Sunscreen spray capable of rapidly forming film and preparation method of sunscreen spray
The sunscreen spray prepared through specific ratios and treatment methods solves the skin sensitivity, insufficient sunscreen and stability of the sunscreen spray, improves the waterproofness and sunscreen index, and achieves effective protection and stability of the skin.
Patent Information
- Application Number
- CN202411561921.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-04
- Publication Date
- 2024-12-17
- Estimated Expiration
- Not applicable · inactive patent
AI Technical Summary
The existing sunscreen sprays have problems such as skin sensitivity, insufficient sun protection, poor storage stability, microplastic pollution and poor waterproofing, especially in the seaside environment, which cannot effectively protect the skin.
Using specific ratio raw materials, including ethylhexyl methoxycinnamate, sunscreen synergist, moisturizer, emulsifier and skin conditioner, a rapid film-forming sunscreen spray is prepared through fermentation and filtration. Enhance its sun protection index, stability and waterproofness while reducing irritation.
It improves the sun protection index and waterproofness of sunscreen spray, improves the skin's protective effect, reduces irritation, and maintains stability in different environments, meeting the needs of efficient protection and safe use.
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Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of cosmetics, and particularly relates to a fast-film-forming sunscreen spray and a preparation method thereof. Background Art
[0002] Sunscreen spray is a convenient sunscreen product that is sprayed on the skin in the form of a spray to help prevent UV damage to the skin. Unlike traditional products, sunscreen spray is easy to use and can be carried with you and re-sprayed at any time. It can make up for the problem of not being able to re-apply sunscreen when outdoors for a long time, and it does not have the greasy trouble of general sunscreen products.
[0003] As a convenient sunscreen product, sunscreen spray is indeed loved by many consumers, but due to its special design and ingredients, it also has some technical problems and potential risks: (1) Skin sensitivity: Some ingredients (such as some chemical sunscreens) may irritate the skin of some people and cause allergic reactions. (2) Insufficient sunscreen: Compared with sunscreen, the protective layer formed by sunscreen spray may be thinner, the SPF value is usually lower, and it cannot achieve a high level of UV protection. (3) Physical properties: The storage stability of sunscreen spray in different environments is not ideal. (4) Microplastic pollution: Some sunscreen sprays may contain microplastic components. These tiny particles are difficult to degrade after entering the water, causing long-term impacts on the environment. (5) Waterproofness: The seaside environment is a place where sunscreen sprays are frequently used, but some sunscreen sprays are not waterproof and the sunscreen effect cannot be guaranteed.
[0004] The existing technology usually uses physical sunscreens and chemical sunscreens to improve the sunscreen performance of sunscreen sprays. For example, the full-band chemical sunscreen oxatriazole is compounded with nano titanium dioxide to effectively improve the sunscreen performance of sunscreen spray aerosols. However, the nano titanium dioxide particles in the sunscreen spray are easily inhaled during use, which may cause irritation or damage to the respiratory tract. Long-term inhalation of nanoparticles may also have adverse effects on lung health, which cannot meet the needs of the existing market.
[0005] Therefore, there is an urgent need for a fast film-forming sunscreen spray and a preparation method thereof. Summary of the invention
[0006] The purpose of the present invention is to provide a fast film-forming sunscreen spray and a preparation method thereof.
[0007] In order to achieve the above object, the present invention provides the following technical solutions:
[0008] A fast film-forming sunscreen spray comprises the following raw materials in percentage by weight: 1-3% of ethylhexyl methoxycinnamate, 1-3% of diethylhexyl butyramido triazone, 2-4% of sunscreen enhancer, 4-6% of moisturizer, 1-2% of skin conditioner, 5-6% of emulsifier, 1-2% of glyceryl stearate citrate, 0.8-1.4% of polydimethylsiloxane, 0.03-0.06% of disodium EDTA, 0.05-0.1% of phenoxyethanol, 0.1-0.3% of methylparaben, and the balance is water.
[0009] Furthermore, the preparation method of the sunscreen enhancer comprises the following steps:
[0010] (1) Plumeria alba flowers, Helichrysum angustifolium flowers and Perilla frutescens leaves are mixed and crushed to less than 100 meshes to obtain mixed micro powder;
[0011] (2) Mixing the mixed micropowder and water in a weight ratio of 1:(10-15) to obtain a first mixed solution, adding composite bacteria to the first mixed solution, wherein the composite bacteria includes Lactobacillus acidophilus, Bifidobacterium lactis and Bifidobacterium breve, and the amount of Lactobacillus acidophilus is 10 6 -10 7 CFU / mL first mixed solution; the dosage of Bifidobacterium lactis is 10 7 -10 8 CFU / mL first mixed solution; the dosage of Bifidobacterium breve is 10 8 -10 9 CFU / mL first mixed solution; ferment at 38-40°C for 6-8h, sterilize, and obtain a first fermentation solution;
[0012] (3) filtering the first fermentation broth using a 0.22-0.45 μm filter membrane, and spray-drying the filtrate to obtain a sunscreen enhancer.
[0013] Furthermore, the weight ratio of white frangipani flowers, white leaf immortelle flowers and white osmanthus leaves is 1:(1.2-1.4):(0.6-0.8).
[0014] In the prior art, the sun protection index is often increased by increasing the amount of sunscreen added, but too much sunscreen will cause a burden on the skin, affect the feeling of use, and make the skin feel stuffy. The present invention can improve the sun protection index of the sunscreen spray by adding a sunscreen synergist. The sunscreen synergist is fermented by specific strains and is rich in natural antioxidants, such as flavonoids, polyphenols, etc., which can neutralize free radicals and reduce oxidative stress caused by ultraviolet rays, thereby protecting the skin from ultraviolet damage. At the same time, the sunscreen synergist can improve the dispersibility of the sunscreen in the formula, so that it forms a more uniform protective layer on the skin surface, without using too much sunscreen, and can improve the overall sunscreen effect. However, the addition of the sunscreen synergist will cause the sunscreen spray to produce certain skin irritation.
[0015] Furthermore, the moisturizing agent is selected from one or more of glycerol glucoside, oldenlandia diffusa extract, and ginkgo biloba root extract.
[0016] Furthermore, the moisturizing agent comprises glycerol glucoside, OLDENLANDIADIFFUSA extract and LITHOSPERMUMOFFICINALE root extract in a weight ratio of (0.3-0.5):(1.4-1.6):1.
[0017] Furthermore, the preparation method of the ginkgo lithospermum root extract comprises the following steps:
[0018] (1) crushing the ginkgo lithospermum officinale root to less than 100 meshes to obtain ginkgo lithospermum officinale root powder;
[0019] (2) mixing the root of Ginkgo biloba and water in a weight ratio of 1:(10-15) to obtain a second mixed solution; adding animal Bifidobacterium to the second mixed solution, wherein the amount of animal Bifidobacterium is 10 6 -10 7 CFU / mL second mixed solution; ferment at 38-40℃ for 3-5h, sterilize, and continue to add Lactobacillus casei, the amount of Lactobacillus casei is 10 8 -10 9 CFU / mL second mixed solution, ferment at 38-40°C for 3-5h, sterilize, and finally add Lactobacillus brevis, the amount of Lactobacillus brevis is 107-108 CFU / mL second mixed solution, ferment at 38-40°C for 2-4h, sterilize to obtain a second fermentation liquid;
[0020] (3) The second fermentation broth is filtered using a 0.22-0.45 μm filter membrane, and the filtrate is spray-dried to obtain a ginkgo root extract.
[0021] The present invention can improve the irritation of the sunscreen spray by adding a moisturizer to the sunscreen spray, making the sunscreen spray safe and non-irritating, and improving the waterproofness of the sunscreen spray. Analysis shows that glycerol glucoside is an efficient moisturizer, which can attract and lock the moisture in the skin, maintain the hydration state of the skin, and reduce the skin irritation and discomfort caused by dryness. The oldenlandia diffusa extract has a significant anti-inflammatory effect, can reduce the skin inflammatory reaction caused by ultraviolet rays, and alleviate the symptoms such as redness, swelling, and pain after sun exposure. The ginkgo lithospermum root extract is rich in antioxidants, such as shikonin, etc., which can neutralize the free radicals caused by ultraviolet rays, reduce the oxidative stress of the skin, and protect the skin from damage. At the same time, the moisturizer has film-forming properties, can form a transparent protective film on the skin surface, make the sunscreen agent better attached to the skin, reduce the shedding caused by friction or sweat, and improve the waterproofness of the sunscreen spray.
[0022] Furthermore, the emulsifier is selected from one or more of cetyl PEG / PPG-10 / 1 polydimethylsiloxane, glyceryl stearate citrate, and polyglyceryl-4 isostearate.
[0023] Further, the emulsifier includes cetyl PEG / PPG-10 / 1 polydimethylsiloxane, glyceryl stearate citrate and polyglyceryl-4 isostearate in a weight ratio of (1.5-1.7):1:(0.2-0.4).
[0024] The present invention can improve the stability of the sunscreen spray at room temperature by adding an emulsifier. The emulsifier can mix oil and water together to form a stable emulsion. In the sunscreen spray, the emulsifier can evenly mix the oily sunscreen and the aqueous component to prevent stratification and separation. When a specific ratio of emulsifiers, a specific ratio of white frangipani flowers, white leaf immortelle flowers and white osmanthus leaves, and a ginkgo lithospermum root extract prepared by a specific preparation method are used, the stability of the sunscreen spray at low and high temperatures can be improved. Analysis shows that emulsifiers have different HLB values, and a suitable emulsifier combination can better adapt to the formula requirements of the sunscreen spray. The system stability under this condition is better, and the natural ingredients in the extract can enhance the stability of the formula.
[0025] Furthermore, the skin conditioning agent is selected from one or more of yeast / rice fermentation product filtrate, neopentyl glycol diheptanoate, and D-panthenol.
[0026] In order to improve the stability of the sunscreen spray under accelerated conditions, the skin conditioner further comprises yeast / rice fermentation product filtrate, neopentyl glycol diheptanoate and D-panthenol in a weight ratio of (1.2-1.4):1:(0.4-0.6).
[0027] The present invention also provides a method for preparing the fast film-forming sunscreen spray, comprising the following steps:
[0028] (1) adding water, disodium EDTA and methylparaben into a water phase pot, stirring and heating to 80-85° C. until completely dissolved, and keeping the temperature for 15-20 minutes to obtain a water phase component;
[0029] (2) adding ethylhexyl methoxycinnamate, diethylhexyl butyramido triazone, emulsifier, glyceryl stearate citrate and polydimethylsiloxane into an oil phase pot, stirring and heating to 80-85° C. until completely dissolved, and keeping the temperature for 15 minutes to obtain an oil phase component;
[0030] (3) mixing the aqueous phase component and the oil phase component, and homogenizing at a speed of 1800-2000 rpm for 5-10 min to obtain a mixed material;
[0031] (4) Cooling the mixture to 40-45° C., adding the remaining components, homogenizing at a rate of 1000-1200 rpm for 5-8 min, cooling to room temperature, and filling to obtain the fast film-forming sunscreen spray.
[0032] Compared with the prior art, the advantages and beneficial effects of the present invention are:
[0033] 1. The present invention can improve the sun protection index of the sunscreen spray by adding a sunscreen synergist.
[0034] 2. The present invention can improve the irritation of the sunscreen spray by adding a moisturizer into the sunscreen spray, making the sunscreen spray safe and non-irritating, and at the same time improve the waterproofness of the sunscreen spray.
[0035] 3. When a specific ratio of emulsifiers, a specific ratio of white frangipani flowers, white leaf immortelle flowers and white osmanthus leaves and a ginkgo root extract prepared by a specific preparation method are used, the stability of sunscreen spray at low and high temperatures can be improved.
[0036] 4. By adding skin conditioners in a specific ratio, the stability of sunscreen spray under accelerated conditions can be improved. DETAILED DESCRIPTION
[0037] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0038] The raw materials used in the following examples of the present invention are all commercially available products:
[0039] Lactobacillus acidophilus, accession number: CCTCCAB2010208, was purchased from China Center for Type Culture Collection.
[0040] Bifidobacterium animalis, accession number: SHBCCD24407AS1.1852, was purchased from China Center for Type Culture Collection.
[0041] Lactobacillus casei, accession number: SHBCCD24737, was purchased from Shanghai Microbiological Collection Center.
[0042] Bifidobacterium lactis, accession number: SHBCCD24675, was purchased from Shanghai Microbiological Collection Center.
[0043] Bifidobacterium breve, accession number: SHBCCD24424JCM7017, was purchased from Shanghai Microbiological Collection Center.
[0044] Lactobacillus brevis, accession number: SHBCCD14346, was purchased from Shanghai Microbiological Collection Center.
[0045] Glyceryl Stearate Citrate, CAS: 55840-13-6.
[0046] Polydimethylsiloxane, Wuhan Huaxiang Kejie Biotechnology Co., Ltd., KF-6017 polydimethylsiloxane.
[0047] Cetyl PEG / PPG-10 / 1 polydimethylsiloxane, Wuhan Lanabai Pharmaceutical Chemical Co., Ltd.
[0048] Glyceryl stearate citrate, Wuhan Huaxiang Kejie Biotechnology Co., Ltd., CAS: 55840-13-6.
[0049] Polyglyceryl-4 isostearate, CAS No. 91824-88-3, Wuhan Kanos Technology Co., Ltd.
[0050] Glyceryl glucoside, CAS: 22160-26-5, Wuhan Lanabai Pharmaceutical Chemical Co., Ltd.
[0051] Oldenlandia diffusa extract, Jinhui (Guangzhou) Technology Co., Ltd.
[0052] Yeast / rice fermentation product filtrate was purchased from Jining Tangyi Chemical Co., Ltd., cosmetic grade.
[0053] Neopentyl glycol diheptanoate, CAS: 68855-18-5. Jining Tangyi Chemical Co., Ltd.
[0054] D-Panthenol, Shanghai Quanyan Biotechnology Co., Ltd.
[0055] Example 1
[0056] The present embodiment provides a fast film-forming sunscreen spray, comprising the following raw materials in percentage by weight: 2.2% of ethylhexyl methoxycinnamate, 1.5% of diethylhexyl butyramido triazone, 3.4% of sunscreen enhancer, 5.7% of moisturizer, 1.8% of skin conditioner, 5.3% of emulsifier, 1.4% of glyceryl stearate citrate, 1.1% of polydimethylsiloxane, 0.04% of disodium EDTA, 0.07% of phenoxyethanol, 0.2% of methylparaben, and the balance is water;
[0057] The preparation method of the sunscreen enhancer comprises the following steps:
[0058] (1) mixing white frangipani flowers, white leaf immortelle flowers and white osmanthus leaves in a weight ratio of 1:1.3:0.7, and crushing to less than 100 mesh to obtain a mixed fine powder;
[0059] (2) Mixing the mixed micropowder and water in a weight ratio of 1:12 to obtain a first mixed solution, adding composite bacteria to the first mixed solution, wherein the composite bacteria includes Lactobacillus acidophilus, Bifidobacterium lactis and Bifidobacterium breve, and the amount of Lactobacillus acidophilus is 10 6 CFU / mL first mixed solution; the dosage of Bifidobacterium lactis is 10 8 CFU / mL first mixed solution; the dosage of Bifidobacterium breve is 10 9 CFU / mL first mixed solution; ferment at 39°C for 7h, sterilize, and obtain a first fermentation solution;
[0060] (3) Filter the first fermentation broth using a 0.22 μm filter membrane, and spray-dry the filtrate to obtain a sunscreen enhancer.
[0061] The emulsifier includes cetyl PEG / PPG-10 / 1 polydimethylsiloxane, glyceryl stearate citrate and polyglyceryl-4 isostearate in a weight ratio of 1.6:1:0.3.
[0062] The moisturizing agent comprises glycerol glucoside, oldenlandia diffusa extract and ginkgo biloba root extract in a weight ratio of 0.4:1.5:1.
[0063] The preparation method of the ginkgo lithospermum root extract comprises the following steps:
[0064] (1) crushing the ginkgo lithospermum officinale root to less than 100 meshes to obtain ginkgo lithospermum officinale root powder;
[0065] (2) mixing the ginkgo lithospermum root and water in a weight ratio of 1:12 to obtain a second mixed solution; adding animal Bifidobacterium to the second mixed solution, wherein the amount of animal Bifidobacterium is 10 6 CFU / mL second mixed solution; ferment at 39°C for 4h, sterilize, and continue to add Lactobacillus casei, the amount of Lactobacillus casei is 10 8CFU / mL of the second mixed solution, fermented at 39°C for 4h, sterilized, and finally added with Lactobacillus brevis at a dosage of 10 7 CFU / mL second mixed solution, ferment at 39°C for 3h, sterilize to obtain second fermentation solution;
[0066] (3) The second fermentation broth was filtered using a 0.22 μm filter membrane, and the filtrate was spray-dried to obtain a ginkgo root extract.
[0067] The skin conditioning agent includes yeast / rice fermentation product filtrate, neopentyl glycol diheptanoate and D-panthenol in a weight ratio of 1.3:1:0.5.
[0068] The method for preparing the fast film-forming sunscreen spray comprises the following steps:
[0069] (1) adding water, disodium EDTA and methylparaben into a water phase pot, stirring and heating to 82° C. until completely dissolved, and keeping the temperature for 18 minutes to obtain a water phase component;
[0070] (2) adding ethylhexyl methoxycinnamate, diethylhexyl butyramido triazone, emulsifier, glyceryl stearate citrate and polydimethylsiloxane into an oil phase pot, stirring and heating to 82° C. until completely dissolved, and keeping the temperature for 15 minutes to obtain an oil phase component;
[0071] (3) mixing the aqueous phase component and the oil phase component under a vacuum degree of -0.5 MPa, and homogenizing at a rate of 1900 rpm for 8 min to obtain a mixed material;
[0072] (4) The mixture was cooled to 42° C., the remaining components were added, and the mixture was homogenized at a rate of 1100 rpm for 7 min. The mixture was cooled to room temperature and filled to obtain the fast film-forming sunscreen spray.
[0073] Example 2
[0074] The present embodiment provides a fast film-forming sunscreen spray, comprising the following raw materials in percentage by weight: 3% ethylhexyl methoxycinnamate, 1% diethylhexyl butyramido triazone, 4% sunscreen enhancer, 4% moisturizer, 2% skin conditioner, 5% emulsifier, 2% glyceryl stearate citrate, 0.8% polydimethylsiloxane, 0.06% disodium EDTA, 0.05% phenoxyethanol, 0.3% methylparaben, and the balance is water;
[0075] The preparation method of the sunscreen enhancer comprises the following steps:
[0076] (1) mixing white frangipani flowers, white leaf helichrysanthemum flowers and white osmanthus leaves in a weight ratio of 1:1.2:0.8, and crushing to less than 100 mesh to obtain a mixed fine powder;
[0077] (2) Mixing the mixed micropowder and water in a weight ratio of 1:10 to obtain a first mixed solution, adding composite bacteria to the first mixed solution, wherein the composite bacteria includes Lactobacillus acidophilus, Bifidobacterium lactis and Bifidobacterium breve, and the amount of Lactobacillus acidophilus is 10 7 CFU / mL first mixed solution; the dosage of Bifidobacterium lactis is 10 7 CFU / mL first mixed solution; the dosage of Bifidobacterium breve is 10 9 CFU / mL first mixed solution; ferment at 38°C for 8h, sterilize, and obtain a first fermentation solution;
[0078] (3) Filter the first fermentation broth using a 0.22 μm filter membrane, and spray-dry the filtrate to obtain a sunscreen enhancer.
[0079] The emulsifier includes cetyl PEG / PPG-10 / 1 polydimethylsiloxane, glyceryl stearate citrate and polyglyceryl-4 isostearate in a weight ratio of 1.5:1:0.2.
[0080] The moisturizing agent comprises glycerol glucoside, oldenlandia diffusa extract and ginkgo biloba root extract in a weight ratio of 0.3:1.4:1.
[0081] The preparation method of the ginkgo lithospermum root extract comprises the following steps:
[0082] (1) crushing the ginkgo lithospermum officinale root to less than 100 meshes to obtain ginkgo lithospermum officinale root powder;
[0083] (2) mixing the ginkgo lithospermum root and water in a weight ratio of 1:15 to obtain a second mixed solution; adding animal Bifidobacterium to the second mixed solution, wherein the amount of animal Bifidobacterium is 10 7 CFU / mL second mixed solution; ferment at 40℃ for 5h, sterilize, and continue to add Lactobacillus casei, the amount of Lactobacillus casei is 10 8 CFU / mL of the second mixed solution, fermented at 40°C for 3h, sterilized, and finally added with Lactobacillus brevis at a dosage of 10 8 CFU / mL second mixed solution, fermented at 40°C for 4h, sterilized to obtain a second fermentation solution;
[0084] (3) The second fermentation broth was filtered using a 0.22 μm filter membrane, and the filtrate was spray-dried to obtain a ginkgo root extract.
[0085] The skin conditioning agent includes yeast / rice fermentation product filtrate, neopentyl glycol diheptanoate and D-panthenol in a weight ratio of 1.2:1:0.4.
[0086] The method for preparing the fast film-forming sunscreen spray comprises the following steps:
[0087] (1) adding water, disodium EDTA and methylparaben into a water phase pot, stirring and heating to 85° C. until completely dissolved, and keeping the temperature for 20 minutes to obtain a water phase component;
[0088] (2) adding ethylhexyl methoxycinnamate, diethylhexyl butyramido triazone, emulsifier, glyceryl stearate citrate and polydimethylsiloxane into an oil phase pot, stirring and heating to 80° C. until completely dissolved, and keeping the temperature for 15 minutes to obtain an oil phase component;
[0089] (3) mixing the aqueous phase component and the oil phase component under a vacuum degree of -0.5 MPa, and homogenizing at a rate of 2000 rpm for 5 min to obtain a mixed material;
[0090] (4) The mixture is cooled to 45° C., the remaining components are added, and the mixture is homogenized at a rate of 1200 rpm for 8 min. The mixture is cooled to room temperature and filled to obtain the fast film-forming sunscreen spray.
[0091] Comparative Example 1
[0092] The difference between this comparative example and Example 1 is: a fast-film-forming sunscreen spray, comprising the following raw materials in percentage by weight: 3.2% of ethylhexyl methoxycinnamate, 0.5% of diethylhexyl butyramido triazone, 4.4% of sunscreen enhancer, 2.7% of moisturizer, 2.8% of skin conditioner, 6.3% of emulsifier, 1.4% of glyceryl stearate citrate, 1.1% of polydimethylsiloxane, 0.04% of disodium EDTA, 0.07% of phenoxyethanol, 0.2% of methylparaben, and the balance is water.
[0093] Comparative Example 2
[0094] The difference between this comparative example and Example 1 is that white frangipani flowers, white leaf immortelle flowers and white osmanthus leaves are mixed in a weight ratio of 1:1:1, and crushed to less than 100 meshes to obtain mixed micro powder.
[0095] Comparative Example 3
[0096] The difference between this comparative example and Example 1 is that the composite bacteria include animal Bifidobacterium, Lactobacillus casei and Lactobacillus brevis. The amount of animal Bifidobacterium is 10 6 CFU / mL first mixed solution; the dosage of Lactobacillus casei is 10 8 CFU / mL first mixed solution; the dosage of Lactobacillus brevis is 10 9 CFU / mL of the first mixed solution.
[0097] Comparative Example 4
[0098] The difference between this comparative example and Example 1 is that the emulsifier includes cetyl PEG / PPG-10 / 1 polydimethylsiloxane, glyceryl stearate citrate and polyglyceryl-4 isostearate in a weight ratio of 1:1:1.
[0099] Comparative Example 5
[0100] The difference between this comparative example and Example 1 is that the emulsifier includes polyglycerol 3 polyricinoleate, PEG-30 dipolyhydroxystearate and PEG-20 sorbitan isostearate in a weight ratio of 1.6:1:0.3, all of which are purchased from Shanghai Yoshida Chemical Industry Co., Ltd.
[0101] Comparative Example 6
[0102] The difference between this comparative example and Example 1 is that the moisturizing agent comprises glycerol glucoside, Hedyotis diffusa extract and Ginkgo biloba root extract in a weight ratio of 1:1:1.
[0103] Comparative Example 7
[0104] The difference between this comparative example and Example 1 is that the ginkgo lithospermum root extract is a commercially available product purchased from Ningxia Kaiyuan Biotechnology Co., Ltd., and is extracted in a 10:1 ratio.
[0105] Comparative Example 8
[0106] The difference between this comparative example and Example 1 is that different strains are used in the preparation of the ginkgo lithospermum root extract, and the ginkgo lithospermum root and water are mixed in a weight ratio of 1:12 to obtain a second mixed solution; Lactobacillus acidophilus is added to the second mixed solution, and the amount of Lactobacillus acidophilus is 10 6 CFU / mL second mixed solution; ferment at 39℃ for 4h, sterilize, and continue to add Bifidobacterium breve, the amount of Bifidobacterium breve is 10 8 CFU / mL of the second mixed solution, fermented at 39°C for 4h, sterilized, and finally added with Lactobacillus brevis at a dosage of 10 7 CFU / mL of the second mixed solution, ferment at 39°C for 3h, and sterilize to obtain a second fermentation solution.
[0107] Comparative Example 9
[0108] The difference between this comparative example and Example 1 is that the skin conditioner comprises yeast / rice fermentation product filtrate, neopentyl glycol diheptanoate and D-panthenol in a weight ratio of 1:1:1.
[0109] Performance Testing
[0110] The sunscreen sprays prepared in Examples 1-2 and Comparative Examples 1-9 were used as samples for performance testing.
[0111] 1. Human skin patch test
[0112] Test population: Volunteers aged between 20 and 50 were selected and randomly divided into 9 groups, with 20 people in each group;
[0113] Test method: First clean the skin of the test area with physiological saline and wait for 5 minutes to dry; select a qualified patch tester, take 0.5mL of sample into the patch tester in a closed patch test, and apply special tape to the back of the subject, and ask the subject how it feels; bathing is prohibited during the test; the subject keeps the patch area dry within 48 hours, avoids intense exercise, scratching the patch area, and long-term sunlight exposure, etc. After 48 hours, remove the tester and mark it. After 30 minutes, wait for the indentation to disappear and make a judgment under sufficient light. Record the results according to the skin reaction grade standard in the "Hygiene Standards for Skin Care Products". The skin adverse reaction grade standard is shown in Table 1 below. If there is any discomfort during the process, stop the test immediately. The results are shown in Table 2.
[0114] Table 1 Grading of skin adverse reactions
[0115]
[0116]
[0117] Table 2 Human skin patch test results
[0118]
[0119] It can be seen from Table 1 that in Comparative Example 1, the ratio of the sunscreen spray is changed, and the irritation of the sunscreen spray becomes greater. In Comparative Example 6, the ratio of the moisturizer is different. In Comparative Example 7, the ginkgo lithospermum root extract is a commercially available product. In Comparative Example 8, different strains of bacteria are used in the preparation of the ginkgo lithospermum root extract, all of which will lead to greater irritation of the sunscreen spray. This shows that the synergistic combination of components can improve the irritation of the sunscreen spray, and the moisturizer has a significant effect on improving the irritation of the sunscreen spray.
[0120] 2. Human body sun protection performance test:
[0121] Determination of SPF value of cosmetics:
[0122] The test was carried out in accordance with the specific requirements of the "Technical Specifications for Safety of Cosmetics" (2015 edition). A xenon arc lamp was used as a daylight simulator, and all performance indicators met the requirements of the measurement specifications. A total of 9 subjects were selected, including 0 males and 9 females, divided into 9 groups, with 1 person in each group, aged 30 to 50 years old, with an average age of 42.0±6.9 years old, which met the voluntary selection criteria for the subjects.
[0123] Reference substance: SPF value 16.1±2.4, prepared according to the standard formula of medium-high SPF standard substance (P2) in the "Technical Specifications for Safety of Cosmetics" (2015 edition). The subject takes a prone position and the back is irradiated. The minimum erythema dose (MED value) of the subject's skin to ultraviolet radiation is predicted 24 hours before the test, and the ultraviolet radiation dose is adjusted according to the predicted results for the test object. On the day of the test, a spot no less than 30cm on the subject's back is first selected. 2 Normal skin area, (2.00±0.05)mg / cm 2 Apply the test object or reference substance evenly on the above-mentioned area with the dosage, and then select the irradiation dose according to the specification requirements, and irradiate in three situations: ① Do not apply the test object on the subject's skin; ② Apply the reference substance; ③ Apply the test object.
[0124] The experimental results were observed after 24 hours, and the MED values under the three conditions were recorded respectively.
[0125] SPF value calculation method:
[0126] The SPF value of the test article or reference article for protecting a single subject is expressed as follows:
[0127] SPFi = MED value of protected skin ÷ MED value of unprotected skin
[0128] Determination of cosmetic long-wave ultraviolet protection index (PFA value):
[0129] The inspection was carried out in accordance with the specific requirements of the "Technical Specification for Safety of Cosmetics" (2015 edition). A daylight simulator xenon arc lamp was used, and all performance indicators met the requirements of the measurement specifications. A total of 9 subjects were selected, including 4 males and 5 females, and divided into 9 groups, with 1 person in each group. They ranged in age from 29 to 55 years old, with an average age of 42.4±4.7 years old, and met the voluntary inclusion criteria for the subjects. Control substance: PFA value 12.7±2.0, prepared according to the S2 formula in the ISO24442 method. The subject lies in a prone position, and his back is irradiated. The minimum melanization amount (MPPD value) of the subject's skin to ultraviolet radiation is predicted 24 hours before the test, and the ultraviolet radiation amount is adjusted according to the predicted results for the test object. The test first selects an area of no less than 30cm on the subject's back. 2 For normal skin area, (2.00±0.05)mg / cm 2 Apply the test object or reference product evenly on the above area; then select the UVA exposure amount according to the specification requirements, and irradiate in three situations: ① No test object is applied to the subject's skin; ② The reference product is applied; ③ The test object is applied. Observe the experimental results after 2-4 hours, and record the MPPD values in the three situations respectively.
[0130] Calculation method of PFA value:
[0131] The PFA value of the test substance or reference substance protecting a single subject is expressed as follows:
[0132] PFAi = MPPD value of protected skin ÷ MPPD value of unprotected skin
[0133] Individual PFA values are required to be accurate to one decimal place. The arithmetic mean of the PFA values of all subjects of the measured object protection is calculated, and the integer part is the PFA value of the measured sample. The sampling error of the estimated mean can calculate the standard deviation and standard error of the group of data. The 95% confidence interval (95% CI) of the mean is required to be no more than 17% of the mean. The number of subjects is increased until the above requirements are met, but it shall not exceed 25 people.
[0134] The results are shown in Table 3.
[0135] Table 3 SPF and PFA values
[0136]
[0137]
[0138] As shown in Table 3, in Comparative Example 1, the sun protection index decreased significantly by changing the ratio of the sunscreen spray. In Comparative Example 2, the ratios of white frangipani flowers, white leaf immortelle flowers and white osmanthus leaves were different; in Comparative Example 3, different strains were used to prepare the sunscreen enhancer, and the sun protection index also decreased significantly. This shows that the ratio of the components and the use of the sunscreen enhancer have a great influence on the sunscreen performance of the sunscreen spray.
[0139] 4. Determination of general water resistance of sunscreen cosmetics:
[0140] The inspection was carried out in accordance with the specific requirements of the "Technical Specification for Safety of Cosmetics" (2015 edition). A xenon arc lamp of a daylight simulator was used, and all performance indicators met the requirements of the measurement specifications. A total of 9 subjects were selected from each group, including 0 males and 9 females, and divided into 9 groups, with 1 subject in each group, aged 30 to 60 years old, with an average age of 45.0±5.6 years old, which met the voluntary inclusion criteria for the subjects. Control substance: SPF value 16.1±2.4, prepared according to the standard formula of the medium and high SPF standard substance (P2) in the "Technical Specification for Safety of Cosmetics" (2015 edition). The subjects were in a prone position, and their backs were irradiated. The minimum erythema dose (MED value) of the subject's skin to ultraviolet radiation was predicted 24 hours before the test, and the ultraviolet radiation dose was adjusted according to the predicted results for the test of the object under test. On the day of the test, a spot not less than 30cm was first selected on the subject's back. 2 Normal skin area, (2.00±0.05)mg / cm 2Apply the test object or reference product evenly to the above area, wait for 15-30 minutes or proceed as required by the label instructions. The subject will have moderate activities in the water for 20 minutes, and rest for 20 minutes after getting out of the water. Then, enter the water and do moderate activities for another 20 minutes, end the water activities, and wait for the skin to dry. Then select the ultraviolet irradiation dose according to the specification requirements, and irradiate in three conditions: ① The subject's skin is not coated with the test object; ② The reference product is applied; ③ The test object is applied. Observe the experimental results after 24 hours, and record the MED values in the three conditions respectively.
[0141] Calculation method of SPF value after bathing:
[0142] The SPF value of the test article or reference article for protecting a single subject is expressed as follows:
[0143] SPFi = MED value of protected skin ÷ MED value of unprotected skin
[0144] Individual SPF values are required to be accurate to one decimal place. The arithmetic mean of the SPF values of all subjects protected by the test object after 40 minutes of bathing is calculated, and the integer part is the SPF value of the measured sample after bathing. The sampling error of the estimated mean can calculate the standard deviation and standard error of the group of data. The 95% confidence interval (95% CI) of the mean is required to not exceed 17% of the mean, otherwise the number of subjects should be increased (not more than 25) until the above requirements are met.
[0145] The results are shown in Table 4.
[0146] Table 4 SPF value after bathing
[0147] SPF value Example 1 36 Example 2 30 Comparative Example 1 21 Comparative Example 2 24 Comparative Example 3 27 Comparative Example 4 24 Comparative Example 5 25 Comparative Example 6 23 Comparative Example 7 22 Comparative Example 8 23 Comparative Example 9 25
[0148] It can be seen from Table 4 that in Comparative Example 1, the ratio of the sunscreen spray is changed, and the waterproof effect is significantly lower than that of Examples 1-2. In Comparative Example 6, the ratio of the moisturizer is different. In Comparative Example 7, the ginkgo lithospermum root extract is a commercially available product. In Comparative Example 8, the strain of bacteria used in the preparation of the ginkgo lithospermum root extract is different, and the waterproof effect is significantly lower than that of Examples 1-2.
[0149] 5. Stability test: The samples were placed in an environment of 25°C, -10°C and 45°C, and were taken out every week to observe whether there were any abnormalities. The test period was 8 weeks. After the test period, the test samples were taken out and restored to room temperature (25°C). The appearance of the test samples was observed and recorded. Samples were taken, and the same amount of material was weighed in a centrifuge tube and placed in a centrifuge. The speed was set to 2000r / min and the time was 30min. The centrifuge was started. After the test, the centrifuge tube was taken out, the appearance was observed, and recorded.
[0150] The specific details are shown in Table 5.
[0151] Table 5 Sunscreen spray stability test results
[0152]
[0153]
[0154] It can be seen from Table 5 that in Comparative Example 1, the ratio of the sunscreen spray is changed, and the overall stability decreases. In Comparative Example 2, the ratios of white frangipani flowers, white leaf immortelle flowers and white osmanthus leaves are different. In Comparative Example 3, the strains used to prepare the sunscreen enhancer are different, and the stability of the sunscreen spray under high and low temperature and variable temperature conditions decreases; in Comparative Example 4, the ratios of the emulsifiers are different, and in Comparative Example 5, the types of emulsifiers are different, and the overall stability of the sunscreen spray decreases; in Comparative Example 6, the ratios of the moisturizers are different, and the stability of the sunscreen spray under high and low temperature and variable temperature conditions decreases; in Comparative Example 7, the ginkgo lithospermum root extract is a commercially available product, and in Comparative Example 8, the strains used in the preparation of the ginkgo lithospermum root extract are different, and the stability of the sunscreen spray under high and low temperature and variable temperature conditions decreases; in Comparative Example 9, the ratios of the skin conditioners are different, and the stability of the sunscreen spray under high and low temperature and variable temperature conditions decreases.
[0155] The above is a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principles of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.
Claims
1. A fast-film-forming sunscreen spray. It is characterized in that The invention comprises the following raw materials in percentage by weight: 1-3% ethylhexyl methoxycinnamate, 1-3% diethylhexyl butyramido triazone, 2-4% sunscreen enhancer, 4-6% moisturizer, 1-2% skin conditioner, 5-6% emulsifier, 1-2% glyceryl stearate citrate, 0.8-1.4% polydimethylsiloxane, 0.03-0.06% disodium EDTA, 0.05-0.1% phenoxyethanol, 0.1-0.3% methylparaben, and the balance is water; The preparation method of the sunscreen enhancer comprises the following steps: (1) mixing white frangipani flowers, white leaf helichrysanthemum flowers and white osmanthus leaves, and crushing them to less than 100 meshes to obtain mixed fine powder; (2) Mixing the mixed micropowder and water in a weight ratio of 1:(10-15) to obtain a first mixed solution, adding composite bacteria to the first mixed solution, the composite bacteria comprising Lactobacillus acidophilus, Bifidobacterium lactis and Bifidobacterium breve, the amount of Lactobacillus acidophilus being 10 6 -10 7 CFU / mL first mixed solution; the dosage of Bifidobacterium lactis is 10 7 -10 8 CFU / mL first mixed solution; the dosage of Bifidobacterium breve is 10 8 -10 9 CFU / mL first mixed solution; ferment at 38-40°C for 6-8h, sterilize, and obtain a first fermentation solution; (3) Filtering the first fermentation broth using a 0.22-0.45 μm filter membrane, and spray-drying the filtrate to obtain a sunscreen enhancer.
2. The fast film-forming sunscreen spray according to claim 1, It is characterized in that The weight ratio of white frangipani flowers, white-leaf immortelle flowers and white osmanthus leaves is 1:(1.2-1.4):(0.6-0.8).
3. The fast film-forming sunscreen spray according to claim 1, It is characterized in that The emulsifier is selected from one or more of cetyl PEG / PPG-10 / 1 polydimethylsiloxane, glyceryl stearate citrate, and polyglyceryl-4 isostearate.
4. The fast film-forming sunscreen spray according to claim 3, It is characterized in that The emulsifier includes cetyl PEG / PPG-10 / 1 polydimethylsiloxane, glyceryl stearate citrate and polyglyceryl-4 isostearate in a weight ratio of (1.5-1.7):1:(0.2-0.4).
5. The fast film-forming sunscreen spray according to claim 1, It is characterized in that The moisturizing agent is selected from one or more of glycerol glucoside, oldenlandia diffusa extract, and ginkgo physalis root extract.
6. The fast film-forming sunscreen spray according to claim 5, It is characterized in that The moisturizing agent comprises glyceryl glucoside, oldenlandia diffusa extract and ginkgo biloba root extract in a weight ratio of (0.3-0.5):(1.4-1.6):
1.
7. The fast film-forming sunscreen spray according to claim 5, It is characterized in that The preparation method of the ginkgo lithospermum root extract comprises the following steps: (1) crushing the root of Ginkgo biloba to less than 100 meshes to obtain Ginkgo biloba root powder; (2) Mixing the root of Ginkgo biloba and water in a weight ratio of 1:(10-15) to obtain a second mixed solution; adding animal Bifidobacterium to the second mixed solution, wherein the amount of animal Bifidobacterium is 10 6 -10 7 CFU / mL second mixed solution; ferment at 38-40℃ for 3-5h, sterilize, and continue to add Lactobacillus casei, the amount of Lactobacillus casei is 10 8 -10 9 CFU / mL of the second mixed solution, ferment at 38-40℃ for 3-5h, sterilize, and finally add Lactobacillus brevis. The amount of Lactobacillus brevis is 10 7 -10 8 CFU / mL second mixed solution, ferment at 38-40°C for 2-4h, sterilize to obtain a second fermentation solution; (3) The second fermentation broth is filtered using a 0.22-0.45 μm filter membrane, and the filtrate is spray-dried to obtain a ginkgo root extract.
8. The fast film-forming sunscreen spray according to claim 1, It is characterized in that The skin conditioning agent is selected from one or more of yeast / rice fermentation product filtrate, neopentyl glycol diheptanoate, and D-panthenol.
9. The fast film-forming sunscreen spray according to claim 8, It is characterized in that The skin conditioning agent includes yeast / rice fermentation product filtrate, neopentyl glycol diheptanoate and D-panthenol in a weight ratio of (1.2-1.4):1:(0.4-0.6).
10. A method for preparing the fast film-forming sunscreen spray according to any one of claims 1 to 9, It is characterized in that The following steps are involved: (1) Add water, disodium EDTA and methylparaben to the water phase pot, stir and heat to 80-85°C until completely dissolved, keep warm for 15-20 minutes, and obtain the water phase component; (2) Add ethylhexyl methoxycinnamate, diethylhexyl butyramido triazone, emulsifier, glyceryl stearate citrate and polydimethylsiloxane into the oil phase pot, stir and heat to 80-85°C until completely dissolved, and keep warm for 15 minutes to obtain the oil phase component; (3) Mixing the aqueous phase component and the oil phase component, and homogenizing at a speed of 1800-2000 rpm for 5-10 minutes to obtain a mixed material; (4) Cooling the mixture to 40-45° C., adding the remaining components, homogenizing at a rate of 1000-1200 rpm for 5-8 minutes, cooling to room temperature, and filling to obtain the fast film-forming sunscreen spray.
