CN117064781A - Safe and mild sun-screening composition and application thereof - Google Patents
Safe and mild sun-screening composition and application thereof Download PDFInfo
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- CN117064781A CN117064781A CN202311131007.2A CN202311131007A CN117064781A CN 117064781 A CN117064781 A CN 117064781A CN 202311131007 A CN202311131007 A CN 202311131007A CN 117064781 A CN117064781 A CN 117064781A
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- Prior art keywords
- sunscreen
- sun
- screening
- oil
- water
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- 239000000203 mixture Substances 0.000 title claims abstract description 82
- 238000012216 screening Methods 0.000 title abstract description 47
- 239000000516 sunscreening agent Substances 0.000 claims abstract description 157
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- XVAMCHGMPYWHNL-UHFFFAOYSA-N bemotrizinol Chemical compound OC1=CC(OCC(CC)CCCC)=CC=C1C1=NC(C=2C=CC(OC)=CC=2)=NC(C=2C(=CC(OCC(CC)CCCC)=CC=2)O)=N1 XVAMCHGMPYWHNL-UHFFFAOYSA-N 0.000 claims abstract description 19
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- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/49—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
- A61K8/494—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with more than one nitrogen as the only hetero atom
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- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
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- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
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- A61K8/40—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
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- A61K8/49—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
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- A61Q17/04—Topical preparations for affording protection against sunlight or other radiation; Topical sun tanning preparations
Landscapes
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Abstract
The invention discloses an ethanol-free oil-in-water type safe and mild sun-screening composition and application thereof, wherein the sun-screening composition comprises the following components: bis-ethylhexyloxyphenol methoxyphenyl triazine, diethylhexylbutyrylaminotriazinone, ethylhexyl triazinone, methylenebis-benzotriazole tetramethylbutylphenol, lauroyl lysine, a lipid component comprising dibutyl adipate and butyloctanol salicylate, a lower polyol, an emulsifier, and the balance water, and the like. The sun-screening agent combination adopted by the invention does not contain physical sun-screening agent, has no heavy feel, is more fresh and cool in skin feel, is easier to smear uniformly, does not whiten, is safe and mild, does not irritate, and has high sun-screening index.
Description
Technical Field
The present invention relates to a safe and mild sunscreen composition and application thereof, and more particularly, to an ethanol-free, oil-in-water type safe and mild sunscreen composition and application thereof.
Background
In daily life, people can contact ultraviolet rays brought by sunlight every day, and a proper amount of ultraviolet rays are beneficial to human health, but skin and eyes can be damaged after long-term exposure to ultraviolet rays, skin problems such as skin relaxation and aging, skin pigmentation, long color spots and the like can be caused when sun is sunk in a daily and monthly manner, and skin inflammation, burn and even canceration can be caused seriously. Therefore, in order to maintain healthy and beautiful skin, people should take sunproof measures.
Common sun protection measures are mainly blocking or absorbing long-wave Ultraviolet (UVA) and medium-wave Ultraviolet (UVB) which are relatively harmful to human skin. In recent years, many sun-screening cosmetics have appeared on the market, and these products are added with physical sun-screening agents capable of blocking, reflecting or scattering ultraviolet rays, or chemical sun-screening agents capable of absorbing ultraviolet rays, so as to achieve the purpose of protecting skin and prevent skin from tanning, damage and aging. The existing sun-proof cosmetics comprise two systems of water-in-oil and oil-in-water, wherein the water-in-oil sun-proof cosmetics have good waterproof effect, but have thick and greasy skin feel and smoldering skin feel. The oil-in-water type sun-proof cosmetic has light and comfortable skin feel, is easy to push away paste, has better use feel, and is easy to clean after use.
Sunscreen cosmetics may represent the ability to protect against UVA and UVB with PA and SPF, respectively. The protection capability of the PA is usually indicated by "+", with more "+" indicating a longer protection time. SPF is represented by an index, and the protection capability (such as SPF15, SPF 30, SPF 50 and the like) of the SPF15 is shown, the sun-screening cosmetic can filter more than 90% of ultraviolet rays, and the larger the SPF value is, the stronger the sun-screening cream has the UVB protection capability and the longer the sun-screening time is.
At present, most of the sun-screening cosmetics on the market are chemical sun-screening agents and physical sun-screening agents combined to improve sun-screening effect. Common physical sunscreens are titanium dioxide and zinc oxide, but the addition of the physical sunscreens can lead to thick and heavy skin feel of the product, and the skin is whitened and pseudo-whitened after use, and is not easy to be uniformly smeared. In addition, the cleansing agent needs to be cleaned fully after use, otherwise, physical sunscreens may remain on the skin, causing skin problems such as pore blocking, acne growth, and closed mouth growth. The chemical sunscreen agent has strong ultraviolet absorption effect and wider protective range, and can convert the absorbed ultraviolet radiation into infrared radiation or heat energy, so most of sunscreen cosmetics can be added with the chemical sunscreen agent.
To solve various problems occurring in the current commercial sunscreen cosmetics, those skilled in the relevant art are constantly making various attempts and developing new product systems. For example:
chinese patent application 201711298204.8 discloses a sun-screening whitening skin care composition and a preparation method thereof, the sun-screening whitening skin care composition comprising: sunscreens, emollients, conditioning agents, moisturizers, antioxidants and functional adjuvants, the sunscreens used include titanium dioxide, ethylhexyl methoxycinnamate, ethylhexyl salicylate, ethylhexyl triazone, octocrylene, benzophenone-3 and hexyl diethylaminohydroxybenzoate. The sun-screening agent comprises a chemical sun-screening agent and a physical sun-screening agent titanium dioxide, and the whitening characteristic of the physical sun-screening agent is utilized to prepare the sun-screening and whitening skin-care composition, however, the acceptance of the sun-screening and whitening skin-care composition to the market is not high, firstly, the skin feel is thick when the sun-screening agent is used, and secondly, the sun-screening and whitening skin-care composition is required to be cleaned and removed after the sun-screening agent is used. The applicant has abandoned this application.
Chinese patent 201911275282.5 discloses a blue light and infrared resistant sunscreen composition comprising: 1 part of butterflybush flower extract, 4 parts of needle-shaped titanium dioxide with the particle size of 1-100 mu m, polysiloxane-151 parts, 2.5 parts of PEG-10 polydimethylsiloxane, 1.5 parts of cetyl PEG/PPG-10/1 polydimethylsiloxane, 3 parts of octyl polymethylsiloxane, 10 parts of cyclopentadimethicone and C 12-15 Alcohol benzoate 7 parts, isononyl isononanoate 3 parts, disteardimonium hectorite 0.8 parts, ethylhexyl methoxycinnamate 6 parts, octocrylene 3 parts, butyl methoxy dibenzoylmethane 2 parts, bis-ethylhexyl oxyphenol methoxyphenyl triazine 3 parts, nano titanium dioxide 8 parts, nano zinc oxide 6 parts, glycerin 5 parts, butanediol 3 parts, betaine 1 part, sodium chloride 0.6 parts, phenoxyEthanol 0.5 parts, ethylhexyl glycerol 0.1 parts, and 1, 2-pentanediol 1.5 parts. The formulation is also very skin-friendly.
Chinese patent application 202110556384.5 discloses a water-in-oil cosmetic composition comprising a skin active ingredient selected from ethylhexyl methoxycinnamate, homosalate, hexyl diethyltoluoylbenzoate, octocrylene, ethylhexyl triazone, bis-ethylhexyl oxyphenoxyphenyl triazine, polysiloxane-15, terphenyl triazine, ethylhexyl salicylate, benzophenone-3, avobenzone (butylmethoxydibenzoylmethane), phenylbenzimidazole sulfonic acid, isopentyl p-methoxycinnamate, methylenebis-benzotriazole tetramethylbutylphenol, diethylhexylbutyrylaminotriazone, p-xylylene dicarbamate, cresol, gallol trioleate, 4-methylbenzylidene camphor, menthol anthranilate, benzophenone-4, benzophenone-8, cinossalate, dimethyl panacil ethylhexyl ester, titanium dioxide, zinc oxide, diphenyl benzoquinone, sodium bis-benzoquinone, and water-soluble derivatives of vitamin a, water-soluble vitamin α -soluble derivative of vitamin a, and physiologically active ingredients of vitamin a, including water-soluble α -and water-soluble derivative of vitamin a. However, most consumers prefer the skin feel of oil-in-water products over water-in-oil sunscreen products.
Chinese patent application 202180054228.7 discloses a sunscreen or daily care composition comprising: (i) an ultraviolet absorber water dispersion composition comprising: (a) Micronized methylenebis-benzotriazolyltetramethylbutylphenol and (b) at least one polyglycerol monoalkyl ester; and (ii) at least one oil soluble UVA filter which is a combination of diethylamino hydroxybenzoyl hexyl benzoate and butyl methoxydibenzoyl methane. According to this application, it may further comprise at least one additional UV filter selected from the group consisting of water-soluble UVA filters, UVB filters and/or broadband filters, preferably: disodium phenylbisbenzimidazole tetrasulfonate is used as a water-soluble UVA filter, ethylhexyl triazone, diethylhexyl butyryl triazone, phenylbenzimidazole sulfonic acid, and combinations thereof are used as UVB filters, bis-ethylhexyl oxyphenol methoxyphenyl triazine, 2- (2H-benzotriazol-2-yl) -6- [ (2-ethylhexyl oxy) methyl ] -4-methylphenol, cresol trazotrisiloxane, and combinations thereof are used as broadband filters.
Chinese patent 202110797954.X discloses a pickering child sun block comprising: 2-10 parts of Pickering stabilizer; 5-20 parts of a sun-screening agent; 5-20 parts of dibutyl adipate; 2-5 parts of polydimethylsiloxane; 0.1 to 1 part of wood oil with flat core; 5-20 parts of humectant; 1-5 parts of purslane extracting solution; 0.05-2 parts of thickener; 0.2 to 0.5 part of p-hydroxyacetophenone; 0-1 part of arginine; wherein the sun-screening agent comprises a water-soluble sun-screening agent and an oil-soluble sun-screening agent; the Pickering stabilizer is prepared by mixing octenyl aluminum succinate modified starch and silica or mixing octenyl aluminum succinate modified starch, silica and beta-cyclodextrin. The pickering system requires a large amount of porous powder.
Chinese patent application 202110857415.0 discloses a sunscreen cosmetic composition comprising hyaluronic acid and/or hyaluronate, wherein the sunscreen agent may be one or more of water-soluble sunscreen agent and oil-soluble sunscreen agent; the water-soluble sunscreen agent is selected from one or more of benzophenone-4, benzophenone-5, benzylidene camphorsulfonic acid and its salts, camphorbenzalkonium methylsulfate, disodium phenyldibenzimidazole tetrasulfonate, phenylbenzimidazole sulfonic acid, potassium, sodium and triethanolamine salts, terephthalylidene camphorsulfonic acid and its salts; the oil soluble sunscreen agent is selected from one or more of 3-benzylidene camphor, 4-methylbenzylidene camphor, benzophenone-3, bis-ethylhexyloxyphenol methoxyphenyl triazine, butyl methoxydibenzoylmethane, diethylaminobenzoyl hexyl benzoate, diethylhexyl butyryl triazinone, cresol trazotrisiloxane, dimethyl PBPA ethylhexyl ester, ethylhexyl methoxycinnamate, ethylhexyl salicylate, ethylhexyl triazinone, homosalate, isoamyl p-methoxycinnamate, methylenebis-benzotriazole tetramethylbutyl phenol, octocrylene, PEG-25 para-aminobenzoic acid, polyacrylamide methylbenzylidene camphor, polysiloxane-15, titanium dioxide and zinc oxide.
To obtain a good sunscreen product, at least the following problems are solved: (1) Problems with whole product systems, such as water-in-oil systems, oil-in-water systems, or powder dispersions, of course, average consumers generally prefer the skin feel of oil-in-water systems with equal protection capabilities; (2) Screening and collocation of sunscreens requires consideration of various problems, such as problems of each of physical sunscreens and chemical sunscreens, stability problems of sunscreens, skin feel problems of sunscreens, transdermal absorption problems of sunscreens, toxicity and decomposition toxicity problems of sunscreens themselves, collocation problems, and synergy problems.
For example, in the aforementioned patent application 202180054228.7, the UVA filter used is a diethylamino hydroxybenzoyl hexyl benzoate which is thermally unstable and may decompose at relatively low temperatures, and which is susceptible to thermally decomposition to form highly reactive free radicals, thereby having a strong oxidizing effect. Thus, the diethylamino hydroxybenzoyl hexyl benzoate EWG yellow standard has a lower component safety score (3 points), and is not approved for use by the FDA in the united states; the light stability of the used butyl methoxy dibenzoyl methane is not high, and the butyl methoxy dibenzoyl methane can be gradually decomposed after being irradiated by ultraviolet rays, so that the sun-screening effect is gradually lost; the component has certain toxicity, and can easily generate active chlorine for promoting oxidation when meeting sunlight, and the active chlorine is harmful to human body. Many consumers react to this ingredient to easily stain clothing and fumigate eyes.
As another example, although a number of sunscreens are exemplified in the aforementioned patent application 202110857415.0, the sunscreens used in all of the examples are diethylamino hydroxybenzoyl hexyl benzoate + ethylhexyl methoxycinnamate + physical sunscreens, the problem of diethylamino hydroxybenzoyl hexyl benzoate has been discussed previously, ethylhexyl methoxycinnamate (C 18 H 26 O 3 ) Although otherwise relatively desirable, the molecular weight is less than 300 and the risk of percutaneous absorption is relatively high.
The pickering stabilizers in the foregoing patent 202110797954.X are colloidal particles, a large amount of colloidal particles may cause the product to rub mud, the use feel is poor, the sun-protection effect is reduced, and the colloidal particles have problems in biocompatibility, biodegradability, source sustainability and the like, so that the pickering stabilizers are limited in application in sun-protection products, and cannot meet the demands of consumers on low-cost, natural environment-friendly and safe sun-protection products.
In addition, the water-soluble sunscreen disodium phenylbisbenzimidazole tetrasulphonate mentioned in the aforementioned patent applications 202180054228.7 and 202110857415.0 and in the aforementioned patent 202110797954.X is fluorescent and may cause skin allergy symptoms in infants and skin-sensitive persons, and sensitive muscles and infants should be avoided.
At present, a plurality of traditional organic sunscreens with small molecules are added into a sun-proof product, and the traditional organic sunscreens have certain transdermal absorbability and can cause skin irritation, allergy and other problems.
With the development of cosmetic products, consumers are increasingly focusing on the mildness of the products, however, there are few mild sunscreen cosmetics suitable for sensitive skin on the market at present, and therefore, there is a need to develop a safe and mild sunscreen cosmetic.
Therefore, proper sunscreens and combinations are selected to prepare safe and mild sunscreens cosmetics.
Disclosure of Invention
The object of the present invention is to provide a novel ethanol-free, oil-in-water, safe and mild sunscreen composition which is free of physical sunscreens, chemical sunscreens of small molecules and irritant sunscreens.
In one aspect, to achieve the above object of the present invention, the present invention provides an ethanol-free, oil-in-water, safe and mild sunscreen composition, wherein the sunscreen composition comprises the following components in weight percent:
1-8% of oil-soluble broad-spectrum ultraviolet absorbent bis-ethylhexyloxyphenol methoxyphenyl triazine;
2-10% of the UVB absorber diethylhexyl butyramidotriazinone;
0.5-5% of an oil soluble UVB absorber ethylhexyl triazone;
2-10% of a broad-spectrum ultraviolet absorber methylene bis-benzotriazole tetramethylbutylphenol dispersion;
0.2-4% lauroyl lysine, which primarily serves to improve the dispersibility and adhesion of the sunscreen;
5-16% of more than one lower polyol which mainly plays a role in moisture retention;
15-40% of grease component which not only plays a role of a solvent of a sun-screening agent, but also plays a role of moisturizing skin;
1.6-8% of emulsifying agent which mainly plays a role in emulsification; and
the balance of water.
In the sun-screening composition system, the formula does not contain alcohol with great irritation and traditional preservative, does not contain controversial chemical sun-screening agent, does not contain physical sun-screening agent, does not cause skin whitening, and does not need makeup removal after use. In addition, the sun-proof composition can adopt an oil-in-water type emulsification technology, is light and thin in skin feel, is easy to apply uniformly, is not greasy when applied, is not sticky when sweated, and can meet the requirements of consumers on the skin feel.
In the sun-screening composition system, the combination of sun-screening agents adopts macromolecular chemical sun-screening agents (the molecular weight is at least more than 500), has better safety and mildness, can not permeate into skin and be absorbed by the skin, has high light stability and lasting effect, realizes efficient sun-screening, reduces the irritation of the sun-screening composition, is suitable for sensitive skin, and solves the problems of the existing sun-screening cosmetics.
In the sun-screening composition system, in order to improve sun-screening capability, safety, mildness and freshness, bis-ethylhexyl oxyphenol methoxyphenyl triazine, diethyl hexyl butyryl amino triazinone, ethylhexyl triazinone and methylene bis-benzotriazole tetramethyl butyl phenol are carefully selected as the compounded core sun-screening agent, and the sun-screening composition system can be prepared into mild oil-in-water type sun-screening cosmetics, has good high-low temperature stability, and has more fresh skin feel and is easier to apply uniformly compared with water-in-oil type sun-screening cosmetics. Wherein:
the bis-ethylhexyloxyphenol methoxyphenyl triazine is a high-efficiency oil-soluble broad-spectrum ultraviolet absorber with the absorption wavelength between 290 and 370nm, and can provide broad-spectrum UVA and UVB absorption. The sunscreen component has English INCI name of Bis-ethylhexyloxyphenol methoxy phenyl triazine, CAS number of 187393-00-6, and chemical formula of C 38 H 49 N 3 O 5 The molecular weight is 627.81, and the structural formula is shown in the following formula I:
the double-ethyl hexoxyphenol methoxyphenyl triazine has high safety (low toxicity) and high light stability, can be protected for a long time, and can improve the SPF value. It can also enhance the photostability of other sunscreens, act as stabilizers for other chemical sunscreens, have strong compatibility with other chemical sunscreens, and have excellent synergism.
Diethyl hexyl butyramide triazinone is a novel high-efficiency ultraviolet filter, is a UVB absorber, has the English INCI name Diethylhexyl butamido triazone, the CAS number of 154702-15-5 and the chemical formula of C 44 H 59 N 7 O 5 The molecular weight is 765.98, and the structural formula is shown in the following formula II:
the diethylhexyl butyramide triazinone is an alcohol-soluble and oil-soluble component, has strong light absorption, good light stability, can provide high SPF index, and has good solubility in various common grease for cosmetics, low toxicity and high safety.
Ethylhexyl triazone is a high-efficiency light-stable oil-soluble UVB absorbent with effective absorption wavelength of 290-320nm, english INCI name of Ethylhexyl triazone, CAS number of 88122-99-0, and chemical formula of C 48 H 66 N 6 O 6 The molecular weight is 823.07, and the structural formula is shown in the following formula III:
ethylhexyl triazone is almost non-toxic. The oil-soluble absorbent has no irritation to eyes and skin, no sensitization, and is called as the oil-soluble absorbent with the strongest UVB absorbing capacity, and has strong light stability and water resistance. Due to its natural polarity, it has a good affinity for the keratin of the skin, so that excellent anti-washing effects can be achieved when used in sunscreen products. The ultraviolet light-absorbing composite material has a large molecular structure and high ultraviolet light absorption efficiency, has a broad-spectrum sun-screening effect, can not only prevent ultraviolet light in a UVB section, but also prevent ultraviolet light in a UVA section, and can improve the SPF value by being compounded with other broad-spectrum sun-screening agents.
The Methylene bis-benzotriazole tetramethyl butyl phenol can be dispersed in water to form nanoscale organic particles, and has a unique ultraviolet absorbent with high light absorption value in the near visible light band, the English INCI name is methyl bis-benzotriazolyl tetramethylbutylphenol, the CAS number is 103597-45-1, and the chemical formula is C 41 H 50 N 6 O 2 The molecular weight is 658.86, and the structural formula is shown in the following formula IV:
the methylene bis-benzotriazole tetramethyl butyl phenol has low toxicity, does not irritate eyes and skin, and has no sensitization effect. The sunscreen component exhibits the widest ultraviolet absorption range, has a higher extinction coefficient for both UVA and UVB, provides strong UVA-band absorption, and increases the UVA-PF sun protection index. It can play a triple role: the inherent light-stable organic molecules play a role in ultraviolet absorption, the superfine structure brings about the effects of dispersing and reflecting light, and the synergistic effect can be provided by compounding the light-stable organic molecules with other oil-soluble sunscreens.
The inventors of the present invention found through comparative experiments that the above four sunscreen components were compounded to have the best effect of preventing ultraviolet radiation (see the following embodiments for details).
The sun-screening composition of the invention adopts macromolecular chemical sun-screening agents, and the molecular weight of the sun-screening composition is as low as 600, so the sun-screening composition has better safety and mildness, can not permeate into skin and be absorbed by skin, has high light stability and lasting effect, realizes efficient sun screening, reduces the irritation of the sun-screening composition and is suitable for sensitive skin.
In order to solve the defect of poor waterproof and sweat-proof effects of the pure sunscreen cream, the organic powder lauroyl lysine of an amino acid source is added into the formula to improve the skin adhesion, improve the dispersibility and the adhesion of a chemical sunscreen agent, and in addition, the chemical sunscreen agent ethylhexyl triazone with good water resistance is added to further improve the sweat-proof and waterproof effects.
In fact, in the present invention, lauroyl lysine is also a skin conditioner, which is an amino acid derivative, is prepared from natural coconut oil fatty acid, has excellent lubricity, softness and extensibility, and can provide excellent skin feel. It has certain hydrophobicity and can raise the sweat-preventing and water-proof effect of the sun-proof cosmetics.
Preferably, in the sunscreen composition system of the present invention, the grease component employed comprises at least one ester component and at least one silicone oil component. The silicone oil component may be one or more selected from the group consisting of: polydimethylsiloxane, octyl polymethylsiloxane, phenyl polytrimethylsiloxane, diphenylsiloxyphenyl polytrimethylsiloxane, and cyclic polymethylsiloxane. The silicone may further provide a soft skin feel to the sunscreen composition.
Preferably, in the sunscreen composition system of the present invention, the grease component employed comprises at least dibutyl adipate and butyl octanol salicylate. Dibutyl adipate and butyl octanol salicylate are used as solvents of the sun-screening agent, and have good solubility on the sun-screening agent, so that the sun-screening composition can stably exist at high temperature (45 ℃) and low temperature (-16 ℃) and cannot be separated out. And the two grease components are light and thin in skin feel and have no greasy feel.
More preferably, in the sunscreen composition system of the present invention, the sunscreen composition comprises, in weight percent, 8-15% dibutyl adipate and 9-20% butyl octanol salicylate; further preferably, the sunscreen composition comprises dibutyl adipate and butyl octanol salicylate in a total amount of 21 to 35%, more preferably 22 to 29% by weight of the composition.
Preferably, in the sunscreen composition of the present invention, the methylene bis-benzotriazole-based tetramethylbutylphenol dispersion employed is a water-dispersed nano-sized organic particle formed by using decyl glucoside as a dispersant.
Unlike CN 202180054228.7, which uses polyglycerol monoalkyl ester as dispersant to disperse methylenebis-benzotriazole-tetramethylbutylphenol, decyl glucoside is used as dispersant in the present invention, and decyl glucoside is cheap and mild, has good compatibility and dissolution ability with other compounds, and contributes to long-term stability and uniformity of the system.
In addition, the surfactant system of the present invention employs emulsifiers of 100% natural source index, sodium stearyl glutamate, cetostearyl alcohol, cetostearyl glucoside. Sodium stearoyl glutamate is a powerful emulsifier with high safety, is suitable for various different types of products, and has excellent compatibility with inorganic and organic sunscreens.
In the sunscreen composition system of the present invention, the lower polyol that mainly plays a role in moisture retention is one or more selected from the group consisting of: glycerol, 1, 3-butanediol, 1, 2-hexanediol, 1, 3-propanediol and ethylhexyl glycerol.
In the sun-screening composition system, glycyrrhetinic acid stearate can be used as a soothing and repairing component, has the effects of resisting inflammation, soothing allergy, whitening skin, repairing damage after sun, and relieving skin irritation, can reduce skin redness, and further improves the mildness of the formula. In addition, the allantoin also has anti-inflammatory effect, can reduce irritation and protect skin, reduce damage to the skin caused by the environment, and ensure the mildness of the sun-screening product.
The formulations disclosed above may be used as base formulations for the sunscreen compositions of the present invention, which may further comprise components commonly used in cosmetics, particularly in sunscreen cosmetics, such as antioxidants, pH adjusters, chelating agents, thickeners, and the like, but excluding some more irritating components such as alcohols, conventional preservatives, disputed chemical sunscreens, and the like.
In summary, in the sunscreen composition system designed by the invention, bis-ethylhexyl oxyphenol methoxyphenyl triazine, diethyl hexyl butyryl amino triazone, ethylhexyl triazone and methylene bis-benzotriazole tetramethyl butyl phenol are adopted as core sunscreens, dibutyl adipate and butyl octanol salicylate are adopted as oil-soluble solvents, and thickeners, skin conditioning agents, emulsifying agents and the like are selected to be used on the basis, so that the ethanol-free, safe and mild sunscreen cosmetic which can be prepared by adopting the oil-in-water emulsification technology is built.
As a specific embodiment of the present invention, in the sunscreen composition of the present invention, it comprises the following components in weight percent:
1.2-6% of bis-ethylhexyloxyphenol methoxyphenyl triazine;
4-8% of diethylhexyl butyramidotriazinone;
0.8-3% ethylhexyl triazone;
4.5-9% methylene bis-benzotriazolyl tetramethylbutylphenol dispersion;
0.5-3.5% lauroyl lysine;
7-13% lower polyol;
21-35% of a fat component;
2-7% of an emulsifier;
and the balance water.
As another embodiment of the present invention, in the sunscreen composition of the present invention, it comprises the following components in weight percent:
1.5-4% of bis-ethylhexyloxyphenol methoxyphenyl triazine;
5-7.5% diethylhexyl butyramidotriazinone;
1.0-2.5% ethylhexyl triazone;
6-9% methylene bis-benzotriazolyl tetramethylbutylphenol dispersion;
1.0-3.0% lauroyl lysine;
8-12% lower polyol;
21-30% of a fat component;
3-6% of an emulsifier;
and the balance water.
As a further embodiment of the sunscreen composition of the present invention, the formulation is shown in Table 1:
TABLE 1
In another aspect, the present invention provides the use of the above-described sunscreen composition for the preparation of an oil-in-water type sunscreen cosmetic. The oil-in-water type sunscreen cosmetic can be sunscreen emulsion, sunscreen cream, sunscreen spray, sunscreen gel or sunscreen lotion.
In a further aspect, to achieve the object of the present invention, the present invention also provides a process for preparing the above-mentioned sunscreen composition, which comprises the steps of:
1) Adding the group A raw materials into an emulsifying pot, heating to 80-85 ℃, starting stirring and homogenizing for 5-20 minutes until the materials are completely dissolved;
2) Adding the raw materials of the group B into an oil phase pot, heating to 80-85 ℃, and stirring until the raw materials are completely dissolved;
3) When the temperature of the emulsifying pot is 80-85 ℃, adding the raw materials in the oil phase pot into the emulsifying pot, and simultaneously starting stirring and homogenizing for 5-20 minutes until the raw materials are completely uniform;
4) When the temperature of the emulsifying pot is reduced to 60-65 ℃, adding the aqueous solution of the raw materials of the group C, and stirring until uniform;
5) Dispersing part of water and methylene bis-benzotriazole tetramethylbutyl phenol dispersion liquid uniformly in advance, then adding the mixture into an emulsifying pot, adding ethylhexyl glycerol into the emulsifying pot, and stirring until uniform;
6) Filtering and discharging by using a 200-mesh filter screen.
In the above method, the specific temperature, the specific stirring speed, the time, etc. may be specifically determined according to the actual situation.
Compared with the existing sun-screening composition, the sun-screening composition has the following beneficial effects:
1) The invention adopts safe and mild sun-screening agent combination, does not contain physical sun-screening agent, has no heavy feel, and can efficiently screen sun;
2) The sun-proof composition can be prepared into an oil-in-water sun-proof product, and compared with the water-in-oil sun-proof product, the sun-proof composition has more fresh skin feel and is easier to smear uniformly;
3) Dibutyl adipate and butyl octanol salicylate are used as oil-soluble solvents of the sun-screening agent, so that the sun-screening agent is stable at high and low temperatures and is not greasy;
4) Lauroyl lysine is adopted and is matched with ethylhexyl triazinone with strong water resistance, so that the sweat-proof and waterproof effects are good;
5) The formula system is suitable for consumers with sensitive skin;
6) The formula system disclosed by the invention is light and thin in skin feel, easy to paint and push away, free from whitening, safe, mild, free from irritation and high in sun protection index.
The present invention will be further described with reference to the following specific embodiments, which are merely illustrative of certain specific embodiments of the invention and are not intended to limit the invention.
Detailed Description
Example 1 and comparative examples 1-9: preparation of sunscreen cosmetic
Table 2 below shows the formulations of example 1 and comparative examples 1-4 (for evaluation of product stability and safety) and Table 3 shows the formulations of example 1 and comparative examples 5-9 (for evaluation of product UV protection).
The sunscreen cosmetics of example 1 and comparative examples 1 to 9 of the present invention were prepared according to the formulation ratios shown in the following tables 2 and 3 by the following preparation methods, to obtain the sunscreen cosmetics of example 1 of the present invention and the sunscreen cosmetics of comparative examples 1 to 9:
1) Adding the group A raw materials into an emulsifying pot, heating to 80-85 ℃, starting stirring and homogenizing for 5-20 minutes until the materials are completely dissolved;
2) Adding the raw materials of the group B into an oil phase pot, heating to 80-85 ℃, and stirring until the raw materials are completely dissolved;
3) When the temperature of the emulsifying pot is 80-85 ℃, adding the raw materials in the oil phase pot into the emulsifying pot, and simultaneously starting stirring and homogenizing for 5-20 minutes until the raw materials are completely uniform;
4) When the temperature of the emulsifying pot is reduced to 60-65 ℃, adding the aqueous solution of the raw materials of the group C, and stirring until uniform;
5) Dispersing part of water and methylene bis-benzotriazole tetramethylbutyl phenol dispersion liquid uniformly in advance, adding the mixture into an emulsifying pot, adding ethylhexyl glycerol into the emulsifying pot, and stirring until the mixture is uniform;
6) Filtering and discharging by using a 200-mesh filter screen.
TABLE 2
The methylene bis-benzotriazole tetramethylbutylphenol used in Table 2 was a dispersion thereof, and the effective amount of the methylene bis-benzotriazole tetramethylbutylphenol was about 3%.
TABLE 3 Table 3
Test evaluation experiment of the products of example 1 and comparative examples 1 to 9
1. Product appearance and physicochemical index
Appearance: white emulsion
Heat resistance (45.+ -. 2 ℃ C.). 3 months, restoring the room temperature without abnormality;
cold-resistant (-16±2 ℃). 3 months, restoring the room temperature without abnormality;
2. stability assessment:
example 1 and comparative examples 1 to 4 were each stored at-16℃at 25℃and 45℃for 3 months and at 50℃for 1 month. The appearance of the material after 1 day, after 1 month, and after 3 months was observed, and the observation results are shown in Table 4.
TABLE 4 stability test of example 1 and comparative examples 1-4
As can be seen from table 4, example 1 and comparative examples 3 and 4 have good stability; comparative examples 1-2 show that dibutyl adipate and butyl octanol salicylate determine the solubility of the sunscreen, and that a reduction in the amount of these two oils results in precipitation of the sunscreen at low temperatures, indicating that the amount of these two oils in example 1 is the preferred amount to ensure product stability.
3. Product safety evaluation
Cosmetic irritation evaluation was performed on the sunscreen cream formulations of example 1 and comparative examples 1 to 4.
The group of subjects was females, 30, between 18 and 60 years of age. The skin of the subject is healthy, the history of skin diseases and allergies is avoided, and the habit of using sun-screening cosmetics in the mean time accords with the volunteer selection standard of the subject. Randomly, 5 groups of 6 persons each.
The test method is a human body patch test. Selecting qualified patch tester, placing about 0.020-0.025g of test object into the patch tester, applying the patch tester with test object on the back or forearm flexor side of the subject with non-irritating adhesive tape, and applying on skin with palm light pressure for 24 hr. After removing the spot tester for 30min, the skin reaction is observed after the indentation disappears. If the result is negative, the spot test is observed again 24h and 48h after the spot test. The results were recorded according to 2007 "cosmetic health Specification" and 2015 "cosmetic safety Specification" as reference standards.
Evaluation criteria: level 0: a negative reaction; stage 1: suspicious reactions, only weak erythema; 2 stages: weak positive response, erythema, infiltration, edema, and possibly papules; 3 stages: strong positive reaction, erythema, infiltration, edema, papule, and reaction beyond the test area; 4 stages: very strong positive response, marked erythema, severe infiltration, edema, blepharospermia, and response beyond the test area.
The human skin patch experiment result shows that: each group of subjects observed the skin reactions of the subjects 24h and 48h after the test by the patch experiments of the sun protection emulsions (creams) of example 1 and comparative examples 1 to 4, and all subjects were negative in skin reactions, which indicated that the sun protection emulsions (creams) prepared by the present invention were safe.
4. In vitro UV value test:
4.1, test instrument: the FilmQAPro software performs in vitro SPF/PA value testing.
4.2, test information:
TABLE 5
4.3, test sample information:
a sun block (cream) formulation was set up as a test sample using the core sun block composition, see table 3.
4.4, test methods/materials and System introduction:
the testing method comprises the following steps: samples (example 1 and comparative examples 5-9) were smeared on Gafchromic film and placed in an irradiation box simulating sunlight for irradiation. The charge number in the film measures the performance change of the material after being irradiated by rays, and then the irradiated film is analyzed and processed by film QAPro software under a standard curve.
Gafchromic film: similar to skin tissue equivalence, medical grade is accurate, average effective nuclear charge number zeff=6.8, human skin zeff=7.4. The change in performance of the material after radiation exposure is measured by the number of charges in the film and analyzed by the system. The film is classified into two types, HD-V2 (for testing SPF values) and EBT-3 (for testing PA values).
Standard graph: under the UVA/UVB standard curve, sample sun protection value analysis is carried out, and a software analysis value 'Raverage' is read, wherein the corresponding optical density value < cGy > is recorded, and the value is the optical density value of the sample after irradiation.
4.5, test results: please refer to table 6:
TABLE 6
| SPF value | PA value | |
| Example 1 | 63.8 | +++ |
| Comparative example 5 | 13 | Without any means for |
| Comparative example 6 | 56.5 | +++ |
| Comparative example 7 | 35.8 | ++ |
| Comparative example 8 | 43.5 | +++ |
| Comparative example 9 | 58.5 | +++ |
From table 6 above, comparative example 5, in which only two UVB absorbers (diethylhexylbutyrylaminotriazinone+ethylhexyl triazinone) were added, the SPF and PA values were greatly reduced, demonstrating that the good sunscreen effect was achieved by the combination of UVA filtering effect sunscreens bis-ethylhexyloxyphenol methoxyphenyl triazine and methylenebis-benzotriazole tetramethyl butylphenol, which were able to provide PA values; comparative example 6 does not add bis-ethylhexyloxyphenol methoxyphenyl triazine but increases the content of methylenebis-benzotriazole-tetramethylbutylphenol, the SPF value is still lower than example 1, demonstrating that the addition of the sunscreen agent effectively increases the SPF value; comparative example 7 does not add methylenebis-benzotriazole-tetramethylbutylphenol, but increases the content of bis-ethylhexyloxyphenol methoxyphenyl triazine, the SPF value is much lower than that of example 1, and the PA value is also lowered, indicating that methylenebis-benzotriazole-tetramethylbutylphenol has a large contribution to the increase of the SPF value and the PA value; comparative example 8 without added diethylhexyl butyrylaminotriazinone, increased ethylhexyl triazinone content, lower SPF values than example 1, demonstrated that diethylhexyl butyrylaminotriazinone contributed significantly to the SPF values; comparative example 9 does not add ethylhexyl triazone, improves the content of diethyl hexyl butyryl triazone, and compared with example 1, the SPF value is reduced, but the cost is greatly increased, and the increase of the total content of the sun-screening agent also causes the skin feel to be greasy and thick.
In summary, the compound combination of the sun-screening agent provided by the invention can effectively improve sun-screening effect, and each sun-screening agent component is critical to sun-screening value, which is indispensable.
5. Human trial evaluation:
the sunscreen cream (cream) and the commercial sunscreen cream 1 of example 1 and comparative examples 1 to 4, 6 and 9 were applied to the faces of 12 volunteer panelists 18 to 60 years old, and the respective skin feel frivolous, mild, easy-to-wash, easy-to-smear were evaluated.
The specific method comprises the following steps: samples of 8 products were distributed to 12 volunteers, each for 3 days, and sensory evaluation was performed before and after each product use. The experience is best in 5 minutes, the experience is worst in 4 minutes, and any value can be taken between 1 and 5 minutes in 1 minute. The evaluation results are shown in Table 7.
TABLE 7
| Experience feel | Light and thin feeling | Mildness of | Difficulty in cleaning | Degree of easy application |
| Example 1 | 4.5 | 4.7 | 4.7 | 4.8 |
| Comparative example 1 | 4.6 | 4.5 | 4.6 | 4.5 |
| Comparative example 2 | 4.6 | 4.6 | 4.7 | 4.5 |
| Comparative example3 | 4.6 | 4.7 | 4.8 | 4.1 |
| Comparative example 4 | 4.5 | 4.4 | 4.7 | 4.8 |
| Comparative example 6 | 4.5 | 4.4 | 4.3 | 4.3 |
| Comparative example 9 | 3.8 | 4.0 | 3.7 | 4.2 |
| Commercial sun cream 1 | 4.3 | 4.5 | 4.6 | 4.5 |
Remarks: no experience test was performed due to the poor sun protection effect of comparative examples 5, 7 and 8
As can be seen from table 7 above, compared with the commercial sun cream 1 and example 1, the sun cream (cream) of the present invention has lighter and thinner skin feel, better mildness, easy cleaning, easy pushing away and even application; although the reduction of the amount of dibutyl adipate and butyl octanol salicylate used can improve the frivolity of skin feel, the low-temperature stability of comparative examples 1-2 is reduced; the easy smearing degree of the comparative example 3 is reduced, which shows that lauroyl lysine is helpful for improving the spreadability of the product and has important influence on skin feel; the mildness of comparative example 4 decreased, indicating that the addition of glycyrrhetinic stearate helps to promote mildness of the sun protection milk (cream); comparative example 6 has reduced mildness and ease of cleaning and ease of application, which indicates that bis-ethylhexyloxyphenol methoxyphenyl triazine has milder properties by itself, and that methylenebis-benzotriazole tetramethylbutylphenol is a nanoscale organic particle, and the increase in the content of the organic particle possibly affects the ease of cleaning and ease of application, and at this time, the skin feel can be improved by adjusting the emulsifier and the grease in the formulation; comparative example 9 had a poor feel because the total content of the sunscreens was increased by 2% as compared with example 1, and a large increase in the sunscreens resulted in poor skin feel and increased irritation.
In summary, the optimal proportion of the sun-screening composition provided by the invention can provide better skin feel and mildness, and the sun-screening emulsion (cream) preparation built by adopting the sun-screening composition can bring good sun-screening effect and skin feel, and meets the requirements of consumers on sun-screening products.
Examples 2 to 6: preparation of sunscreen cosmetic
The sunscreen cosmetics of examples 2 to 6 of the present invention were prepared by the same preparation method as in example 1 and comparative examples 1 to 9, and the formulations of examples 2 to 6 are shown in Table 8 below:
TABLE 8
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Claims (10)
1. An ethanol-free, oil-in-water, safe and mild sunscreen composition, wherein the sunscreen composition comprises the following components in weight percent:
1-8% of oil-soluble broad-spectrum ultraviolet absorbent bis-ethylhexyloxyphenol methoxyphenyl triazine;
2-10% of the UVB absorber diethylhexyl butyramidotriazinone;
0.5-5% of an oil soluble UVB absorber ethylhexyl triazone;
2-10% of a broad-spectrum ultraviolet absorber methylene bis-benzotriazole tetramethylbutylphenol dispersion;
0.2-4% lauroyl lysine, which primarily serves to improve the dispersibility and adhesion of the sunscreen;
5-16% of more than one lower polyol which mainly plays a role in moisture retention;
15-40% of grease component which not only plays a role of a solvent of a sun-screening agent, but also plays a role of moisturizing skin;
1.6-8% of emulsifying agent which mainly plays a role in emulsification; and
the balance of water.
2. A sunscreen composition according to claim 1 wherein said oil component comprises at least one ester component and at least one silicone oil component.
3. A sunscreen composition according to claim 1 wherein said grease component comprises at least dibutyl adipate and butyl octanol salicylate.
4. A sunscreen composition according to claim 1, wherein said methylenebis-benzotriazole-tetramethylbutylphenol is a water-dispersible nanoscale organic particulate formed by the use of decyl glucoside as a dispersant. The lower polyol is one or more selected from the group consisting of: glycerol, 1, 3-butanediol, 1, 2-hexanediol, 1, 3-propanediol and ethylhexyl glycerol.
5. A sunscreen composition according to claim 3, wherein the sunscreen composition comprises, in weight percent, 8-15% dibutyl adipate and 9-20% butyl octanol salicylate.
6. A sunscreen composition according to claim 5, wherein the sunscreen composition comprises a total amount of dibutyl adipate and butyl octanol salicylate of 21-35% by weight.
7. A sunscreen composition according to claims 1-6, wherein the composition comprises the following components in weight percent:
1.2-6% of bis-ethylhexyloxyphenol methoxyphenyl triazine;
4-8% of diethylhexyl butyramidotriazinone;
0.8-3% ethylhexyl triazone;
4.5-9% methylene bis-benzotriazolyl tetramethylbutylphenol dispersion;
0.5-3.5% lauroyl lysine;
7-13% lower polyol;
21-35% of a fat component;
2-7% of an emulsifier; and
the balance of water.
8. The sunscreen composition of claim 7, wherein the sunscreen composition comprises, in weight percent:
1.5-4% of bis-ethylhexyloxyphenol methoxyphenyl triazine;
5-7.5% diethylhexyl butyramidotriazinone;
1.0-2.5% ethylhexyl triazone;
6-9% methylene bis-benzotriazolyl tetramethylbutylphenol dispersion;
1.0-3.0% lauroyl lysine;
8-12% lower polyol;
21-30% of a fat component;
3-6% of an emulsifier; and
the balance of water.
9. Use of a sunscreen composition according to claims 1-8 for the preparation of an oil-in-water type sunscreen cosmetic.
10. The use according to claim 9, wherein the oil-in-water type sunscreen cosmetic is a sunscreen emulsion, a sunscreen cream, a sunscreen spray, a sunscreen gel or a sunscreen lotion.
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| CN202311131007.2A CN117064781A (en) | 2023-09-04 | 2023-09-04 | Safe and mild sun-screening composition and application thereof |
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