A sunscreen composition containing active components of peony and a preparation method and application thereof

Abstract

The application discloses a sunscreen composition containing peony active ingredients and a preparation method and application thereof, and belongs to the technical field of daily chemical products. The product has a gel network structure based on a specific formula composition, presents an oil-in-water system, and contains hydrophilic sunscreen agents and oleophilic sunscreen agents, which can realize high stability in the structure without using additional solvents or emulsifiers, and the two sunscreen agents can realize the comprehensive performance of efficient synergistic anti-blue light, antioxidation, anti-sunlight dermatitis and post-sun care in cooperation with peony active ingredients and other functional components, without worrying about problems such as skin irritation or acne caused by excessive additives or complex components in existing products. In addition, the product has good skin moisturizing effect, high clarity and spreadability during use, fast film forming speed, small irritation and good use experience.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of daily chemical products, in particular to a sunscreen composition containing peony active ingredients and a preparation method and application thereof. BACKGROUND

[0002] Sunscreen is a relatively important function of existing skin care products, but current sunscreen products have many defects: (1) Some products will introduce a large amount of sunscreen to improve the SPF value (sun protection factor) of the product, which can easily cause skin irritation and allergy problems, and is not friendly to sensitive skin people; (2) Most sunscreen products use water-in-oil system formulations to maintain the stability and effectiveness of the sunscreen, but this also means that the product contains a large amount of solvents and emulsifiers, making the overall product feel heavy, and causing discomfort and greasy feeling after application; (3) Some mild sunscreen products are friendly to sensitive skin people, but these products have single function and cannot meet the comprehensive performance requirements of anti-blue light, anti-oxidation, anti-sunlight dermatitis and post-sun repair; (4) In order to improve the functionality and fashionability of the product, some sunscreen products will introduce some ingredients such as fragrances, alcohol, silicone oil, filler powder, etc. to improve the user experience or improve the moisturizing property of the product, but these additional ingredients can easily cause blockage of human skin pores, and even cause acne and acne after long-term use.

[0003] Therefore, there is currently no sunscreen product that can effectively solve the above-mentioned defects and has comprehensive and efficient performance. SUMMARY

[0004] Based on the defects of the prior art, the purpose of the present application is to provide a sunscreen composition containing peony active ingredients, which has a gel network structure based on a specific formula composition, presents an oil-in-water system, and contains hydrophilic sunscreen and lipophilic sunscreen which can achieve high stability without using additional solvents or emulsifiers in the structure. At the same time, the two sunscreens can synergize with peony active ingredients and other functional components to achieve high-efficiency comprehensive performance of anti-blue light, anti-oxidation, anti-sunlight dermatitis and post-sun repair, without worrying about skin irritation or acne caused by excessive additives or complex ingredients in existing products. In addition, the product has good skin moisturizing effect, high clarity and spreadability during use, fast film-forming speed, low irritation, and good user experience.

[0005] In order to achieve the above-mentioned purposes, the technical scheme adopted by the present application is as follows:

[0006] A sunscreen composition containing peony active ingredients, comprising the following components by weight:

[0007] 0.5-3 parts of alpha crystal phase emulsifier, 0.5-6 parts of co-emulsifier, 1-5 parts of lipophilic sunscreen, 0.5-5 parts of hydrophilic sunscreen, 0.02-2 parts of phosphorylcholine polymer, 0.1-20 parts of peony extract, 5-20 parts of solvent and 25-30 parts of water;

[0008] The co-emulsifier is at least one of cetyl alcohol, stearyl alcohol, arachidyl alcohol and behenyl alcohol;

[0009] The solvent is a mixture of polar solvent and non-polar solvent;

[0010] The peony extract is extracted by NaDES solvent.

[0011] In the sunscreen composition of the present application, based on the interaction of each component, an alpha crystal phase gel structure is formed, which is a "lattice" structure composed of layers of bilayer ester compounds and water, and in the structure, the alpha crystal phase emulsifier molecules are oriented and arranged with polar groups opposite to each other, and the alkyl chains are parallel and closely arranged. The alpha crystal phase gel structure formation mechanism is that during emulsification, the temperature reaches above the Krafft temperature, the lipophilic components such as lipophilic sunscreen change from solid to chaotic liquid, and the hydrophilic components such as hydrophilic sunscreen, molecular peony extract and the like penetrate between the polar groups of the emulsifier, forming a uniform lamellar mesophase structure, when cooled to room temperature, the lipophilic components will recrystallize and arrange into a regular lattice, and the same solubility of the hydrophilic components will still be between the polar groups, forming an alpha crystal phase gel structure. For the lipophilic sunscreen, in the process of participating in the formation of the alpha crystal phase gel structure, it will be inserted into the hydrophobic tail chain of the emulsifier bilayer, and will be solubilized in the alkane chain segment area of the amphiphilic component. Since the lipophilic sunscreen molecules have a certain polarity, the further introduced C9-C12 alkane solvent is to weaken the interaction between the hydrophobic tail chain of the alpha crystal phase emulsifier and the hydrophobic tail chain of the emulsifier bilayer.

[0012] In addition, the co-emulsifier with the same length of alkyl chain as the alpha crystal phase emulsifier is selected to make the alpha crystal phase emulsifier arrange more orderly and closely at the oil / water interface, reduce the mobility of the molecules, and promote the formation of the alpha crystal phase gel structure. If this component is lacking, the integrity and stability of the alpha crystal phase gel structure cannot be guaranteed.

[0013] Under the structure, the sunscreen ingredients are completely wrapped, so the stability of the sunscreen ingredients can be effectively guaranteed without introducing a large amount of stabilizing ingredients, thereby improving the SPF value of the product and avoiding the interaction between the sunscreen ingredients and the skin during use. Meanwhile, the phosphocholine polymer in the component concentrates on the outermost layer to form a secondary protective layer. After the component contacts the skin, the component forms a film, and the hydrophobic side chain of the component interacts with the hydrophobic group of the sunscreen ingredients, thereby hindering the subcutaneous penetration of the sunscreen ingredients, and finally avoiding the irritation of the sunscreen ingredients to the skin. Meanwhile, the lipophilic sunscreen, the hydrophilic sunscreen, and the peony extract extracted by the specific solvent in the product have a synergistic effect in terms of anti-ultraviolet, anti-blue light, anti-sunlight dermatitis, and post-sun care. The comprehensive effect of skin sunscreen and care is far superior to that of existing products, and the use experience of the product is good. The product is suitable for various skin types, including sensitive skin.

[0014] Preferably, the alpha crystal phase emulsifier is at least one of C20 alcohol phosphate, C22 alcohol phosphate, glycerol monostearate, cetyl alcohol phosphate, and olive oil polyglyceryl-6 ester.

[0015] More preferably, the alpha crystal phase emulsifier is C20 alcohol phosphate, and the co-emulsifier is arachidyl alcohol.

[0016] C20 alcohol phosphate is an anionic emulsifier with a linear monalkyl phosphate structure, which has strong emulsifying ability and high stability. Arachidyl alcohol is a high-carbon linear fatty acid with an amphiphilic structure, and the length of its hydrophobic carbon chain is comparable to that of C20 alcohol phosphate. Therefore, when the two are synergistically combined, the alpha crystal gel structure formed has the best integrity and stability.

[0017] More preferably, the weight ratio of C20 alcohol phosphate to arachidyl alcohol is (0.8-1.2):(0.8-1.2).

[0018] Preferably, the lipophilic sunscreen is at least one of ethylhexyl triazone (EHT), butyl methoxydibenzoylmethane (BMDM), homosalate (HMS), ethylhexyl salicylate (EHS), bis-ethylhexyloxyphenol methoxyphenyl triazine (BBT), and diethylamino hydroxybenzoyl hexyl benzoate (DHHB).

[0019] Preferably, the hydrophilic sunscreen is at least one of methylene bis-benzotriazolyl tetramethylbutylphenol (BBT), phenyl benzimidazole sulfonic acid (PBSA), and disodium phenyl dibenzimidazole sulfonate (DPDT).

[0020] As the main functional components in the sunscreen composition of the present application, the hydrophilic sunscreen agent and the lipophilic sunscreen agent, in addition to the difference in polarity, both need to maintain good sunscreen effect, and have protective effect on both ultraviolet UVA and UVB. The above-mentioned lipophilic and hydrophilic sunscreen agent types can all achieve the expected effect.

[0021] More preferably, the lipophilic sunscreen agent is a mixture of ethylhexyl triazone and bis-ethylhexyloxyphenol methoxyphenyl triazine, and the weight ratio of the two is 1:(0.5-5).

[0022] Ethylhexyl triazone is the most effective oil-soluble UVB band absorber at present, and has high light stability, and has no estrogen-like and androgen-like effects. Bis-ethylhexyloxyphenol methoxyphenyl triazine is also a new type of broad-spectrum ultraviolet absorber, and also has no estrogen-like and androgen-like effects. The inventors have found through experiments that the two substances can achieve excellent ultraviolet absorption and protection effect when they are used in the content limited by the relevant regulations.

[0023] More preferably, the hydrophilic sunscreen agent is methylene bis-benzotriazolyl tetramethylbutylphenol.

[0024] More preferably, the methylene bis-benzotriazolyl tetramethylbutylphenol is a dispersion of methylene bis-benzotriazolyl tetramethylbutylphenol, and the mass concentration is 40-60wt%.

[0025] Methylene bis-benzotriazolyl tetramethylbutylphenol has good absorption and protection effect on both ultraviolet UVA and UVB, and will not be absorbed by the skin, so it is very suitable for use in the sunscreen composition of the present application.

[0026] Preferably, the polar solvent is at least one of dibutyl adipate, propylene glycol dicaprylate / dicaprate, and coco-caprylate / caprate, and the non-polar solvent is at least one of isohexadecane and C9-C12 alkane.

[0027] Preferably, the solvent is a mixture of propylene glycol dicaprylate / dicaprate and C9-C12 alkane, and the weight ratio of the two is 1:(0.1-2).

[0028] As described above, the role of the solvent is to weaken the interaction between the lipophilic sunscreen agent and the hydrophobic tail chain of the alpha crystal phase emulsifier. Propylene glycol dicaprylate / dicaprate is a high-polarity oil that has good solubility for the lipophilic sunscreen agent itself, and C9-C12 alkane is a non-polar oil that can promote the alpha gel emulsifier to form a stable lamellar structure, so that the product has high spreading property and a refreshing and non-greasy skin feel. The two can achieve the best sunscreen effect and use experience when used in a specific ratio.

[0029] Preferably, the phosphorylcholine polymer is at least one of polyquaternium-51 (PMB), polyphosphocholine ethylene glycol acrylate (PMPC).

[0030] More preferably, the phosphorylcholine polymer is polyquaternium-51.

[0031] Polyquaternium-51 is an artificially synthesized cell membrane structure biomimetic material, which has higher compatibility with the skin when applied to the skin, can effectively form a biological protective film and inhibit the penetration of sunscreen ingredients, and also has certain moisturizing effect.

[0032] Preferably, the NaDES solvent is a mixture of butanediol and betaine, and the molar ratio of the two is (1-10):1.

[0033] More preferably, the preparation method of the NaDES solvent is: mixing butanediol and betaine at 75-80°C for 1-2h to obtain the NaDES solvent.

[0034] NaDES solvent is a low-melting point liquid formed by hydrogen bond acceptor and hydrogen bond donor through hydrogen bond interaction and liquefaction. When it contacts with plant raw materials, hydrogen bonds and van der Waals forces are formed. These interaction forces can more effectively and directionally extract water-soluble and oil-soluble active ingredients in plant raw materials, and the concentration of representative active ingredients such as polyphenols, flavonoids, and vitamins in the extraction product is higher, so the effect is better.

[0035] Preferably, the amount of peony extract is 1-1.5 parts.

[0036] Under the above ratio, the active ingredients in the peony extract can better play the excellent synergistic sunscreen and repair effect.

[0037] More preferably, the preparation method of the peony extract is: mixing peony branch / flower / leaf dry powder with an aqueous solution of NaDES solvent and ultrasonic extraction treatment, then performing solid-liquid separation, and the obtained liquid phase is concentrated, dried, and then dispersed with water to obtain the peony extract.

[0038] More preferably, the mass concentration of the aqueous solution of the NaDES solvent is 20-80%wt%, and the mass ratio of the aqueous solution of the NaDES solvent to the peony branch / flower / leaf dry powder is 1:(0.02-0.2).

[0039] More preferably, the ultrasonic power during the ultrasonic extraction treatment is 100-400W, and the treatment time is 1-2h. The solid-liquid separation adopts centrifugal separation treatment, and the speed during the centrifugal separation is 8000-12000r / min, and the time is 15-30min.

[0040] More preferably, the solute concentration of the peony extract is 0.1-0.8 mg / mL.

[0041] Through experiments of the inventor, the biological active ingredient molecules in the product prepared by the above conditions are smaller and richer, which not only can assist the sunscreen ingredients to achieve synergistic sunscreen and repair effects, but also can take into account the moisturizing and hydrating effects on the skin.

[0042] Preferably, the sunscreen composition containing peony active ingredients comprises the following components by weight:

[0043] C20 alcohol phosphate 1.5-2.5 parts, peanut alcohol 1.5-2.5 parts, ethylhexyl triazone 0.5-1.5 parts, bis-ethylhexyloxyphenol methoxyphenyl triazine 1-2 parts, methylene bis-benzotriazolyl tetramethyl butyl phenol 4.5-5.5 parts, propylene glycol dicaprylate / dicaprate 7.5-8.5 parts, C9-C12 alkane 1.5-2.5 parts, polyquaternary ammonium salt-51 0.3-0.8 parts, peony extract 0.5-1.5 parts, and water 28-32 parts.

[0044] The inventor found through experiments that the sunscreen composition prepared under the above preferred formula has the best synergistic skin sunscreen and after-sun repair effects, and excellent use experience.

[0045] Another object of the present application is to provide a preparation method of the sunscreen composition containing peony active ingredients, comprising the following steps:

[0046] (1) Mix the alpha crystal phase emulsifier, co-emulsifier and solvent and heat to 82-85℃ to dissolve, ultrasonic dispersion, then cool to 70-75℃ and add lipophilic sunscreen to dissolve, to obtain mixture A;

[0047] (2) Mix the hydrophilic sunscreen, peony extract and water and heat to dissolve, to obtain mixture B;

[0048] (3) Mix mixture A and mixture B and homogenize once, then add phosphocholine polymer and homogenize twice, cool, to obtain the sunscreen composition containing peony active ingredients.

[0049] The preparation method of the product of the present application has simple operation steps and low equipment requirements, and under the conditions, a complete alpha crystal phase gel structure can be formed in the product, which is beneficial to the stability, efficacy and skin mildness of the sunscreen ingredients and plant active ingredients.

[0050] Preferably, in the step (3), the rate of the first homogenization treatment is 7000-9000 rpm, the time is 2-4 min, the rate of the second homogenization treatment is 3000-5000 rpm, and the time is 2-4 min.

[0051] Another object of the present application is to provide a sunscreen cream comprising the sunscreen composition containing the active ingredient of the peony as described in the present application.

[0052] The sunscreen composition as described in the present application has excellent active efficacy and high compatibility with other components of the conventional sunscreen skin care products, and can be effectively applied in the preparation of the popular sunscreen products such as the sunscreen cream.

[0053] Preferably, in the sunscreen cream, the mass percentage content of the sunscreen composition containing the active ingredient of the peony is 10-60 wt%.

[0054] More preferably, the sunscreen cream comprises the following components with the mass percentage content: the sunscreen composition containing the active ingredient of the peony 10-60%, the humectant 1-10%, the thickening agent 0.1-2%, the pH adjusting agent 0.1-1%, the chelating agent 0.02-1%, the preservative 0.5-2%, and the balance of water.

[0055] More preferably, the humectant is at least one of butylene glycol, diglycerol, glycerol, panthenol; the thickening agent is at least one of carbomer, acrylates / C10-C30 alkyl acrylate crosspolymer, hydroxyethyl cellulose, xanthan gum; the pH adjusting agent is at least one of triethanolamine, arginine; the chelating agent is at least one of sodium gluconate, disodium EDTA, tetrasodium EDTA; and the preservative is at least one of caprylhydroxamic acid, p-hydroxyacetophenone, pentylene glycol, 1,2-hexanediol.

[0056] More preferably, the sunscreen cream is composed of the following components with the mass percentage content: the sunscreen composition containing the active ingredient of the peony 35-45%, butylene glycol 4-6%, carbomer 0.1-0.5%, arginine 0.5-1%, sodium gluconate 0.05-0.15%, p-hydroxyacetophenone 0.4-0.6%, pentylene glycol 0.4-0.6%, and the balance of water.

[0057] The sunscreen cream according to the present application can form a highly closed protective film on the surface of the skin after being in contact with the skin and being evenly applied under the formula, reducing the contact and penetration of sunscreen ingredients with the skin, while the sunscreen ingredients can fully cooperate with the plant active peony extract to play the sunscreen and care effects. Based on the high efficiency of the sunscreen composition, the sunscreen cream does not need to introduce sunscreen agents with potential allergenicity, the possibility of interfering with endocrine, and reproductive development toxicity such as octocrylene, benzophenone-3, homosalate, and methoxy cinnamic acid ethylhexyl ester, and does not need to add functional agents such as silicone oil, essence, alcohol, titanium dioxide, and the like which can easily increase the burden of the skin, block the pores, even breed acne and comedones, and the like, and has excellent use effect, is suitable for various skin types, and has a refreshing and comfortable feeling.

[0058] In addition, some conventional sunscreen cream products introduce some ingredients such as benzophenone-3, 4-methyl-alkyl camphor, methyl p-hydroxybenzoate, and ethyl p-hydroxybenzoate which cause coral bleaching, while the product according to the present application does not need to introduce such ingredients to achieve excellent effect, and thus belongs to marine biology friendly products.

[0059] The present application has the beneficial effect that the present application provides a sunscreen composition containing peony active ingredients, which has a gel network structure based on a specific formula composition, presents an oil-in-water system, and contains hydrophilic sunscreen agents and lipophilic sunscreen agents which can achieve high stability in the structure without using additional solvents or emulsifiers, while the two sunscreen agents can cooperate with the peony active ingredients and the remaining functional components to achieve high efficient comprehensive performance of anti-blue light, anti-oxidation, anti-sunlight dermatitis, and after-sun repair, without worrying about skin irritation or acne caused by excessive additives or complex ingredients in existing products; in addition, the product has good skin moisturizing effect, has high clarity and spreadability when used, has fast film forming speed, has small irritation, and has good use experience. BRIEF DESCRIPTION OF DRAWINGS

[0060] Figure 1 A schematic diagram of the stable structure of the sunscreen composition containing peony active ingredients according to the present application after being applied on the skin epidermis. DETAILED DESCRIPTION

[0061] In order to better illustrate the purposes, technical solutions and advantages of the present application, the present application will be further described below in combination with specific examples and comparative examples, which are intended to help understand the contents of the present application in detail, rather than limit the present application. All other examples obtained by those of ordinary skill in the art without any creative work shall fall within the protection scope of the present application. The experimental reagents and instruments involved in the implementation of the present application are all common reagents and instruments unless otherwise specified. The methylene bis-benzotriazolyl tetramethylbutylphenol used in each example and comparative example is a commercially available methylene bis-benzotriazolyl tetramethylbutylphenol dispersion with a mass concentration of 50wt%.

[0062] Examples 1-16

[0063] An embodiment of the present application relates to a sunscreen composition containing a peony active ingredient and a preparation method and application thereof. The raw material components of the sunscreen composition containing the peony active ingredient are shown in Table 1,

[0064] The α crystal phase emulsifier 1 is C20 alcohol phosphate;

[0065] The α crystal phase emulsifier 2 is cetyl alcohol phosphate;

[0066] The co-emulsifier 1 is arachidyl alcohol;

[0067] The co-emulsifier 2 is cetyl alcohol;

[0068] The hydrophilic sunscreen agent 1 is methylene bis-benzotriazolyl tetramethylbutylphenol;

[0069] The hydrophilic sunscreen agent 2 is a solution of phenyl benzimidazole sulfonic acid with a mass concentration of 25wt% (phenyl benzimidazole sulfonic acid: tromethamine: water 1:0.5:2.5);

[0070] The lipophilic sunscreen agent 1 is ethylhexyl triazone;

[0071] The lipophilic sunscreen agent 2 is bis-ethylhexyloxyphenol methoxyphenyl triazine;

[0072] The lipophilic sunscreen agent 3 is diethylamino hydroxybenzoyl hexyl benzoate;

[0073] The solvent 1 is propylene glycol dicaprylate / dicaprate;

[0074] The solvent 2 is C9-C12 alkane;

[0075] The phosphorylcholine polymer is polyquaternium-51;

[0076] The peony extract is self-made, and the preparation method is as follows: 200 g of commercially available peony branch / flower / leaf dry powder is sieved through a 100 mesh sieve, then mixed with a 2 kg aqueous solution of the NaDES solvent, and subjected to ultrasonic extraction treatment at 200 W for 1.5 h, then subjected to solid-liquid separation by centrifugation at 10,000 rpm for 30 min, the obtained liquid phase is concentrated into a paste by rotary evaporation at 45℃, dried to constant weight, then dispersed uniformly with water and configured into a dispersion liquid of 0.5 g / mL, and the peony extract is obtained.

[0077] The preparation method of the aqueous solution of the NaDES solvent is as follows: butanediol and betaine are mixed at a molar ratio of 5:1 at 75-80℃ for 1.5 h to obtain the NaDES solvent, then the NaDES solvent and water are mixed uniformly at a mass ratio of 1:2 to obtain the aqueous solution of the NaDES solvent.

[0078] The preparation method of the sunscreen composition containing the peony active ingredient comprises the following steps:

[0079] (1) The alpha crystal phase emulsifier, co-emulsifier and solvent are mixed and heated to 82-85℃ for dissolution, ultrasonic dispersion for 2-3 min until uniform, then cooled to 70-75℃ and the lipophilic sunscreen agent is added and dissolved to obtain mixture A;

[0080] (2) The hydrophilic sunscreen agent, peony extract and water are mixed and heated for dissolution to obtain mixture B;

[0081] (3) Mixture A and mixture B are mixed and subjected to primary homogenization treatment, then the phosphorylcholine polymer is added and subjected to secondary homogenization treatment, and cooled to obtain the sunscreen composition containing the peony active ingredient; wherein the primary homogenization treatment is at a speed of 8000 rpm for 3 min, and the secondary homogenization treatment is at a speed of 4000 rpm for 3 min.

[0082] Table 1

[0083]

[0084]

[0085] Comparative Examples 1-8

[0086] The differences between the comparative examples and Example 1 are only in the composition and ratio of the raw materials of the preparation components of the sunscreen composition, as shown in Table 2.

[0087] The emulsifier is cetylstearyl glucoside;

[0088] The co-emulsifier 3 is myristyl alcohol;

[0089] Table 2

[0090]

[0091]

[0092] Comparative Example 9

[0093] The difference between this comparative example and Example 1 is only that the preparation method of the peony extract is as follows: 200 g of commercially available peony branch / flower / leaf dry powder is sieved through a 100-mesh sieve, then 8 times the mass of water is added for dispersion and soaked at 60°C for 1 h, then 200W ultrasonic treatment is performed for 1.5 h, the mixture is subjected to solid-liquid separation, the liquid phase is collected, and the solid phase is subjected to the soaking and ultrasonic treatment steps for 3 times, the obtained liquid phases are combined, then subjected to solid-liquid separation by centrifugation at 10,000 rpm for 30 min, the obtained liquid phase is concentrated into a paste by rotary evaporation at 45°C, dried to constant weight, then uniformly dispersed with water and configured into a dispersion liquid of 0.5 g / mL, and the peony extract is obtained.

[0094] Comparative Example 10

[0095] The difference between this comparative example and Example 1 is only that the preparation method of the peony extract is as follows: 200 g of commercially available peony branch / flower / leaf dry powder is sieved through a 100-mesh sieve, then 1 L of anhydrous ethanol is added for soaking for 24 h, then constant temperature reflux is performed at 60°C for 3 h, then subjected to solid-liquid separation by centrifugation at 10,000 rpm for 30 min, the obtained liquid phase is concentrated into a paste by rotary evaporation at 45°C, dried to constant weight, then uniformly dispersed with water and configured into a dispersion liquid of 0.5 g / mL, and the peony extract is obtained.

[0096] Comparative Example 11

[0097] The difference between this comparative example and Example 1 is only that the peony extract is replaced by a scutellaria extract, and the preparation method of the scutellaria extract is as follows: 200 g of commercially available scutellaria dry powder is sieved through a 100-mesh sieve, then 1 L of anhydrous ethanol is added for soaking for 24 h, then constant temperature reflux is performed at 60°C for 3 h, then subjected to solid-liquid separation by centrifugation at 10,000 rpm for 30 min, the obtained liquid phase is concentrated into a paste by rotary evaporation at 45°C, dried to constant weight, then uniformly dispersed with water and configured into a dispersion liquid of 0.5 g / mL, and the scutellaria extract is obtained.

[0098] Comparative Example 12

[0099] The difference between this comparative example and Example 1 is only that the peony extract is replaced by a scutellaria extract, and the preparation method of the scutellaria extract is as follows: 200 g of commercially available scutellaria dry powder is sieved through a 100-mesh sieve, then mixed with 2 kg of an aqueous solution of a NaDES solvent and subjected to 200W ultrasonic extraction treatment for 1.5 h, then subjected to solid-liquid separation by centrifugation at 10,000 rpm for 30 min, the obtained liquid phase is concentrated into a paste by rotary evaporation at 45°C, dried to constant weight, then uniformly dispersed with water and configured into a dispersion liquid of 0.5 g / mL, and the scutellaria extract is obtained.

[0100] The method for preparing the aqueous solution of NaDES solvent is as follows: Butanediol and betaine are mixed and reacted at 75-80°C for 1.5 h in a molar ratio of 5:1 to obtain the NaDES solvent. Then, the NaDES solvent and water are mixed evenly in a mass ratio of 1:2 to obtain the aqueous solution of NaDES solvent.

[0101] Example of effect 1

[0102] To preliminarily verify that the sunscreen composition containing peony active ingredients described in this invention does not rapidly penetrate the skin and cause irritation, transdermal absorption tests were conducted on samples from various embodiments and comparative examples: Undamaged pig skin with the fat layer removed was selected under a dissecting microscope. Several pieces of skin of the same size were cut, washed with PBS, and the surface moisture was blotted dry with filter paper. The skin was fixed on a Franz diffusion cell, with the stratum corneum facing the administration chamber and the dermis facing the receiving chamber. 15 mL of PBS was added to the receiving chamber, and air bubbles were removed to ensure there were no air bubbles between the dermis and the receiving solution. The effective penetration area was 0.36π cm². 2 Turn on the instrument beforehand, adjust the water bath temperature to 32±1℃, set the stirring speed to 300rpm, and stir the sunscreen compositions prepared in each example / comparative example at 2.0mg / cm³. 2 The sample was applied to the surface of the stratum corneum at a certain rate, sealed with a sealing film, and covered with aluminum foil to prevent liquid evaporation. After 8 hours, the pigskin was removed, the surface residue was gently wiped with absorbent cotton, and the stratum corneum was peeled off with 3M medical tape. The pigskin was cut into pieces, extracted, and mixed with the liquid in the receiving cell. The mixture was filtered through a 0.45µm microporous membrane, and the transdermal absorption of the sunscreen was tested using HPLC according to the "Cosmetic Safety Technical Specifications (2015)".

[0103] The test results are shown in Table 3.

[0104] Table 3

[0105]

[0106]

[0107] As can be clearly seen from the table, when the α-crystalline emulsifier, co-emulsifier, solvent, and phosphorylcholine polymer in the sunscreen composition of the present invention are combined in a specific ratio, a gel structure and an outer protective film can be effectively formed, such as... Figure 1 As shown, this ensures that the transdermal absorption of the product remains at a low level after contact with the skin's epidermis, preventing the sunscreen ingredients from rapidly penetrating into the dermis. However, as can be seen from the comparative products, once the α-crystalline emulsifier is replaced with other conventional system components, it cannot effectively form an α-crystalline gel structure that maintains the stability and barrier properties of the sunscreen ingredients. As described in Comparative Example 1, its transdermal absorption reaches 5 μg / cm³. 2The above; at the same time, from Comparative Examples 3 and 4, it can be seen that the penetration of lipophilic sunscreen agents in the product is higher, and if all lipophilic sunscreen agent ingredients are selected, it is possible to cause more obvious skin irritation. From Comparative Example 7, it can be seen that the phosphocholine polymer is crucial for the skin isolation of the sunscreen components in the product, and if it is lacking, it will cause the sunscreen components to quickly enter the skin, thereby causing skin irritation problems.

[0108] Example 2

[0109] In order to verify the anti-blue light effect of the peony active ingredient-containing sunscreen composition according to the present application, the anti-blue light test was performed on the products prepared from each example and comparative example: HaCaT (human keratinocytes) in the logarithmic growth phase were inoculated in a 96-well plate at a density of 1.0 x 10 4 cell / mL, and cultured in a 37°C, 5% CO2 incubator for at least 24 h, the old culture solution was removed, washed with PBS, the blank group and the control group were replaced with new culture solution, and the experimental group was replaced with culture solution containing 1 mg / mL of the sunscreen composition obtained from the example / comparative example to be tested. The cells were irradiated with blue light at 15 J / cm 2 The distance was 30 cm, the cells in the blank group were not exposed to blue light, and after blue light irradiation, the cell survival rate of each group was determined by CellTiter 96 (MTS), each experiment was repeated three times, the average value of the final results was calculated, and the calculation formula of the cell survival rate was: cell survival rate (%) = sample group OD / blank group OD * 100%;

[0110] The results are shown in Table 4.

[0111] Table 4

[0112] Product Cell survival rate (%) Example 1 90.3 Example 2 91.6 Example 3 89.7 Example 4 82.3 Example 5 85.1 Example 6 78.4 Example 7 89.2 Example 8 87.7 Example 9 86 Example 10 78.8 Example 11 92.5 Example 12 79.4 Example 13 88.3 Example 14 90.5 Example 15 84.1 Example 16 84.0 Comparative Example 1 58.2 Comparative Example 2 67.4 Comparative Example 3 86.3 Comparative Example 4 57.6 Comparative Example 5 70.4 Comparative Example 6 50.7 Comparative Example 7 71.6 Comparative Example 8 53.6 Comparative Example 9 56.0 Comparative Example 10 54.9 Comparative Example 11 57.2 Comparative Example 12 62.5 Control group 55.0 Blank group 100

[0113] As can be seen from Table 4, the survival rate of the control group is only 55%, indicating that blue light irradiation has a greater impact on the lethality of cells, while after using the products of each example, the survival rate of the test cells reaches more than 75%, and the highest can reach more than 92%. In contrast, the cell survival rate of Comparative Examples 1 and 2 is lower, indicating that only under the gel structure of the alpha crystal phase, the sunscreen ingredients can fully play the anti-blue light effect, and other emulsion systems cannot achieve similar effects. At the same time, in terms of anti-blue light efficacy, hydrophilic sunscreen agents are more important than lipophilic sunscreen agents. If this component is missing, as described in Comparative Example 4, there is almost no anti-blue light effect after use. At the same time, according to the performance of Comparative Examples 6-12, solvents, phosphocholine polymers and peony extracts in the product also play a greater role in anti-blue light effect, especially peony extract, which can only be obtained by using NaDES solvent extraction process to ensure specific synergistic anti-blue light effect. If a conventional water extraction or alcohol extraction process is used, or an extract prepared from other plant materials, similar effects cannot be achieved.

[0114] Example 3

[0115] In order to verify that the sunscreen composition containing peony active ingredients according to the present application has an inhibitory effect on ultraviolet-induced inflammation, the products prepared in each example and comparative example were subjected to ultraviolet-induced anti-inflammatory test: several HaCaT (human keratinocytes) were taken and cultured in RPMI-1640 medium containing 10% fetal bovine serum, 100 U / mL penicillin and 100 μg / mL streptomycin at 37°C, 5% CO2, and saturated 98% humidity. Logarithmic growth phase cells were selected, inoculated in a 96-well culture plate, and cultured for 24 h until the cells were completely adherent. The blank group was replaced with new culture medium, and the experimental group was replaced with RPMI164 containing 1 mg / mL of sunscreen composition samples obtained from each example / comparative example. After 12 h of incubation, the cells were irradiated with 30 mJ / cm2dose of UVB at a distance of 15 cm. After irradiation, the cell culture supernatant was collected, and the concentration of IL-8 in the supernatant was detected using a human ELISA kit. Each experiment was repeated three times, and the average value was taken. The IL-8 inhibition rate was calculated, and the formula was as follows: IL-8 inhibition rate (%) = (A 2 / A 空白组 -A 样品组 ) / A 空白组 *100%.

[0116] The test results are shown in Table 5.

[0117] Table 5

[0118]

[0119]

[0120] As can be seen from Table 5, the products of the embodiments of the present application have a significant inhibitory effect on the inflammatory factor IL-8 generated by ultraviolet irradiation, and according to the products of the embodiments and comparative examples, it can be seen that the peony extract in the product is the key component corresponding to the effect, and the peony extract prepared by other traditional extraction methods cannot exert a similar effect to the peony extract extracted by the NaDES solvent described in the present application, and the extract products prepared from plant raw materials such as Scutellaria baicalensis Georgi, which has a similar active component composition to peony, also do not have a similar effect, indicating that the active component composition in the peony extract described in the present application has uniqueness with the IL-8 inhibitory effect; in addition, the excellent IL-8 inhibitory effect of each embodiment is due to the synergistic effect of other components in addition to the active components of the peony extract, as described in the products of Comparative Examples 7 and 8, the IL-8 inhibition rates of the products obtained are comparable when the phosphocholine polymer and the peony extract are absent, indicating that the two components have a synergistic effect in the anti-inflammatory process and are indispensable.

[0121] Example 4

[0122] In order to verify the comprehensive sunscreen effect of the sunscreen composition containing the active components of peony described in the present application, the products of the embodiments and comparative examples were prepared into sunscreen creams, and the raw materials for preparing the sunscreen creams are shown in Table 6.

[0123] Table 6

[0124] Component Mass percentage (%) Butylene glycol 5 Carbomer 0.2 Arginine 0.4 Sodium gluconate 0.1 p-Hydroxyacetophenone 0.5 Hexylene glycol 0.5 Example / Comparative Example Product 40 Water Balance

[0125] The preparation method of the sunscreen cream is as follows: the butanediol, carbomer, arginine, sodium gluconate, water and p-hydroxyacetophenone are mixed uniformly and heated to 60-65°C, and stirring is continued, the product of the embodiment / comparative example is added and homogenized at a speed of 3000 rpm for 3 min, cooled, mixed uniformly with hexanediol, filtered, and the sunscreen cream is obtained.

[0126] The prepared sunscreen cream was tested for SPF value: a needle syringe matched with the SPF-290 analyzer was used to drop the sunscreen cream obtained from each embodiment and comparative example in a dot shape on the surface of a PMMA substrate, a finger with a latex finger sleeve was used to spread it to form a uniform sample layer of 2 mg / cm 2 The sample layer was placed in an environment of 20°C and 60% humidity for natural drying for 20 min, 6 points were randomly selected on the transparent film for testing, and after the test was completed, the results of 6 tests were analyzed by the software matched with the SPF-290 analyzer, and the SPF value was calculated according to ISO24443. Each sample was tested three times, and the average value was taken as the final result. The test results are shown in Table 7.

[0127] Table 7

[0128] Product SPF value Example 1 45.6 Example 2 41.5 Example 3 42.7 Example 4 40.5 Example 5 40.7 Example 6 38.6 Example 7 44.1 Example 8 40.2 Example 9 45.3 Example 10 42.1 Example 11 45.5 Example 12 37.4 Example 13 41.6 Example 14 42.8 Example 15 44.5 Example 16 41.4 Comparative Example 1 25.6 Comparative Example 2 28.7 Comparative Example 3 29.5 Comparative Example 4 30.9 Comparative Example 5 41.3 Comparative Example 6 19.6 Comparative Example 7 36.4 Comparative Example 8 29.5 Comparative Example 9 35.4 Comparative Example 10 30.3 Comparative Example 11 39.6 Comparative Example 12 41

[0129] As can be seen from Table 7, the product of the present application has excellent comprehensive sunscreen effect, and the SPF value can be maintained at 35 or above, especially the product of Example 1, the SPF value can reach 45.6. In contrast, the SPF values of the products of Comparative Examples 1-6 are all low, which shows that in the product, in addition to the sunscreen ingredients, the α crystal phase emulsifier, the co-emulsifier and the solvent all play a synergistic effect, only under the α crystal phase gel structure, each active ingredient can fully exert the sunscreen effect; on the other hand, compared with the product of Comparative Example 8 which does not contain peony extract, the peony extracts prepared by the conventional water extraction and alcohol extraction method in Comparative Examples 9 and 10 are used as components, but the SPF value of the final product is not greatly improved, which shows that the peony extracts prepared by different processes are based on the difference of active ingredients, and not all have ideal sunscreen activity effect.

[0130] Effect Example 5

[0131] In order to verify the after-sun repair effect of the sunscreen composition containing peony active ingredients of the present application, the sunscreen cream prepared in Example 1 and the sunscreen cream prepared in Comparative Example 4 were evaluated for after-sun repair effect: each product was divided into an experimental group, and 10 volunteers were selected for each experimental group, aged 20-50 years old, all having sunburned skin, and having skin burning, red and swollen phenomena; the trans-epidermal water loss (TEWL) value of the volunteers on the left and right cheeks was measured by a CK instrument probe, and the average value of 3 values on the left and right cheeks was taken as the data of the skin water loss (TEWL) of the cheeks before use (D0). After the test, the volunteers needed to use the samples of each example and comparative example, and after cleaning the skin in the morning, an appropriate amount of sample was applied to the skin, and it was applied once a day at noon, and after 7 days of continuous use, the volunteers were interviewed, and the TEWL value of D7 was tested, and the use feeling was evaluated by the test results.

[0132] The test results are shown in Table 8.

[0133] Table 8

[0134] Product Moisture content change rate (%) TEWL change rate (%) Example 1 32.7 -25.6 Comparative Example 1 25.6 -18.5 Comparative Example 2 30.8 -20.9 Comparative Example 3 22.7 -25.0 Comparative Example 4 33.4 -14.7 Comparative Example 5 26.4 -12.5 Comparative Example 6 25.5 -8.1 Comparative Example 7 23.2 -16.8 Comparative Example 8 26.0 -13.6 Comparative Example 9 28.5 -20.4 Comparative Example 10 27.9 -17.2 Comparative Example 11 29.1 -21.6 Comparative Example 12 30.2 -22.1

[0135] The results show that although the product of this invention forms a protective film on the skin surface to inhibit the penetration of sunscreen ingredients, it does not affect the overall post-sun moisturizing effect of the product, and the transepidermal water loss rate of the skin after using the product is low. In contrast, the products of Comparative Examples 1-8, due to the absence and substitution of α-phase emulsifier, co-emulsifier, sunscreen agent, solvent, peony extract, and phosphocholine polymer, could not achieve the post-sun repair effect of the product of Example 1. The skin moisture content change rate after use was low or the transepidermal water loss rate was high (the two are not completely correlated). The performance of the products of Comparative Examples 9-12 was also inferior to that of the product of Example 1, indicating that the composition of active ingredients in peony extract also has a direct impact on the post-sun repair efficacy of the final product.

[0136] Example 6

[0137] To verify the superior user experience of the sunscreen composition containing peony active ingredients described in this invention, the sunscreen lotion prepared in Example 4 (prepared in Example 1) and the sunscreen lotion prepared in the comparative example were evaluated for skin feel and irritation. 130 subjects with sensitive skin, aged 25-45 years, who regularly use cosmetics, were recruited and randomly divided into 13 groups. Clinical trials were conducted to evaluate the sunscreen lotions prepared in Example 1 and the comparative example. The scoring criteria were as follows: Lightness was scored from 1 to 10 points based on oiliness, with higher scores indicating a lighter feel; Spreadability was scored from 1 to 10 points based on ease of application, with higher scores indicating better spreadability; Film-forming speed was scored from 1 to 10 points based on film-forming speed, with higher scores indicating faster film formation; Irritation was scored from 1 to 10 points, with higher scores indicating greater irritation (0 points indicating no irritation). Similar to Example 5, the same commercially available sunscreen was used as a control group for the same tests.

[0138] The statistical results are the average values ​​of each group, as shown in Table 9.

[0139] Table 9

[0140] Product Freshness Spreading property Film formation speed Irritation Example 1 9.7 9.5 9.2 0 Comparative Example 1 9.0 9.5 8.7 0.9 Comparative Example 2 9.6 9.3 9.1 0 Comparative Example 3 9.9 7.0 8.8 0 Comparative Example 4 7.5 7.5 8.6 0.8 Comparative Example 5 7.2 6.5 9.2 0.5 Comparative Example 6 8.5 7.3 7.6 1.2 Comparative Example 7 9.4 9.6 8.4 0.7 Comparative Example 8 9.6 9.6 9.1 0.6 Comparative Example 9 9.6 9.4 9.3 0.3 Comparative Example 10 9 9.6 9.0 0.4 Comparative Example 11 9.4 8.6 8.5 0.6 Comparative Example 12 9.5 8.9 8.3 0.3

[0141] As can be seen from Table 9, the sunscreen cream prepared from the sunscreen composition of the present application has excellent skin feel and use experience, high lightness and spreadability, fast film forming speed, and no irritation. Compared with the product of Example 1, the product of Comparative Example 1 has higher irritation, which corresponds to Example 1, indicating that when the gel structure cannot be formed in the product, the sunscreen ingredient will quickly penetrate the skin, resulting in irritation, and the absence of the structure also affects the use skin feel, spreadability and film forming property of the product. According to Comparative Examples 4 and 7-8, the irritation of the lipophilic sunscreen in the product is higher, and too much will cause skin irritation, while the choline phosphate polymer and peony extract in the product can synergistically inhibit the permeability of the sunscreen ingredient after being applied to the skin, and the absence of one of them will increase the irritation of the product. According to the products of Comparative Examples 9-12, when the plant active ingredients in the product are different, the skin feel, spreadability, film forming property and irritation degree of the product are different, and only the peony extract prepared by the specific process of the present application can achieve the ideal comprehensive effect, so that the product has good use experience.

[0142] Finally, it should be noted that the above examples are only used to illustrate the technical solutions of the present application and not to limit the protection scope of the present application. Although the present application has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solutions of the present application can be modified or replaced by equivalents without departing from the essence and scope of the technical solutions of the present application.

Claims

1. A sunscreen composition comprising an active ingredient of Paeonia suffruticosa, characterized in that, The sunscreen composition containing active ingredients of peony comprises the following components by weight: 0.5-3 parts of alpha crystal phase emulsifier, 0.5-6 parts of co-emulsifier, 1-5 parts of lipophilic sunscreen, 0.5-5 parts of hydrophilic sunscreen, 0.02-2 parts of phosphorylcholine polymer, 0.1-20 parts of peony extract, 5-20 parts of solvent and 25-30 parts of water; The alpha crystal phase emulsifier is at least one of C20 alcohol phosphate, C22 alcohol phosphate and cetyl alcohol phosphate; The phosphorylcholine polymer is polyquaternium-51; The co-emulsifier is at least one of cetyl alcohol, stearyl alcohol, arachidyl alcohol and behenyl alcohol; The solvent is a mixture of polar solvent and non-polar solvent; the polar solvent is propylene glycol dicaprylate / dicaprate; the non-polar solvent is at least one of isohexadecane and C9-C12 alkane; The peony extract is extracted by a NaDES solvent; the NaDES solvent is a mixture of butanediol and betaine, and the molar ratio of the two is (1-10):

1.

2. The sunscreen composition containing the active ingredient of Paeonia suffruticosa according to claim 1, wherein the active ingredient of Paeonia suffruticosa is contained in an amount of 0.01 to 10% by weight. The lipophilic sunscreen is at least one of ethylhexyl triazone, butyl methoxydibenzoylmethane, homosalate, ethylhexyl salicylate, bis-ethylhexyloxyphenol methoxyphenyl triazine and diethylamino hydroxybenzoyl hexyl benzoate; the hydrophilic sunscreen is at least one of methylene bis-benzotriazolyl tetramethylbutylphenol, phenylbenzimidazole sulfonic acid and disodium phenyl dibenzimidazole sulfonate.

3. The sunscreen composition containing the active ingredient of Paeonia suffruticosa according to claim 1, wherein the active ingredient of Paeonia suffruticosa is contained in an amount of 0.01 to 10% by weight. The preparation method of the NaDES solvent is as follows: butanediol and betaine are mixed and reacted at 75-80℃ for 1-2h to obtain the NaDES solvent.

4. The sunscreen composition containing the active ingredient of Paeonia suffruticosa according to claim 1, wherein the active ingredient of Paeonia suffruticosa is contained in an amount of 0.01 to 10% by weight. The preparation method of the peony extract is as follows: peony branch / flower / leaf dry powder is mixed with an aqueous solution of the NaDES solvent and subjected to ultrasonic extraction treatment, followed by solid-liquid separation; the obtained liquid phase is concentrated and dried, and then dispersed in water to obtain the peony extract; the solute concentration of the peony extract is 0.1-0.8mg / mL.

5. The sunscreen composition containing the active ingredient of Paeonia suffruticosa according to claim 1, wherein the active ingredient of Paeonia suffruticosa is contained in an amount of 0.01 to 10% by weight. The sunscreen composition containing active ingredients of peony comprises the following components by weight: C20 alcohol phosphate 1.5-2.5 parts, arachidyl alcohol 1.5-2.5 parts, ethylhexyl triazone 0.5-1.5 parts, bis-ethylhexyloxyphenol methoxyphenyl triazine 1-2 parts, methylene bis-benzotriazolyl tetramethylbutylphenol 4.5-5.5 parts, propylene glycol dicaprylate / dicaprate 7.5-8.5 parts, C9-C12 alkane 1.5-2.5 parts, polyquaternium-51 0.3-0.8 parts, peony extract 0.5-1.5 parts and water 28-32 parts.

6. The method for preparing the sunscreen composition containing the active ingredient of Paeonia suffruticosa according to any one of claims 1 to 5, wherein, The method comprises the following steps: (1) mixing the alpha crystal phase emulsifier, co-emulsifier and solvent, heating to 82-85℃ for dissolution, ultrasonic dispersion, then cooling to 70-75℃ and adding the lipophilic sunscreen for dissolution to obtain mixture A; (2) mixing the hydrophilic sunscreen, peony extract and water and heating for dissolution to obtain mixture B; (3) mixing mixture A and mixture B and once homogenization, then adding the phosphorylcholine polymer and twice homogenization, and cooling to obtain the sunscreen composition containing active ingredients of peony.

7. A sunscreen milk, characterized by A sunscreen composition comprising the peony active ingredient according to any one of claims 1 to 5.

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