CN110801402A - Sunscreen composition and preparation method thereof - Google Patents

Sunscreen composition and preparation method thereof Download PDF

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CN110801402A
CN110801402A CN201911210237.1A CN201911210237A CN110801402A CN 110801402 A CN110801402 A CN 110801402A CN 201911210237 A CN201911210237 A CN 201911210237A CN 110801402 A CN110801402 A CN 110801402A
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colorant
weight
composition
titanium dioxide
sunscreen
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苏晋峰
邓伟健
林锦雄
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Guangzhou I & B Biological Technology Co Ltd
Guangzhou Aibei Biological Technology Co Ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/29Titanium; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/34Alcohols
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/67Vitamins
    • A61K8/678Tocopherol, i.e. vitamin E
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/92Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
    • A61K8/922Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P29/00Non-central analgesic, antipyretic or antiinflammatory agents, e.g. antirheumatic agents; Non-steroidal antiinflammatory drugs [NSAID]
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q17/00Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
    • A61Q17/04Topical preparations for affording protection against sunlight or other radiation; Topical sun tanning preparations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/08Anti-ageing preparations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/59Mixtures
    • A61K2800/592Mixtures of compounds complementing their respective functions
    • A61K2800/5922At least two compounds being classified in the same subclass of A61K8/18

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Abstract

The invention provides a sunscreen composition and a preparation method thereof, belonging to the field of cosmetics. The composition has synergistic resistance to UVB and near infrared rays IR-A by compounding the sunscreen agent A containing the acicular titanium dioxide and the sunscreen agent B containing the spherical titanium dioxide; has effects in resisting UVA damage by containing zinc dioxide; the synergistic antioxidation and anti-inflammatory effects of the argania spinosa kernel oil, the tocopherol acetate and the bisabolol improve the sun protection value and reduce the influence on skin feel and stability caused by excessive addition of the sun protection agent; the composition realizes the effect of resisting all-band radiation harmful to skin in daily sunlight, and the contained sun-screening agent has high transparency and is easy to be compounded with other cosmetic raw materials for use.

Description

Sunscreen composition and preparation method thereof
Technical Field
The invention belongs to the technical field of cosmetics, and particularly relates to a sunscreen composition and a preparation method thereof.
Background
The use of broad spectrum sunscreens to protect the skin from the harmful effects of the sun, such as skin cancer, premature aging, etc., has become a generally accepted method today. However, more than half of the solar energy received by the skin is visible light and infrared radiation, and the damage caused by the visible light to the skin cannot be ignored, for example, the damage of the visible light to the skin is mainly to generate free radicals and pigmentation; the near infrared IR-A has penetration force to skin higher than that of ultraviolet ray, can generate free radicals to reduce the resistance of skin to oxidative stress, and can cause biological damage to skin, such as collagen fiber destruction, etc., and can enhance the damage of ultraviolet ray to skin and promote skin aging process. There is a lack of solutions for protection against visible and infrared radiation in the products currently on the market.
The mainstream sunscreen product in the market at present mainly realizes the sunscreen function through the independent or combined use of a physical sunscreen agent (reflection/scattering) and a chemical sunscreen agent (absorption). However, both physical and chemical sunscreens suffer from their own drawbacks, such as the dry skin feel of physical sunscreens and the tendency to produce a harsh feel when applied. The chemical sunscreen agents are generally sticky in skin feel, are all limited substances for cosmetics, and have strict limitation on the use amount, so that how to develop a product with high sunscreen value and good skin feel is a big problem in the industry.
Disclosure of Invention
The present invention aims to overcome the above defects in the prior art and provide a sunscreen composition and a preparation method thereof.
In order to achieve the purpose, the invention adopts the technical scheme that:
in a first aspect, the invention provides a sunscreen composition, which comprises the following components in percentage by weight: sunscreen agent A1-5%, sunscreen agent B1-10%; the sunscreen agent A comprises stearoyl glutamic acid and acicular titanium dioxide, and the sunscreen agent B comprises C12-15 alcohol benzoate, silica, polydimethylsiloxane, polyhydroxystearic acid and spherical titanium dioxide, wherein the particle size of the spherical titanium dioxide is 10-15nm or more than 100 nm.
As a preferred embodiment of the composition of the present invention, the sunscreen composition comprises the following components in percentage by weight: sunscreen A5%, sunscreen B8%.
The spherical titanium dioxide with the particle size of 10-15nm can reduce the damage of UVB to skin, the spherical titanium dioxide with the particle size of more than 100nm can reduce the damage of visible light to skin, and the needle-shaped titanium dioxide can reduce the damage of near infrared ray IR-A (wavelength of 750-1500nm) to skin, wherein the structures of the spherical titanium dioxide and the needle-shaped titanium dioxide are shown in figure 1, when the spherical titanium dioxide and the needle-shaped titanium dioxide are compounded, the spherical titanium dioxide and the needle-shaped titanium dioxide have the spatial complementary effect on the structures, so that higher coverage is realized when the spherical titanium dioxide and the needle-shaped titanium dioxide are smeared on the skin. When the composition comprises 1 to 5 wt.% of sunscreen A and 1 to 10 wt.% of sunscreen B, its resistance to UVB/visible light, and also to near infrared light IR- A, is enhanced by the synergistic effect of the spherical titanium dioxide and the acicular titanium dioxide, and in particular when the composition comprises 5 wt.% of sunscreen A and 8 wt.% of sunscreen B, its resistance to UVB/visible light, and also to near infrared light IR- A, is stronger. The transparency of the acicular titanium dioxide is high.
As a preferred embodiment of the composition of the present invention, the acicular titanium dioxide has a particle size of 5 μm. TiO22IR300 (KOBO, USA) contains stearyl glutamic acid 2% and acicular titanium dioxide with a particle size of about 5 μm 98% in mass fraction, respectively, which is mixed with A1K-TiO2(KOBO, U.S.A., containing spherical titanium dioxide having a particle size of 1 μm), sunscreen-grade titanium dioxide (particle size of 10-15nm), and pigment-grade titanium dioxide (particle size of 2-3 μm) are shown in FIG. 2, and the protective effect against infrared rays is shown by TiO2The IR300 has more excellent protection effect on infrared light, in particular to near infrared light IR-A with the wavelength of 750-1500 nm. When the particle size of the acicular titanium dioxide is 5 μm, the paint is almost colorless when applied to the skin.
In a preferred embodiment of the composition of the present invention, the spherical titanium dioxide has a particle size of 15 nm. FIG. 3 shows the light protection effect of spherical titanium dioxide with different particle sizes, wherein the spherical titanium dioxide with 15nm has excellent protection capability against ultraviolet light (i.e. UVB) with the wavelength range of 280-320 nm. Meanwhile, the spherical titanium dioxide with the particle size of 15nm has strong transparency, and is nearly colorless when being smeared on the skin.
As a preferred embodiment of the composition of the present invention, the sunscreen agent a comprises the following components in percentage by weight: 2% of stearoyl glutamic acid and 98% of needle-shaped titanium dioxide; the sunscreen agent B comprises the following components in percentage by weight: 32.5 percent of C12-15 alcohol benzoate, 6 percent of silica, 4 percent of polydimethylsiloxane, 9 percent of polyhydroxystearic acid and 48.5 percent of spherical titanium dioxide.
As a preferred embodiment of the composition of the present invention, said composition further comprises 1-10% by weight of said composition of a sunscreen agent C comprising spherical zinc oxide and triethoxycaprylylsilane; as a more preferred embodiment of the composition according to the invention, said sunscreen agent C represents 7% by weight of the composition, said sunscreen agent comprising the following components in percentage by weight: 97% of spherical zinc oxide and 3% of triethoxyoctylsilane.
As a preferred embodiment of the composition of the present invention, the zinc oxide has a particle size of 15 to 35 nm. FIG. 4 is a graph comparing the sunscreen effect of zinc oxide of different particle sizes, where PPS and PS are defined as follows: when the crystal is very fine, because the surface energy of the crystal grains is very large, the fine crystal grains are easy to be combined together due to weak interaction force, so that agglomeration occurs between the crystal grains, that is, a plurality of fine crystal grains are agglomerated to form larger secondary particles. As can be seen from FIG. 4, the 15-35nm zinc oxide protection range is 290-380nm wavelength UV light, covering the UVB and most of the UVA region, where it acts as the primary UVA filter.
As a preferred embodiment of the composition of the present invention, the composition further comprises the following components in percentage by weight: colorant A1-10%, colorant B0.1-2%, colorant C0.01-1%, colorant D0.01-1%, wherein colorant A is a mixture of titanium dioxide, disodium stearyl glutamate, and aluminum hydroxide, colorant B is a mixture of yellow iron oxide, disodium stearyl glutamate, and aluminum hydroxide, colorant C is a mixture of red iron oxide, disodium stearyl glutamate, and aluminum hydroxide, and colorant D is a mixture of black iron oxide, disodium stearyl glutamate, and aluminum hydroxide. The colorant B, the colorant C and the colorant D contain iron oxide, can absorb visible light and play a role in enhancing the body resistance to visible light. The colorant A contains titanium dioxide, is white, and can play a role in emitting and scattering visible light.
As a more preferred embodiment of the composition of the present invention, the composition further comprises the following components in percentage by weight: colorant A4%, colorant B0.7%, colorant C0.15%, colorant D0.06%, wherein the colorant A comprises the following components by weight percent: 94% of titanium dioxide, 3% of disodium stearoyl glutamate and 3% of aluminum hydroxide; the colorant B comprises the following components in percentage by weight: 96.5% of yellow iron oxide, 3% of disodium stearyl glutamate and 0.5% of aluminum hydroxide; the colorant C comprises the following components in percentage by weight: 96.5% of red iron oxide, 3% of disodium stearyl glutamate and 0.5% of aluminum hydroxide; the colorant D comprises the following components in percentage by weight: 96.5% of black iron oxide, 3% of disodium stearyl glutamate and 0.5% of aluminum hydroxide.
As a preferred embodiment of the composition of the invention, the composition further comprises 0.1-2% by weight of the composition of an active ingredient which is a mixture of argania spinosa kernel oil, tocopherol acetate and bisabolol.
As a more preferred embodiment of the composition of the present invention, the active ingredient constitutes 1% by weight of the composition.
As a more preferred embodiment of the composition of the present invention, the active ingredient comprises the following components in percentage by weight: 80% of argania spinosa kernel oil, 10% of tocopherol acetate and 10% of bisabolol.
ARGANIA SPINOSA (ARGANIA SPINOSA) kernel oil, also known as argan oil, is extracted from the fruit of argan tree and is rich in fatty acids (including large amounts of essential fatty acids, unsaturated fatty acids, and linoleic acid), sterols, vitamin E, and phenolic compounds, wherein the fatty acids maintain a healthy hydration level in humans; the linoleic acid has obvious effects on resisting inflammation, reducing acne and moisturizing when being applied to the skin; essential fatty acids can retard premature skin aging and wrinkles; the phytosterol can help to soften skin, stimulate pores to expel toxin and restore natural lipid barrier; polyphenols are well known antioxidants and can delay skin aging and prolong the duration of action of other antioxidants (e.g. vitamin E, vitamin C) in the human body.
Tocopherol acetate is a derivative of vitamin E, has a good antioxidant effect and better stability, can prevent skin from being rough and chapped, promotes wound healing, prevents inflammation, improves black spots and the like, and thus has good performance in resisting ultraviolet rays on the skin.
The bisabolol is extracted from Chrysanthemum plant, and has antiinflammatory and antibacterial effects. The composition can reduce skin inflammation, relieve skin acne, prevent acne, improve skin irritation resistance, and repair skin with inflammation injury.
Compounding argania spinosa kernel oil, tocopherol acetate and bisabolol, screening out a proper proportion through testing, and achieving the effect of improving the sun protection value under the condition of not adding a sun protection agent by utilizing the synergistic effect of the argania spinosa kernel oil, the tocopherol acetate and the bisabolol in oxidation resistance and inflammation resistance; meanwhile, the influence on skin feeling and stability caused by excessive addition of the sun-screening agent can be reduced.
As a preferred embodiment of the composition of the present invention, the composition is a foundation.
As a preferred embodiment of the composition of the present invention, the composition further comprises the following components in percentage by weight: 1-8% of butanediol dicaprylate/dicaprate (CAS number 211107-84-5), 1-10% of phenyl trimethicone, 5-20% of cyclopenta dimethyl silicone, 1-5% of lauryl PEG-9 polydimethylsiloxyethyl polydimethylsiloxane, 1-5% of PEG-10 polydimethylsiloxane, 1-10% of ethylhexyl methoxycinnamate, 1-5% of ethylhexyl salicylate, 0.1-2% of disteardimonium hectorite, 1-5% of polymethyl methacrylate, 1-15% of butanediol, 0.1-2% of sodium chloride, 0.1-5% of ethanol, 0.05-0.5% of a mixture of octylglycol and ethylhexylglycerin, 0.05-1% of a mixture of phenoxyethanol and ethylhexylglycerin, and the balance of water.
As a more preferred embodiment of the composition of the present invention, the composition further comprises the following components in percentage by weight: 4% of butanediol dicaprylate/dicaprate, 3% of phenyl trimethicone, 17% of cyclopenta dimethyl silicone, 2% of lauryl PEG-9 polydimethylsiloxyethyl dimethyl silicone, 3% of PEG-10 dimethyl silicone, 8% of ethylhexyl methoxycinnamate, 3% of ethylhexyl salicylate, 0.8% of distearyl dimethyl ammonium hectorite, 4% of polymethyl methacrylate, 6% of butanediol, 1% of sodium chloride, 0.3% of ethanol, 0.1% of a mixture of capryl glycol and ethylhexyl glycerol, 0.4% of a mixture of phenoxyethanol and ethylhexyl glycerol, wherein the weight ratio of capryl glycol and ethylhexyl glycerol is capryl glycol: and (3) the weight ratio of the phenoxyethanol to the ethylhexyl glycerin is phenoxyethanol: ethylhexyl glycerin ═ 9: 1.
In a second aspect, the present invention also provides a method for preparing a sunscreen composition, comprising the steps of: mixing butanediol dicaprylate/dicaprate, stearoylglutamic acid, acicular titanium dioxide, spherical zinc oxide, triethoxyoctylsilane, a coloring agent A, a coloring agent B, a coloring agent C and a coloring agent D, grinding, adding C12-15 alcohol benzoate, silica, polydimethylsiloxane, polyhydroxystearic acid, spherical titanium dioxide, phenyl trimethicone, cyclopentadimethylsiloxane, lauryl PEG-9 polydimethylsiloxyethyl polydimethylsiloxane, PEG-10 polydimethylsiloxane, ethylhexyl methoxycinnamate, ethylhexyl salicylate, disteardimonium hectorite, argan kernel oil, tocopherol acetate, bisabolol and polymethyl methacrylate, homogenizing, and stirring to obtain an oil phase; mixing octyl glycol, ethylhexyl glycerol, phenoxyethanol, butanediol, water, sodium chloride and ethanol, and stirring uniformly to obtain a water phase; and adding the water phase into the stirred oil phase, homogenizing and stirring to obtain the sun-screening composition, wherein the colorant A is a mixture of titanium dioxide, disodium stearoyl glutamate and aluminum hydroxide, the colorant B is a mixture of yellow iron oxide, disodium stearoyl glutamate and aluminum hydroxide, the colorant C is a mixture of red iron oxide, disodium stearoyl glutamate and aluminum hydroxide, and the colorant D is a mixture of black iron oxide, disodium stearoyl glutamate and aluminum hydroxide.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the composition of the present invention has A synergistic effect against at least one of UVB, visible light and near infrared IR-A by combining sunscreen A containing acicular titanium dioxide and sunscreen B containing spherical titanium dioxide.
(2) The composition has strong resistance to ultraviolet rays and visible light and infrared light, realizes the resistance effect to the all-band radiation (200-1500nm) harmful to the skin in the sunlight, and simultaneously has high transparency of the contained sun-screening agent, thereby being easy to be compounded with other cosmetic raw materials for use.
(3) The composition improves the sun-screening value and reduces the influence on skin feel and stability caused by excessive addition of the sun-screening agent through the synergistic antioxidant and anti-inflammatory effects of the argania spinosa kernel oil, the tocopherol acetate and the bisabolol.
Drawings
FIG. 1 is an electron microscope photograph of acicular titanium dioxide and spherical titanium dioxide;
FIG. 2 is a graph comparing the sunscreen effect of acicular titanium dioxide with other titanium dioxide;
FIG. 3 is a graph showing the sun-screening effect of spherical titanium dioxide particles of different particle sizes;
FIG. 4 is a graph comparing the sunscreen effect of zinc oxide of different particle sizes.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
Examples 1 to 6
Examples 1-6 are examples of sunscreen compositions of the present invention having the compositions shown in table 1.
TABLE 1 composition/wt% of sunscreen compositions in examples 1-6
Figure BDA0002294168680000071
Figure BDA0002294168680000081
Examples 7 to 12
Examples 7-12 are examples of sunscreen compositions of the present invention having the compositions shown in Table 2.
TABLE 2 composition/wt% of sunscreen compositions in examples 7-12
Figure BDA0002294168680000082
Figure BDA0002294168680000091
Sunscreen agents A of examples 1-12 were all available from Kobo Products, USA, and are all available as TiO2-IR300, and comprise 2% stearyl glutamic acid and 98% acicular titanium dioxide having a particle size of about 5 μm, respectively, by mass fraction; sunscreen agents B, each available from SUNJIN CHEMICAL co., ltd., korea, and each available as TXD60-AB, comprise 32.5% by weight of C12-15 alcohol benzoate, 6% by weight of silica, 4% by weight of polydimethylsiloxane, 9% by weight of polyhydroxystearic acid, and 48.5% by weight of approximately 15nm spherical titanium dioxide; sunscreen C was purchased from SUNJIN CHEMICAL CO., LTD., Korea, and was sold as SUNZnO-NAS, which included 97% by mass of 15-35nm zinc oxide and 3% by mass of triethoxyoctylsilane, respectively; colorant a, colorant B, colorant C, and colorant D were all available from Miyoshi Kasei, Inc. (samo chemie co.), wherein the types of the colorant A are all NAI-TSR-10 and comprise 94 mass percent of titanium dioxide, 3 mass percent of disodium stearyl glutamate and 3 mass percent of aluminum hydroxide respectively, the types of the colorant B are all NAI-MTY-10 and comprise 96.5 mass percent of yellow iron oxide, 3 mass percent of disodium stearyl glutamate and 0.5 mass percent of aluminum hydroxide respectively, the types of the colorant C are all NAI-MTR-10 and comprise 96.5 mass percent of red iron oxide, 3 mass percent of disodium stearyl glutamate and 0.5 mass percent of aluminum hydroxide respectively, and the types of the colorant D are all NAI-MTB-10 and comprise 96.5 mass percent of black iron oxide, 3 mass percent of disodium stearyl glutamate and 0.5 mass percent of aluminum hydroxide respectively; the active ingredients are purchased from Kobo Products, USA, and are sold as SunBoost ATB, and comprise 80% of Aralia elata seed oil, 10% of tocopherol acetate and 10% of bisabolol by weight; the preservative A consists of 70 percent of octyl glycol and 30 percent of ethylhexyl glycerol in percentage by mass respectively; the preservative B consists of 90% of phenoxyethanol and 10% of ethylhexyl glycerol in percentage by mass respectively.
The preparation of the sunscreen combination of examples 1-12 includes the following steps:
(1) preparing an oil phase: mixing butanediol dicaprylic acid/dicaprate, a sun-screening agent A, a sun-screening agent C, a coloring agent A, a coloring agent B, a coloring agent C and a coloring agent D, grinding, adding the sun-screening agent B, phenyl trimethicone, cyclopentadimethylsiloxane, lauryl PEG-9 polydimethylsiloxyethyl polydimethylsiloxane, PEG-10 polydimethylsiloxane, ethylhexyl methoxycinnamate, ethylhexyl salicylate, disteardimonium hectorite, an active ingredient and polymethyl methacrylate, homogenizing, stirring and defoaming to obtain an oil phase;
(2) preparing an aqueous phase: mixing the preservative A, the preservative B, butanediol, water, sodium chloride and ethanol, and uniformly stirring to obtain a water phase;
(3) emulsification: and adding the water phase into the stirred oil phase, homogenizing, stirring and defoaming to obtain the sunscreen composition.
Comparative examples 1 to 5
Comparative examples 1 to 5 are each a sunscreen composition having the composition shown in table 3.
Table 3 composition/wt% of sunscreen combinations in comparative examples 1-5
Figure BDA0002294168680000101
Figure BDA0002294168680000111
Effect example 1 transmittance test
1. Principle of experiment
The transmittance of the samples at 300nm (UVB), 350nm (UVA), 565nm (VIS) and 1125nm (IR-A) was measured using A UV-visible-near-IR spectrophotometer model TP 720 (Techno Tokyo instruments, Inc.), and the resistance of each sample to light of different wavelengths was analyzed, with lower transmittance indicating greater resistance of the sample.
2. Experimental methods
0.5mL of the sample was uniformly spread on a quartz glass plate, and then the transmittances at 300nm, 350nm, 565nm and 1125nm were measured.
3. Results of the experiment
The specific test results are shown in Table 4.
TABLE 4 results of transmittance test of sunscreen compositions of examples 1 to 12 and comparative examples 1 to 5
Figure BDA0002294168680000121
4. Conclusion of the experiment
① it can be seen from examples 1 to 4 that the transmittance at 1125nm (IR-A) gradually decreases with increasing concentration of sunscreen A and the transmittance at 300nm (UVB) gradually decreases with increasing concentration of sunscreen B, but when added in an amount exceeding 8% by weight, the decrease in transmittance is insignificant and the repellency effect tends to be saturated;
② it can be seen from examples 3 and 5 to 6 that the transmittance at 350nm (UVA) gradually decreases with increasing concentration of sunscreen C, but when added in an amount exceeding 7% by weight, the decrease in transmittance is insignificant and the repellency effect tends to be saturated;
③ it can be seen from examples 3, 7 to 8 and comparative example 4 that as the concentrations of the colorants A to D increase, the transmittance at 565nm (VIS) gradually decreases, but when the addition amount exceeds a certain value, the decrease in transmittance is insignificant and the resist effect tends to be saturated;
④ it can be seen from examples 3, 9-12 and comparative example 5 that the concentration of the active ingredient and other non-critical ingredients is increased and the transmittance at each wavelength is not significantly changed, indicating that the active ingredient and other non-critical ingredients have little effect on the transmittance;
⑤ it can be seen from example 3 and comparative examples 1-2 that when sunscreen A and sunscreen B are used for formulation, they have a better protection against light in each wavelength range, and that sunscreen A and sunscreen B show a synergistic effect.
Effect example 2 Sun protection index test
1. Principle of experiment
The test was carried out according to the cosmetic standardization document "Cosmetics-Sun protection test methods-In visualization of the Sun Protection Factor (SPF) (International Standard ISO24444First edition,2010-11-15), each of which was specified as follows:
minimum erythematous spot (MED): causing a clearly visible erythema of the skin, ranging up to the minimum dose of UV irradiation (J/m) required for most of the area of the irradiated spot2) Or minimum time (seconds);
sun Protection Factor (SPF): the ratio of the MED required to cause erythema on skin protected by sunscreen to the MED required to cause erythema on unprotected skin is the SPF of the sunscreen.
2. Experimental methods
(1) Light source
The sunlight simulator xenon arc lamp is used as a light source and must meet the following conditions:
① can continuously generate ultraviolet rays with wavelength of 290 nm-400 nm;
② filtering the light source output by the filter, the ultraviolet ray with wavelength less than 290nm should be less than 1%;
③ filtering the light source output by the filter, the ultraviolet ray with wavelength more than 400nm should be less than 5%;
④ the light source should output stable and uniform light, and its fluctuation range on the irradiated plane should be less than 10%.
(2) Selection of the subject
① selecting 5 healthy volunteer subjects of 18-60 years old;
② there is no history of photosensitivity disease, and no medicine affecting photosensitivity is used in the near term;
③ the skin types of the subject are type I, II and III, i.e. the skin is sensitive to sunlight or ultraviolet irradiation, and sunburn is easy to occur after irradiation, and pigmentation is not easy to occur;
④ the skin of the tested part should be free of pigmentation, inflammation, scar, pigmented nevus, and hairy hair;
⑤ should be excluded from the subjects when they have been subjected to anti-inflammatory drugs such as corticosteroids during pregnancy, lactation, oral or topical administration, or have been subjected to similar tests during the last month;
(3) MED determination method
① posture of subject, irradiating back, and taking forward or prone position;
② sample coating area not less than 30cm2
③ sample dosage and coating method, according to 2mg sample/cm2Weighing the sample, uniformly coating the sample in a test area by using a latex finger stall, and waiting for 15 minutes;
④ predicting MED of the subject, selecting an irradiation area on the skin of the back of the subject 24 hours before the test product, irradiating 5 points with different ultraviolet rays, wherein the irradiation dose or time can be increased in sequence, observing the result after 24 hours, and taking the minimum irradiation dose or the minimum irradiation time when the skin has erythema as the MED of the normal skin of the subject;
⑤ measuring the SPF value of the test sample, namely simultaneously measuring the MED value of the following three cases on the test day;
⑥ determining MED of the subject, adjusting the UV dose for the predicted MED value, re-determining the MED of the unprotected skin of the subject on the day of the test, applying the product to the skin of the subject, determining the MED of the skin under the protection of the product, selecting the dose increase of the 5-point test site, referring to the SPF value range of the sunscreen product formulation, wherein the dose increase of five irradiation points is 25% for the product with SPF value <15, and 15% for the product with SPF value > 15;
⑦ SPF standards were applied to the test sites and the MED of the skin under protection of the standards was determined.
(4) Calculation of SPF value
SPF-MED for protecting skin/MED for unprotected skin Using sunscreen cosmetic
3. Results of the experiment
The specific test results are shown in Table 5.
Table 5 SPF value test results
Group of SPF value
Example 3 58.4
Example 9 45.8
Example 10 58.8
Example 11 54.2
Example 12 57.9
Comparative example 5 44.3
4. Conclusion of the experiment
① it can be seen from examples 3, 9 to 10 and comparative example 5 that the SPF value is gradually increased as the concentration of the active ingredient is increased, but when the addition amount exceeds 1%, the increase in SPF is not significant and the SPF raising effect tends to be saturated;
② it can be seen from examples 3 and 10-11 that the SPF value varies little with the increase and decrease of the concentration of other non-critical components, and the components are judged to have little influence on the sunscreen effect by the transmittance test;
③ it can be seen from the results of the transmittance test and the sun protection index test that the active ingredient does not act to protect the skin from light by reflection, scattering or absorption, but rather acts to inhibit the development of erythema after the skin has been exposed to light by means of oxidation resistance, soothing the skin, etc.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.

Claims (10)

1. A sunscreen composition, characterized in that it comprises the following components in percentage by weight: 1-5% of sun-screening agent A and 1-10% of sun-screening agent B; the sunscreen agent A comprises stearoyl glutamic acid and acicular titanium dioxide, and the sunscreen agent B comprises C12-15 alcohol benzoate, silica, polydimethylsiloxane, polyhydroxystearic acid and spherical titanium dioxide, wherein the particle size of the spherical titanium dioxide is 10-15nm or more than 100 nm.
2. The composition according to claim 1, wherein the sunscreen composition comprises the following components in weight percent: sunscreen agent A5%, sunscreen agent B8%; the sunscreen agent A comprises the following components in percentage by weight: 2% of stearoyl glutamic acid and 98% of needle-shaped titanium dioxide, wherein the needle-shaped titanium dioxide is 5 microns; the sunscreen agent B comprises the following components in percentage by weight: 32.5 percent of C12-15 alcohol benzoate, 6 percent of silica, 4 percent of polydimethylsiloxane, 9 percent of polyhydroxystearic acid and 48.5 percent of spherical titanium dioxide.
3. The composition according to claim 1, further comprising 1-10% by weight of the composition of a sunscreen agent C comprising spherical zinc oxide and triethoxycaprylylsilane.
4. The composition according to claim 3, characterized in that said sunscreen C represents 7% by weight of the composition and comprises the following components in percentage by weight: 97% of spherical zinc oxide and 3% of triethoxyoctylsilane.
5. The composition according to claim 1, further comprising the following components in weight percent: colorant A1-10%, colorant B0.1-2%, colorant C0.01-1%, colorant D0.01-1%, wherein colorant A is a mixture of titanium dioxide, disodium stearyl glutamate, and aluminum hydroxide, colorant B is a mixture of yellow iron oxide, disodium stearyl glutamate, and aluminum hydroxide, colorant C is a mixture of red iron oxide, disodium stearyl glutamate, and aluminum hydroxide, and colorant D is a mixture of black iron oxide, disodium stearyl glutamate, and aluminum hydroxide; preferably, the composition further comprises the following components in percentage by weight: colorant A4%, colorant B0.7%, colorant C0.15%, colorant D0.06%, wherein the colorant A comprises the following components by weight percent: 94% of titanium dioxide, 3% of disodium stearoyl glutamate and 3% of aluminum hydroxide; the colorant B comprises the following components in percentage by weight: 96.5% of yellow iron oxide, 3% of disodium stearyl glutamate and 0.5% of aluminum hydroxide; the colorant C comprises the following components in percentage by weight: 96.5% of red iron oxide, 3% of disodium stearyl glutamate and 0.5% of aluminum hydroxide; the colorant D comprises the following components in percentage by weight: 96.5% of black iron oxide, 3% of disodium stearyl glutamate and 0.5% of aluminum hydroxide.
6. The composition of claim 1, further comprising from 0.1% to 2% by weight of the composition of an active ingredient which is a mixture of argania spinosa kernel oil, tocopherol acetate and bisabolol; preferably, the active ingredient accounts for 1% of the weight of the composition, and comprises the following components in percentage by weight: 80% of argania spinosa kernel oil, 10% of tocopherol acetate and 10% of bisabolol.
7. Composition according to any one of claims 1 to 6, characterized in that it is a foundation.
8. The composition according to claim 7, further comprising the following components in weight percent: 1-8% of butanediol dicaprylate/dicaprate, 1-10% of phenyl trimethicone, 5-20% of cyclopenta dimethyl silicone, 1-5% of lauryl PEG-9 polydimethylsiloxyethyl polydimethylsiloxane, 1-5% of PEG-10 polydimethylsiloxane, 1-10% of ethylhexyl methoxycinnamate, 1-5% of ethylhexyl salicylate, 0.1-2% of distearyl dimethyl ammonium hectorite, 1-5% of polymethyl methacrylate, 1-15% of butanediol, 0.1-2% of sodium chloride, 0.1-5% of ethanol, 0.05-0.5% of a mixture of octylglycol and ethylhexylglycerin, 0.05-1% of a mixture of phenoxyethanol and ethylhexylglycerin, and the balance of water.
9. The composition according to claim 8, further comprising the following components in weight percent: 4% of butanediol dicaprylate/dicaprate, 3% of phenyl trimethicone, 17% of cyclopenta dimethyl silicone, 2% of lauryl PEG-9 polydimethylsiloxyethyl dimethyl silicone, 3% of PEG-10 dimethyl silicone, 8% of ethylhexyl methoxycinnamate, 3% of ethylhexyl salicylate, 0.8% of distearyl dimethyl ammonium hectorite, 4% of polymethyl methacrylate, 6% of butanediol, 1% of sodium chloride, 0.3% of ethanol, 0.1% of a mixture of capryl glycol and ethylhexyl glycerol, 0.4% of a mixture of phenoxyethanol and ethylhexyl glycerol, wherein the weight ratio of capryl glycol and ethylhexyl glycerol is capryl glycol: and (3) the weight ratio of the phenoxyethanol to the ethylhexyl glycerin is phenoxyethanol: ethylhexyl glycerin ═ 9: 1.
10. A method of preparing a sunscreen composition, said method comprising the steps of: mixing butanediol dicaprylate/dicaprate, stearoylglutamic acid, acicular titanium dioxide, spherical zinc oxide, triethoxyoctylsilane, a coloring agent A, a coloring agent B, a coloring agent C and a coloring agent D, grinding, adding C12-15 alcohol benzoate, silica, polydimethylsiloxane, polyhydroxystearic acid, spherical titanium dioxide, phenyl trimethicone, cyclopentadimethylsiloxane, lauryl PEG-9 polydimethylsiloxyethyl polydimethylsiloxane, PEG-10 polydimethylsiloxane, ethylhexyl methoxycinnamate, ethylhexyl salicylate, disteardimonium hectorite, argan kernel oil, tocopherol acetate, bisabolol and polymethyl methacrylate, homogenizing, and stirring to obtain an oil phase; mixing octyl glycol, ethylhexyl glycerol, phenoxyethanol, butanediol, water, sodium chloride and ethanol, and stirring uniformly to obtain a water phase; and adding the water phase into the stirred oil phase, homogenizing and stirring to obtain the sun-screening composition, wherein the colorant A is a mixture of titanium dioxide, disodium stearoyl glutamate and aluminum hydroxide, the colorant B is a mixture of yellow iron oxide, disodium stearoyl glutamate and aluminum hydroxide, the colorant C is a mixture of red iron oxide, disodium stearoyl glutamate and aluminum hydroxide, and the colorant D is a mixture of black iron oxide, disodium stearoyl glutamate and aluminum hydroxide.
CN201911210237.1A 2019-11-28 2019-11-28 Sunscreen composition and preparation method thereof Pending CN110801402A (en)

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