract, codonopsis oligosaccharide and triethylhexanoin in a mass ratio of 1:0.3-0.7:0.2-0.4:0.1-0.3.

[0020] By adopting the above technical scheme and using each component in a specific proportion as an emollient, the anti-wrinkle, moisturizing and antioxidant effects of the sunscreen composition can be effectively improved, and the skin moisturizing, skin adhesion and spreadability of the sunscreen can be further increased, making the composition easier to apply.

[0021] Optionally, the preparation method of the Cardamine extract is as follows: wash Cardamine violet leaves and Auricularia auricula respectively, dry to constant weight, pass through a 100-mesh sieve, mix, and obtain a mixed powder, wherein the mass ratio of Cardamine violet leaves to Auricularia auricula in the mixed powder is 1:0.4-0.6; Weigh the mixed powder, add 66% ethanol by volume, with a liquid-to-solid ratio of 27-30:1, extract for 3.7-4 hours at a temperature of 75-80°C, filter and centrifuge.

[0022] By adopting the above technical scheme, Cardamine violeta has the characteristic of being rich in selenium, has a stronger ability to scavenge DPPH free radicals, has better antioxidant capacity, can inhibit the activity of tyrosinase, and prevent suntan. The ground fungus contains multiple active ingredients such as trehalose, rhamnose, pectin polysaccharides, glucoside, carotene, phycocyanin and extracellular polysaccharides, and thus has good antioxidant, moisturizing and sunscreen effects. The ground fungus can eliminate free radicals or substances that easily generate free radicals, reduce the damaging effects of free radicals on the skin, and alleviate skin aging. The ground fungus has a good moisturizing effect, and has better skin care and moisturizing effects. It also has a good absorption effect on ultraviolet rays, has sunscreen effects, can inhibit the activity of tyrosinase, reduce the synthesis of melanin, and prevent suntan. Moreover, Cardamine violeta and the ground fungus are natural plants, and the components obtained by extraction are natural active components of plants, which are safe, non-toxic and have no side effects on the human body. Therefore, the cardamine extract can better produce antioxidant, sunscreen, whitening, anti-wrinkle and moisturizing effects.

[0023] In a second aspect, the present application provides a method for preparing a high-efficiency sunscreen composition, using the following technical solution: A method for preparing a high-efficiency sunscreen composition comprises the following steps: Mix water and ectoine, heat to 70-75°C, stir evenly to form a transparent solution; Non-nano zinc oxide, silica, emollient and European cork oak bark extract are mixed and ground homogenously, and the transparent solution is added thereto, and homogenized at 65-75° C. for 3-5 minutes to prepare a composition.

[0024] By adopting the above technical solution, the composition can be prepared after the components are mixed and homogenized. The preparation method is simple and easy to industrialize.

[0025] In a third aspect, the present application provides an application of a high-efficiency sunscreen composition in a sunscreen, wherein the addition amount of the high-efficiency sunscreen composition in the sunscreen is 24-27%.

[0026] By adopting the above technical scheme, adding the sunscreen composition to the sunscreen, and controlling the amount of non-nano zinc oxide added in the sunscreen, the sunscreen can have higher sunscreen efficiency, good sunscreen effect and high SPF value.

[0027] In summary, this application has the following beneficial effects: 1. Since the present application adopts non-nano zinc oxide as the main physical sunscreen ingredient, and adds a specific amount of tetrahydromethylpyrimidine carboxylic acid and European cork oak bark extract as auxiliary ingredients, and also uses emollients, etc., it can achieve a good sunscreen effect, and it does not look fake white after application and has high transparency.

[0028] 2. In the present application, carboxymethyl chitosan, collagen peptide and other ingredients are preferably used to pre-treat silica, so that silica can be more easily dispersed in the sunscreen composition, and the application is more uniform. After use, the skin is more delicate and lustrous, and it can also improve the elasticity of the skin and increase the skin's antioxidant capacity.

[0029] 3. In the present application, cyclopentasiloxane, cardamine extract, codonopsis oligosaccharide and triethylhexanoin are preferably used as emollients, which can effectively improve the spreadability of the sunscreen composition, make it easier to spread on the skin, have stronger moisturizing ability, and can also delay skin aging and prevent tanning. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] Figure 1 These are the test results of the chicken embryo chorioallantoic membrane before and after adding normal saline.

[0031] Figure 2 These are the test results of the chicken embryo chorioallantoic membrane before and after adding SDS solution.

[0032] Figure 3 These are the test results of the chick chorioallantoic membrane before and after adding the sunscreen sample in Application Example 1.

[0033] Figure 4 To compare the test results of the chicken embryo chorioallantoic membrane before and after adding sunscreen to test sample 1.

[0034] Figure 5 To compare the test results of the chicken embryo chorioallantoic membrane before and after adding sunscreen to test sample 2.

[0035] Figure 6To compare the test results of the chicken embryo chorioallantoic membrane before and after adding sunscreen to test sample 3.

[0036] Figure 7 Graph showing particle size distribution of non-nano zinc oxide in the examples. DETAILED DESCRIPTION

[0037] The following examples further illustrate the present application in detail. Example

[0038] The raw materials used in the following examples can all be purchased through market sales channels.

[0039] Example 1: A highly effective sunscreen composition, the raw material dosage is shown in Table 1, the non-nano zinc oxide in Table 1 is selected from EverCare, and its particle size distribution is as follows Figure 1 As shown, the particle size of silica is 5 μm, the emollient is cyclopentasiloxane, and the mass ratio of tetrahydromethylpyrimidine carboxylic acid to European cork oak bark extract is 5:1; the preparation method of the above-mentioned high-efficiency sunscreen composition comprises the following steps: S1. Mix water and ectoine, heat to 70°C, and stir evenly to form a transparent solution; S2. Mix non-nano zinc oxide, silica, cyclopentasiloxane and cork oak bark extract, homogenize and grind for 3 minutes, add the transparent solution, and homogenize at 65° C. and 6000 r / min for 5 minutes to obtain a composition.

[0040] Table 1 Amount of raw materials used in the high-efficiency sunscreen composition in Examples 1-5 Example 2: A highly effective sunscreen composition, which differs from Example 1 in that the amounts of raw materials are as shown in Table 1, and the mass ratio of ectoine to the European cork oak bark extract is 2:1.

[0041] Example 3: A highly effective sunscreen composition, which differs from Example 1 in that the amounts of raw materials are as shown in Table 1, and the mass ratio of ectoine to the European cork oak bark extract is 8:1.

[0042] Example 4: A highly effective sunscreen composition, the raw material dosage is as shown in Table 1, the non-nano zinc oxide in Table 1 is selected from EverCare, and its particle size distribution is as follows Figure 1 As shown, the particle size of silica is 5 μm, the emollient is cyclopentasiloxane, and the mass ratio of tetrahydromethylpyrimidine carboxylic acid and European cork oak bark extract is 16:1; The preparation method of the above-mentioned high-efficiency sunscreen composition comprises the following steps: S1. Mix water and ectoine, heat to 75°C, and stir evenly to form a transparent solution; S2. Non-nano zinc oxide, silica, cyclopentasiloxane and cork oak bark extract were mixed, homogenized and ground for 4 minutes, the transparent solution was added, and homogenized at 75° C. and a rotation speed of 6000 r / min for 3 minutes to obtain a composition.

[0043] Example 5: A highly effective sunscreen composition, which differs from Example 1 in that the amounts of raw materials are as shown in Table 1, and the mass ratio of ectoine to the European cork oak bark extract is 4:1.

[0044] Example 6: A highly effective sunscreen composition, which differs from Example 1 in that the silica is pretreated as follows: 12 g of carboxymethyl chitosan is dissolved to obtain a solution with a concentration of 2 wt%, 12 g of collagen peptide, 0.24 g of TG enzyme and 12 g of silica are added, the pH value is adjusted to 7, and the mixture is stirred at 30°C for 12 h. The collagen peptide is a bovine skin collagen peptide selected from Jiangxi Baiying Biotechnology, item number is 2432, and TG enzyme is selected from Xinjurong Jiangsu Chengqian, item number is 067.

[0045] Embodiment 7: A high-efficiency sunscreen composition, which is different from Embodiment 1 in that the silica is pretreated as follows: 10 g of carboxymethyl chitosan is dissolved to obtain a solution with a concentration of 1.5 wt%, 10 g of collagen peptide, 0.2 g of TG enzyme and 12 g of silica are added, the pH value is adjusted to 7, and the mixture is stirred at 28°C for 16 h. The TG enzyme is selected from Xinjurong Jiangsu Chengqian, with a product number of 067. The collagen peptide is tilapia skin collagen peptide. The preparation method of tilapia skin collagen peptide is as follows: the fish skin of tilapia is washed, drained, boiled, minced, and fish skin pieces are obtained. Deionized water 3 times the amount of the fish skin pieces is added, the pH is adjusted to neutral, a composite enzyme is added, and enzymolysis is performed at 55°C for 3.5 h, the temperature is raised to 100°C, and the enzyme is inactivated in a water bath for 20 min. in, cooled to room temperature, centrifuged with 400-mesh gauze at a speed of 10,000 r / min for 15 min, ultrafiltered with an ultrafiltration membrane with a molecular weight cutoff of 1,000 Da, and spray-dried the filtrate to obtain a product. The added amount of the composite enzyme is 3,000 U / g, and the composite enzyme includes neutral protease and papain in a mass ratio of 1:1. The neutral protease is selected from Wuhan Zhonghong Biological and has an enzyme activity of 200,000. The papain is selected from Globo Biological Products and has an enzyme activity of 1,000,000.

[0046] Example 8: A highly effective sunscreen composition, which differs from Example 1 in that the silica is pretreated as follows: 12 g of carboxymethyl chitosan is dissolved to obtain a solution with a concentration of 2 wt%, 12 g of collagen peptide, 0.24 g of TG enzyme and 12g silica, adjust the pH value to 7, stir at 30°C for 12h, the collagen peptide is tilapia skin collagen peptide, and the preparation method of tilapia skin collagen peptide is as follows: the fish skin of tilapia is washed, drained and boiled, minced to obtain fish skin pieces, deionized water 4 times the amount of fish skin pieces is added, the pH is adjusted to neutral, and a composite enzyme is added, enzymolysis is carried out at 50°C for 4h, the temperature is raised to 100°C, enzyme is inactivated in a water bath for 20min, cooled to room temperature, centrifuged with 400 mesh gauze at a speed of 10000r / min for 15min, ultrafiltered with an ultrafiltration membrane with a molecular weight cutoff of 1000Da, and the filtrate is spray-dried to obtain a product, the amount of composite enzyme added is 3000U / g, the composite enzyme includes neutral protease and papain with a mass ratio of 1:1, the neutral protease is selected from Wuhan Zhonghong Biology, and the enzyme activity is 200,000, and the papain is selected from Globo Biological Products, and the enzyme activity is 1 million.

[0047] Example 9: A highly effective sunscreen composition, which differs from Example 8 in that the preparation method of tilapia skin collagen peptide is as follows: (1) washing and draining the skin of tilapia, boiling and mincing to obtain fish skin pieces, adding deionized water 4 times the amount of the fish skin pieces, adjusting the pH to neutral, adding a composite enzyme, performing enzymolysis at 50° C. for 4 h, heating to 100° C., inactivating the enzyme in a water bath for 20 min, cooling to room temperature, centrifuging with 400 mesh gauze at a speed of 10,000 r / min for 15 min, ultrafiltration with an ultrafiltration membrane with a molecular weight cutoff of 1,000 Da, spray drying the filtrate to obtain a polypeptide powder, wherein the amount of the composite enzyme added is 3,000 U / g, the composite enzyme comprises a neutral protease and papain in a mass ratio of 1:1, the neutral protease is selected from Wuhan Zhonghong Biological, and the enzyme activity is 200,000, and the papain is selected from Globo Biological Products, and the enzyme activity is 1,000,000; (2) Add the polypeptide powder to deionized water, adjust the pH value to neutral, add inorganic zinc (zinc sulfate), raise the temperature to 70°C, stir for 30 minutes, concentrate and dry, and the molar ratio of amino acids to zinc ions in the polypeptide powder is 2:1.

[0048] Example 10: A highly effective sunscreen composition, which is different from Example 9 in that the emollient comprises cyclopentasiloxane, cardamine extract, codonopsis oligosaccharide and triethylhexanoin in a mass ratio of 1:0.7:0.4:0.3, and the preparation method of codonopsis oligosaccharide is as follows: add 10 times 95% ethanol to codonopsis powder and reflux extract twice (1h / time) to defat, dry the residue, and extract it 3 times (1h / time) with 12, 10, and 10 times of water, combine the filtrate, concentrate it to 1g / ml, and slowly add 95% Ethanol is added to a final ethanol concentration of 80%, sealed for 24 hours, centrifuged, the supernatant is concentrated under reduced pressure, and freeze-dried to obtain Codonopsis pilosula oligosaccharides; the Cardamine extract is prepared by the following method: Cardamine violet leaves and Auricularia auricula are washed separately, dried to constant weight, passed through a 100-mesh sieve, mixed, and a mixed powder is obtained, wherein the mass ratio of Cardamine violet leaves to Auricularia auricula in the mixed powder is 1:0.6; the mixed powder is weighed, ethanol with a volume fraction of 66% is added, the liquid-to-solid ratio is 30:1, the extraction time is 4 hours at a temperature of 75°C, and the mixture is filtered and centrifuged.

[0049] Example 11: A highly effective sunscreen composition, which differs from Example 9 in that the emollient comprises cyclopentasiloxane, cardamine extract, codonopsis oligosaccharide and triethylhexanoin in a mass ratio of 1:0.3:0.2:0.1, and the preparation method of codonopsis oligosaccharide is as follows: codonopsis powder is refluxed and extracted twice (1h / time) with 10 times 95% ethanol to defat, the residue is dried, and extracted three times (1h / time) with 12, 10, and 10 times of water, the filtrate is combined, concentrated to 1g / ml, and 95% ethanol is slowly added; The extract of Cardamine violeta and Auricularia auricula was prepared by the following method: Cardamine violeta and Auricularia auricula were washed separately, dried to constant weight, passed through a 100-mesh sieve, mixed to obtain a mixed powder, wherein the mass ratio of Cardamine violeta and Auricularia auricula in the mixed powder was 1:0.4; the mixed powder was weighed, 66% ethanol by volume was added, the liquid-to-solid ratio was 27:1, the extraction time was 3.7 hours at a temperature of 80°C, and the mixture was filtered and centrifuged.

[0050] Example 12: A highly effective sunscreen composition, which differs from Example 11 in that the emollient comprises cyclopentasiloxane, codonopsis oligosaccharide and triethylhexanoin in a mass ratio of 1.7:0.4:0.3.

[0051] Example 13: A highly effective sunscreen composition, which differs from Example 11 in that the emollient comprises cyclopentasiloxane, cardamine extract and triethylhexanoin in a mass ratio of 1.4:0.4:0.3.

[0052] Example 14: A highly effective sunscreen composition, which differs from Example 11 in that the emollient comprises cyclopentasiloxane, Cardamine extract and Codonopsis oligosaccharide in a mass ratio of 1.3:0.7:0.4.

[0053] Example 15: A highly effective sunscreen composition, which differs from Example 11 in that no Auricularia auricula is added during the preparation of the Cardamine extract.

[0054] Comparative Example Comparative Example 1: A highly effective sunscreen composition, which differs from Example 1 in that an equal amount of nano zinc oxide is used to replace non-nano zinc oxide.

[0055] Comparative Example 2: A highly effective sunscreen composition, which differs from Example 1 in that an equal amount of ectoine is used to replace the European cork oak bark extract.

[0056] Comparative Example 3: A highly effective sunscreen composition, which differs from Example 1 in that an equal amount of water is used to replace ectoine.

[0057] Comparative Example 4: A sunscreen composition, characterized in that it comprises the following components in parts by weight: 3 parts of polyglutamic acid (molecular weight 1 million), 5 parts of Sophora japonica flower extract, 15 parts of titanium dioxide (50 nm) and 15 parts of zinc oxide (50 nm), 2 parts of 2-o- and ascorbic acid, and 0.15 parts of sodium copper chlorophyll.

[0058] Application Examples Application Examples 1-5: A sunscreen cream is prepared by mixing the raw materials by weight shown in Table 2. The sunscreen compositions in Application Examples 1-5 are prepared correspondingly from Examples 1-5.

[0059] Table 2 Amount of raw materials used in sunscreen in Application Examples 1-5 Application Examples 6-15: A sunscreen cream, which is different from Application Example 1 in that the high-efficiency sunscreen compositions prepared in Examples 6-15 are respectively used.

[0060] Application Example 16: A sunscreen cream, which is different from Application Example 1 in that the sunscreen composition prepared in Comparative Example 1 is used.

[0061] Application Example 17: A sunscreen cream, which is different from Application Example 1 in that the sunscreen composition prepared in Comparative Example 2 is used.

[0062] Application Example 18: A sunscreen cream, which is different from Application Example 1 in that the sunscreen composition prepared in Comparative Example 3 is used.

[0063] Application Example 19: A sunscreen cream, which is different from Application Example 1 in that the sunscreen composition prepared in Comparative Example 4 is used.

[0064] Performance testing 1. Chicken embryo chorioallantoic membrane test: Test sample: sunscreen prepared in Application Example 1 (using the sunscreen composition prepared in Example 1); Comparative test sample 1: sunscreen prepared in Application Example 16 (using the sunscreen composition prepared in Comparative Example 1); Comparative test sample 2: Compared with application example 1, an equal amount of non-nano zinc oxide is used in the sunscreen to replace the sunscreen composition to prepare a sunscreen; Comparative test sample 3: Compared with application example 1, an equal amount of nano zinc oxide is used in the sunscreen to replace the sunscreen composition to prepare a sunscreen.

[0065] Test method: According to SN / T2329-2009 “Chicken Embryo Chorioallantoic Test for Eye Irritation / Corrosion of Cosmetics”, the negative control group is a 0.9% sodium chloride solution, and the positive control group is a 1% SDS solution. The evaluation criteria are shown in Table 3. The test results are shown in Table 4.

[0066] Table 3 End point evaluation method results evaluation ES (end point score) Irritation classification ES=0 No stimulation 0<ES≤4 Mild irritation 4<ES<5.3 Moderate irritation 5.3≤ES Strong irritant / corrosive Table 4 Irritation scores of the test substances Combination Figure 1-6 From the contents of Table 4, it can be seen that the sunscreen prepared by the sunscreen composition prepared in Example 1 has no obvious irritation, and the ES value is only 0.33, which is closest to physiological saline. After nano zinc oxide is used to replace the non-nano zinc oxide in the sunscreen, the ES value increases, and the irritation is higher than that of Application Example 1. In test sample 2, non-nano zinc oxide is used to replace the sunscreen composition, that is, no substances such as ectoine are added. It can be seen that the irritation of the sunscreen is higher than that of Example 1. In comparison test sample 3, the sunscreen prepared by using an equal amount of nano zinc oxide to replace the sunscreen composition has the highest irritation, and the ES reaches 1.67.

[0067] 2. Sunscreen function and skin feel test (1) SPF and PFA test: The sun protection effect is mainly expressed by the SPF (Sun Protection Factor) and PFA (Protection Factor of UVA) values. The SPF value mainly represents the ability of sunscreen products to protect against medium-wave ultraviolet rays UVB, while the PFA value mainly represents the ability of sunscreen products to protect against long-wave ultraviolet rays UVA.

[0068] The SPF value refers to the ratio of the minimum erythema dose (MED) required to produce erythema on skin protected by sunscreen cosmetics to the MED required to produce erythema on unprotected skin. Among them, MED refers to the minimum dose or shortest time of ultraviolet radiation required to cause clearly visible erythema on the skin, and its range reaches most areas of the irradiation point. The higher the SPF value, the greater the protection ability to the skin. The PFA protection values ​​are PA+, PA++, PA+++, and PA++++. When the PFA value is less than 2, the UVA protection effect shall not be marked. When the PFA value is 2-3, it is marked with PA+; when the PFA value is 4-7, it is marked with PA++; when the PFA value is 8-15, it is marked with PA+++; when the PFA value is greater than or equal to 16, it is marked with PA++++. The more "+" signs there are, the better the effect of UVA protection is and the longer the effective protection time is.

[0069] The SPF, PFA and PA tests were conducted using the human body method (China 2015 edition of the "Technical Specifications for Safety of Cosmetics"). Each group of sunscreens was tested 5 times, and the arithmetic mean of the 5 tests was taken. The test results are recorded in Table 4.

[0070] (2) Non-fake whitening effect test: ① Subjects: 15 female volunteers aged 18-35 years old.

[0071] ② Exclusion criteria for subjects: those who have used antihistamines in the past week or immunosuppressants in the past month, those who have applied any anti-inflammatory drugs to the test site in the past two months, patients with insulin-dependent diabetes, patients with asthma or other chronic respiratory diseases being treated, those who have received anti-cancer chemotherapy in the past six months, patients with immunodeficiency or autoimmune diseases, breastfeeding or pregnant women, those whose skin test sites have scars, pigmentation, atrophy, port-wine stains or other blemishes that affect the determination of experimental results, those participating in other clinical trial researchers, and those with a history of severe allergies.

[0072] ③Restrictions: During the test, it is prohibited to perform treatment that may affect the test on the test site; during the test, it is prohibited to use other brands of products and other products that may affect the test; it is prohibited to use products other than test samples.

[0073] ④ Subject withdrawal criteria: During the test, if the subject experiences adverse reactions, is lost to follow-up without reason, violates the research protocol, or other special reasons, after evaluation and confirmation by the project leader, if the subject is no longer suitable to continue the trial, the subject will be asked to withdraw from the test.

[0074] ⑤ Experimental methods: 1) Recruit subjects; 2) Sign the informed consent form; 3) Before enrollment, ask the subjects a series of questions about medical history, health status, etc. according to the inclusion and exclusion criteria, and conduct a compliance assessment of the skin condition of the test site and record it; 4) Qualified subjects should first clean the skin of the test area, sit quietly for 15 minutes in a constant temperature and humidity environment, not drink water or beverages, and stay relaxed. The staff will position the subject's face, and then use VISIA to take pictures of the test area as pre-use data; 5) After the pre-use data measurement is completed, the subjects are explained how to use the sample, and the subjects apply the sample according to the instructions; 6) After the application is completed, the test area is photographed with VISIA as post-use data.

[0075] ⑥Test indicators: Skin brightness L value and skin color ITA value: Use VISIA surface image analyzer to measure the skin's L value and ITA value; Parameter explanation: L value represents the brightness of the skin, the higher the value, the whiter the skin; ITA value represents the color of the skin, the larger the value, the whiter the skin.

[0076] ⑦Data statistical analysis method: Take the data before and after using the sample; Data statistics: 1) Use Graphpad statistical analysis software to perform statistical analysis on the test data, analyze the changes in L value and ITA value before and after using the product, perform t test on the experimental data, and take the significance level α as 0.05; 2) Calculate the rate of change between the initial value and the value after using the product in the sample area and the control area; 3) Change rate = (L value after using the product / ITA value - L value before using the product / ITA value) / L value before using the product / ITA value × 100%, the test result is the average value of 15 subjects, and the test results are recorded in Table 5.

[0077] ⑧Result determination: Compared with the initial value, there is no significant difference in the L value and ITA value of the coated area, indicating that the sunscreen product is not false white. Compared with the initial value, the L value and ITA value of the coated area are significantly increased, indicating that the sunscreen product is false white.

[0078] ⑨ When applying, the subject took 0.2 mL of the sample and applied it on the skin for 10 circles. During the application process, the spreadability was felt. After 2 minutes of use, the greasy feeling was felt and scored. The higher the evaluation score, the better the skin feel. 1 point - very poor, 2 points - poor, 3 points - average, 4 points - good, 5 points - very good. The test results were taken as the average of 15 subjects and the test results were recorded in Table 5.

[0079] Table 5 Performance test of sunscreen It can be seen from the data in Table 5 that non-nano zinc oxide is used in Application Examples 1-5 (Examples 1-5), and it can be seen that the L value and ITA value of the sunscreen before and after use have a small change rate and no significant change, indicating that the sunscreen does not have a false white effect after use, has good spreadability and lightness, is not greasy, and has a good sunscreen effect, which can reach PA+++; while the mass ratios of tetrahydromethylpyrimidine carboxylic acid and European cork oak bark extract in Examples 2 and 3 are 2:1 and 20:1, and the mass ratios of the two in Examples 4 and 5 are 2:1 and 0.2:1. It can be seen that after use, the L value and ITA value of the sunscreen in Example 1 are smaller than those in Examples 2-5, and it has better lightness, transparency, and no false white effect.

[0080] Application Example 6 (Example 6) Compared with Application Example 1, carboxymethyl chitosan, bovine collagen and TG enzyme are also used to pretreat silica. Table 5 shows that the changes in L value and ITA value before and after application are reduced, the application is closer to the skin, and the transparency is better. In Application Examples 7 and 8, tilapia skin is used to prepare collagen polypeptide, which is more transparent, and the changes in L value and ITA value are smaller.

[0081] Application Example 9 (Example 9) uses tilapia skin to prepare polypeptides, and converts inorganic zinc into organic chelated zinc. Compared with Application Example 1, Application Example 6 and Application Example 8, it can be seen that the sunscreen SPF value is increased, the sunscreen ability is increased, and the scores of spreadability and greasiness are increased.

[0082] Compared with Application Example 9, Application Examples 10-11 (Examples 10-11) also use specific proportions of cyclopentasiloxane, cardamine extract, codonopsis extract and triethylhexanoin as emollients. As can be seen in Table 5, the sunscreens prepared in Application Examples 10 and 11 have increased sun protection capabilities, long-lasting sun protection, and are closer to the skin after application without a false white effect.

[0083] Application Example 12 (Example 12) uses cyclopentasiloxane instead of Cardamine extract, Application Example 13 (Example 13) uses cyclopentasiloxane instead of Codonopsis oligosaccharide, and Application Example 14 (Example 14) uses cyclopentasiloxane instead of triethylhexanoin. Compared with Application Example 11, it can be seen that the application effect of the sunscreen prepared in Application Examples 12-14 is slightly reduced.

[0084] Application Example 15 (Example 15) Compared with Application Example 11, Auricularia auricula was not added when preparing the Cardamine extract. Table 5 shows that the sunscreen prepared in Application Example 15 has a slightly decreased sun protection ability.

[0085] In Application Example 16, nano zinc oxide is used instead of non-nano zinc oxide. It can be seen that the L value and ITA value change greatly after application, the fake white is more obvious, and the sun protection ability is not as good as the non-nano zinc oxide in Application Example 1 of this application.

[0086] Application Example 17 and Application Example 18 used the sunscreen compositions prepared in Comparative Example 2 and Comparative Example 3, respectively, and the sunscreens had a serious false white effect after being applied.

[0087] Application Example 19 uses the sunscreen composition prepared in Comparative Example 4. Compared with Application Example 1, its sunscreen ability is poor, the sunscreen is not long-lasting, it is easy to cause false whitening, and the skin feels heavy.

[0088] 3. Detection of the antioxidant and whitening effects of sunscreens: The sunscreens prepared in Application Example 1, Application Examples 6-15, and Application Examples 17-18 were subjected to the following performance tests, and the test results are recorded in Table 6.

[0089] ① Anti-wrinkle effect test: Based on the principle of voluntariness, a total of 110 subjects aged 30-45 years old who met the criteria were recruited. The CBS-805 skin image analysis system was used to test the collagen in the forehead, left cheek, right cheek and chin of the subjects. The average value of the four test sites was taken (repeated measurement 3 times). The test was conducted after mixing and using the product for 8 weeks before use to evaluate the product's improvement effect on the skin. ② Whitening effect detection: Prepare four test solutions A, B, C, and D with phosphate standard buffer solution (PBS, pH = 6.86), tyrosinase solution (200g / mL), L-Dopa solution (prepared with PBS, mass fraction of 0.03%), and sunscreen pretreatment solution (prepared with PBS), place them at a constant temperature of 25°C for 5 minutes, and measure the absorbance value at a wavelength of 475nm. Each group of experiments was repeated 3 times, and the average value was taken to calculate the tyrosinase inhibition rate: Tyrosinase inhibition rate (%) = (A-B)-(C-D)(A-B)×100%, where A: 3mL PBS+0.5mL tyrosinase solution; B: PBS; C: 1mL sample pretreatment solution + 2mL PBS + 0.5mL tyrosinase solution; D: 1mL sample pretreatment solution + 2.5mL PBS.

[0090] ③ Free radical scavenging rate: Take 3mL of 0.2mmol / L DPPH-anhydrous ethanol solution in a cuvette, add 1mL of the test sample, mix well, keep in dark at room temperature for 30min, measure the absorbance at a wavelength of 517nm, and record the absorbance value as A1. The absorbance value of adding 3mL of anhydrous ethanol solution and 1mL of the test sample solution is recorded as A2, and the absorbance value of adding 3mL of DPPH-anhydrous ethanol solution and 1mL of anhydrous ethanol solution is recorded as A3. Calculate the DPPH free radical scavenging rate as follows: DPPH free radical scavenging rate (%) = [1-(A1-A2) / A3] × 100%, and take the average of three measurements.

[0091] Table 6 Efficacy test of sunscreen Compared with Application Example 1, the collagen content in Application Example 6 is increased, the DPPH free radical scavenging rate is improved, and the silica is pretreated to effectively improve the anti-aging, anti-wrinkle, moisturizing and antioxidant effects of the sunscreen.

[0092] In Application Examples 7 and 8, tilapia skin is used to prepare collagen polypeptides. After silica is pretreated, the prepared sunscreen has good in vitro antioxidant activity and produces skin care, moisturizing and anti-skin photoaging effects.

[0093] Application Example 9 (Example 9) uses tilapia skin to prepare polypeptides, and converts inorganic zinc into organic chelated zinc. As can be seen in Table 6, the tyrosinase inhibition rate of the sunscreen increases and the collagen content increases slightly.

[0094] Application Example 10-11 (Example 10-11) Compared with Application Example 9, a specific proportion of cyclopentasiloxane, cardamine extract, codonopsis extract and triethylhexanoin are also used as emollients. As can be seen from Table 6, the collagen content of the subjects increased significantly, the tyrosinase inhibition rate increased, and the DPPH free radical scavenging rate was significantly improved, having strong anti-wrinkle, anti-aging, antioxidant and whitening effects.

[0095] Application Example 12 (Example 12) uses cyclopentasiloxane instead of Cardamine extract, Application Example 13 (Example 13) uses cyclopentasiloxane instead of Codonopsis pilosula oligosaccharides, and Application Example 14 (Example 14) uses cyclopentasiloxane instead of triethylhexanoin. Compared with Application Example 11, the collagen synthesis ability and whitening and antioxidant effects of the sunscreens prepared in Application Examples 12 and 13 are reduced, and the change in Application Example 14 is not obvious.

[0096] Application Example 15 (Example 15) Compared with Application Example 11, Auricularia auricula was not added when preparing the Cardamine extract, and the antioxidant, whitening and anti-aging effects of the sunscreen were slightly reduced, indicating that Auricularia auricula can effectively improve the moisturizing, antioxidant and anti-aging effects of the sunscreen.

[0097] In Application Example 17 and Application Example 18, the sunscreen compositions prepared in Comparative Examples 2 and 3 were used. In Application Example 17, ectoine was used to replace the European cork oak bark extract in the sunscreen composition, and in Application Example 18, water was used to replace ectoine. Compared with Application Example 1, the anti-wrinkle effect and free radical scavenging effect of Application Examples 17 and Application Example 18 were weakened.

[0098] This specific embodiment is merely an explanation of the present application and is not a limitation of the present application. After reading this specification, those skilled in the art may make modifications to the present embodiment without any creative contribution as needed, but such modifications are protected by the patent law as long as they are within the scope of the claims of the present application.

Claims

1. A highly effective sunscreen composition, It is characterized in that The invention comprises the following raw materials in parts by weight: 20-25 parts of non-nano zinc oxide, 1-5 parts of silica, 0.2-0.8 parts of ectoine, 0.05-0.1 parts of European cork oak bark extract, 20-24 parts of emollient and 0.2-0.8 parts of water.

2. The high-efficiency sunscreen composition according to claim 1, Features: The mass ratio of the ectoine to the European cork oak bark extract is 5:

1.

3. The high-efficiency sunscreen composition according to claim 1, Features: The silica is pretreated as follows: Dissolve 10-12 parts by weight of carboxymethyl chitosan to prepare a solution with a concentration of 1.5-2wt%, add 10-12 parts by weight of collagen peptide, 0.2-0.24 parts by weight of TG enzyme and 10-12 parts by weight of silica, adjust the pH value to 7, and stir at 28-30°C for 12-16h.

4. The high-efficiency sunscreen composition according to claim 3, Features: The collagen peptide is tilapia skin collagen peptide.

5. The high-efficiency sunscreen composition according to claim 4, Features: The preparation method of the tilapia skin collagen peptide: The skin of tilapia is washed, drained, boiled, and minced to obtain fish skin crumbs, deionized water 3-4 times the amount of the fish skin crumbs is added, the pH is adjusted to neutral, a composite enzyme is added, and enzymolysis is performed at 50-55° C. for 3.5-4 hours, the enzyme is inactivated, the mixture is cooled, filtered, and the filtrate is spray-dried to obtain a polypeptide powder; Add the polypeptide powder to deionized water, adjust the pH value to neutral, add inorganic zinc, heat to 70-80°C, stir for 30-40 minutes, concentrate and dry. The molar ratio of amino acids to zinc ions in the polypeptide powder is 2:

1.

6. The high-efficiency sunscreen composition according to claim 1, Features: The emollient is selected from at least one of cyclopentasiloxane, cardamine extract, codonopsis oligosaccharide, and triethylhexanoin.

7. The high-efficiency sunscreen composition according to claim 6, Features: The emollient comprises cyclopentasiloxane, cardamine extract, codonopsis oligosaccharide and triethylhexanoin in a mass ratio of 1:0.3-0.7:0.2-0.4:0.1-0.

3.

8. The high-efficiency sunscreen composition according to claim 7, Features: The preparation method of the Cardamine extract is as follows: washing Cardamine violaceae and Auricularia auricula respectively, drying to constant weight, passing through a 100-mesh sieve, mixing to obtain a mixed powder, wherein the mass ratio of Cardamine violaceae to Auricularia auricula in the mixed powder is 1:0.4-0.6; Weigh the mixed powder, add 66% ethanol by volume, with a liquid-to-solid ratio of 27-30:1, extract for 3.7-4 hours at a temperature of 75-80°C, filter and centrifuge.

9. A method for preparing the high-efficiency sunscreen composition according to any one of claims 1 to 8, Features: The following steps are involved: Mix water and ectoine, heat to 70-75°C, stir evenly to form a transparent solution; The non-nano zinc oxide, silica, emollient and European cork oak bark extract are mixed and ground homogenously, and the transparent solution is added thereto, and the mixture is homogenized at 65-75° C. for 3-5 minutes to prepare a composition.

10. Use of the high-efficiency sunscreen composition according to any one of claims 1 to 8 in sunscreen cream, Features: The amount of non-nano zinc oxide in the high-efficiency sunscreen composition added to the sunscreen is 20-25%.

Images