CN116549349A - Efficient sun-screening synergistic agent, sun-screening agent and preparation method of sun-screening synergistic agent - Google Patents

Efficient sun-screening synergistic agent, sun-screening agent and preparation method of sun-screening synergistic agent Download PDF

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Publication number
CN116549349A
CN116549349A CN202310462255.9A CN202310462255A CN116549349A CN 116549349 A CN116549349 A CN 116549349A CN 202310462255 A CN202310462255 A CN 202310462255A CN 116549349 A CN116549349 A CN 116549349A
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parts
sun
sunscreen
phase
screening
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刘山
江玉林
孔越涛
黄晓红
尹全尹
向文浩
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Shanghai Zhumei Biotechnology Co ltd
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Shanghai Zhumei Biotechnology 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
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9783Angiosperms [Magnoliophyta]
    • A61K8/9789Magnoliopsida [dicotyledons]
    • 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
    • A61K8/39Derivatives containing from 2 to 10 oxyalkylene groups
    • 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
    • A61K8/49Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
    • A61K8/4973Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with oxygen as the only hetero atom
    • A61K8/498Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with oxygen as the only hetero atom having 6-membered rings or their condensed derivatives, e.g. coumarin
    • 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
    • A61K8/55Phosphorus compounds
    • A61K8/553Phospholipids, e.g. lecithin
    • 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
    • A61K8/60Sugars; Derivatives thereof
    • A61K8/602Glycosides, e.g. rutin
    • 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
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73Polysaccharides
    • 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
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73Polysaccharides
    • A61K8/731Cellulose; Quaternized cellulose derivatives
    • 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
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/81Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • A61K8/8141Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
    • A61K8/8152Homopolymers or copolymers of esters, e.g. (meth)acrylic acid esters; Compositions of derivatives of such polymers
    • 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
    • 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
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change

Abstract

The invention relates to the technical field of sun protection, in particular to IPC A61K8, and more particularly relates to a high-efficiency sun protection synergist, a sun protection agent and a preparation method thereof. The sun-screening synergistic agent comprises the following components in parts by weight: (1-3): (2-4): (2-4); the sun-screening agent composed of the sun-screening synergistic agent has the advantages of improving sun-screening performance, saving cost, reducing irritation of products and improving use experience.

Description

Efficient sun-screening synergistic agent, sun-screening agent and preparation method of sun-screening synergistic agent
Technical Field
The invention relates to the technical field of sun protection, in particular to IPC A61K8, and more particularly relates to a high-efficiency sun protection synergist, a sun protection agent and a preparation method thereof.
Background
The safety of sunscreens and the environmental impact have been of interest to consumers and the relevant sectors. For consumers, on the basis of meeting the sun protection effect, the safety and the use experience of sun protection products are the most important, and the influence of social public opinion is the second most important. In terms of safety, organic sunscreens tend to cause skin allergies, and inorganic sunscreens tend to cause poor skin feel and inhalational hazards. In beauty salon: 2022 Consumer negative feedback is first in greasy skin feel, whereas conventional sunscreens are oily or require oil to dissolve themselves.
Based on safety, skin feel and regulation, the use of the sunscreen agents is particularly important in reducing the number and the amount of the sunscreen agents, but the protection capability of the sunscreen products is ensured, so that the industry is continuously searching for novel raw materials to meet market demands.
The prior CN201410205970.5 discloses a solid lipid sun-screening particle coated with a sun-screening agent and a preparation method thereof, and 1 to 15 percent of solid sun-screening agent, 3 to 18 percent of liquid sun-screening agent, 2 to 20 percent of solid lipid, 3 to 20 percent of liquid lipid, 3 to 15 percent of solid emulsifier, 0.5 to 20 percent of additive, 0.01 to 0.8 percent of preservative and the balance of deionized water are added, so that the solid lipid sun-screening particle is good in stability, not easy to separate out, and fine and uniform in appearance. But has a certain greasy skin feel after use and has poor use effect.
Prior patent CN202080008613.3 discloses cosmetic compositions comprising a silicone elastomer comprising 0.5-20 wt% of an organic sunscreen agent; and 2-60 wt% of a blend comprising a silicone elastomer gel and a non-silicone solvent selected from hydrocarbons, oils, modified oils, esters, ethers, alcohols, or mixtures thereof; wherein the composition comprises less than 1% by weight of volatile silicone solvent. The product is a washing-free cosmetic with limited sun protection value.
Disclosure of Invention
In order to solve the problems in the prior art, the first aspect of the present invention provides a high-efficiency sun-screening synergist, which comprises a flavone compound, a plant extract, a copolymer and cellulose.
Preferably, the flavone compound comprises one of troxerutin, quercetin, rotenone and catechin; further preferred is troxerutin.
Preferably, the plant extract comprises one or two of flos Hokkaido (Magnola Biondii) flower extract and flos Hokkaido (Magnola Biondii) bark extract; further preferred is a flower extract of Wangchun flowers (Magnola Biondii).
Preferably, the copolymer is an acrylic copolymer.
Preferably, the acrylic copolymer is available from AvoBrite of The HallStar Company TM
Preferably, the cellulose comprises one or more of microcrystalline cellulose, ethylcellulose and ecteinascidin cellulose; further preferred is microcrystalline cellulose.
Preferably, the weight ratio of the flavone compound, the plant extract, the copolymer and the cellulose is (1-3): (1-3): (2-4): (2-4); further preferably, it is 2:2:3:3.
preferably, the troxerutin is purchased from the company of biotechnology, inc. of Saxifraga green; the extract of flos Wallichii (Magnolia Biondii) flowers is purchased from Uygur, shanghai Jia Kai Biotechnology Co., ltd; the acrylic copolymer was purchased from AvoBrite of Hallstar Beauty and Personal care Solutions Company TM The method comprises the steps of carrying out a first treatment on the surface of the The microcrystalline cellulose was purchased from SunSpheres of THE DOW CHEMICAL COMPANY TM BIO SPF Booster。
According to the invention, the sun-screening performance of the sun-screening agent is improved and the use feeling of the sun-screening agent is improved by adding the sun-screening synergistic agent. At present, the sun-screening product has good use feeling and moisturizing and soothing effects while keeping the sun-screening effect. The applicant speculates that in order to reduce the use of inorganic sunscreens and solve the problem of greasy skin feel, troxerutin, a flos mori extract, an acrylic ester copolymer, microcrystalline cellulose and other substances of the sunscreens are selected to perform synergistic action together, so that the ultraviolet absorption of 240-270 nm and 320-380 nm is enhanced, a uniform, durable and stable water-resistant sunscreening layer is formed on the product rapidly, and the degradation of the ultraviolet absorbent can be reduced. The ultraviolet light can be absorbed, and meanwhile, the ultraviolet radiation can be effectively scattered, and the optical path is increased, so that the sun-screening effect is improved. Meanwhile, the addition of the four substances enhances the use feeling of the sun-screening agent.
In the invention, troxerutin, the extract of the flos verruceae, the acrylic ester copolymer and microcrystalline cellulose are added, so that the use feeling of the sun cream is improved, and the sun protection value is also improved. The inventor finds that when only three substances in the sun protection synergistic agent are added, the sun protection value, spreadability, smearing feeling, uniformity, greasy feeling, skin adhesion, water resistance and viscous feeling are all reduced to a certain extent, and when the weight ratio of the four components is (1-3): (1-3): (2-4): (2-4) the effect of the composition is improved, and the effect of the composition is not significantly different from that of the composition without the addition of the sunscreen synergistic agent when only three components are added. The inventor speculates that troxerutin, flos Hederae sinensis extract, acrylic ester copolymer and microcrystalline cellulose respectively enhance the sun-proof effect of the system from four layers of ultraviolet absorption, damage after sun-drying, film forming light stabilization and refraction of UV light, but the solvent system or groups in the various raw materials can interact, when only three raw materials are matched, some active substances in the three raw materials can interact, a complete reticular film structure can not be formed, the scattering efficiency of hollow spheres is weakened, the light layer is reduced, and the sun-proof factor is reduced. When the four raw materials are mutually matched, active substances in the system can be stably combined in the reticular structure to form a complete membrane structure, the scattering function of the hollow sphere can be exerted to a large extent, the absorbance of ultraviolet radiation is enhanced, and therefore the sun protection factor of the formula is improved. Meanwhile, the content of the four substances in the specific range is added, so that the use feeling of the whole sun-screening agent can be improved.
In a second aspect, the present invention provides a sunscreen comprising a high efficiency sunscreen booster comprising the components of phase A, phase B, phase C and phase D;
the phase A comprises, by weight, 1 to 2 parts of a polyglycerol-6 stearate and polyglycerol-6 behenate composition, 4 to 7 parts of ethylhexyl isononanoate, 6 to 9 parts of ethylhexyl methoxycinnamate, 0.5 to 1.5 parts of bis-ethylhexyl oxyphenol methoxyphenyl triazine, 1 to 3 parts of cetyl alcohol phosphate potassium, 0.1 to 10 parts of a glycerol and inulin lauryl carbamate composition, 0.5 to 1.5 parts of dibutyl adipate, and 0.5 to 1.5 parts of behenyl alcohol;
the phase B comprises 1 to 3 parts of cyclopentadimethicone, 0.5 to 1.5 parts of vinyl dimethicone/polymethylsilicone silsesquioxane cross-linked polymer, 1 to 3 parts of octyl polymethylsilicone, and 1 to 3 parts of titanium dioxide and triethoxy octyl silane composition;
the phase C comprises 50 to 65 parts of deionized water, 4 to 7 parts of glycerol, 0.05 to 0.5 part of carbomer, 0.05 to 0.5 part of acrylic acid (ester) or C10-30 alkanol acrylate crosslinked polymer, 0.1 to 1 part of p-hydroxyacetophenone and 0.1 to 1 part of 1, 2-hexanediol;
the phase D comprises 0.5-1.5 parts of methylenebis-benzotriazole tetramethylbutylphenol, deionized water, decyl glucoside, a combination of propylene glycol and xanthan gum, and 0.5-1.5 parts of deionized water.
Preferably, the sun-screening agent further comprises a phase, wherein the phase E comprises 0.1-1 part of amino acid and 0.1-10 parts of deionized water.
Preferably, the amino acid comprises one or more of arginine, serine, glycine, alanine, leucine.
Preferably, the sun-screening agent further comprises an F phase, wherein the F phase comprises 0.1-1.0 part of essence.
Preferably, the sunscreen further comprises a G phase comprising the sunscreen potentiator.
Preferably, the polyglycerol-6 stearate and polyglycerol-6 behenate composition is available from Evonik Operations GmbHCare PBS 6MB;
Preferably, the glycerol, inulin lauryl carbamate is purchased from INUTEC SL1 from mantting trade Inc.
Preferably, the cyclopentadimethicone is purchased from KF-995, which is believed to be the more silicone internationally traded.
Preferably, the vinyl polydimethylsiloxane/polymethylsiloxane silsesquioxane cross-linked polymer is available from BT-9102, new materials science, inc.
Preferably, the octyl polymethylsiloxane is commercially available from SIL ZP-034 octyl silicone oil, inc. of New materials, tokyo.
Preferably, the methylenebis-benzotriazole tetramethylbutylphenol, water, decyl glucoside, propylene glycol, xanthan gum are available from Pasteur (China) IncM。
According to the invention, by adding the polyglyceryl-6 stearate and polyglyceryl-behenate composition, the lipid emulsifying agents such as cetyl phosphate potassium, inulin lauryl carbamate and the like to compound with microcrystalline cellulose and acrylic ester copolymers, the waterproof property of the sunscreen agent is improved. The inventors speculate that the combination of the polyglycerol-6 stearate and the polyglycerol-behenate, the potassium cetyl phosphate, the inulin lauryl carbamate, the microcrystalline cellulose and the acrylic ester copolymer with other substances in the system can form a high-stability system, is easy to smear and spread, and has higher water resistance.
The third aspect of the present invention provides a method for preparing a sunscreen comprising a high efficiency sunscreen enhancer, comprising: pretreating part of raw materials, accurately weighing various raw materials, mixing A, B, C, D, E, F, G phase raw materials, stirring uniformly, keeping no particle state, filtering, filling, and warehousing.
The preparation method of the sun-screening agent containing the efficient sun-screening synergistic agent comprises the following detailed steps:
s1: pretreating the B-phase raw material, the D-phase raw material and the E-phase raw material;
s2: accurately weighing various raw materials in the formula, and placing the raw materials in a clean and sterilized vessel;
s3: adding the raw materials of the phase C into a main pot, heating to 80-90 ℃, homogenizing at a high speed for 2-4 minutes, and ensuring that the raw materials are dissolved until no particles are needed;
s4: adding the raw material of the phase A into a main pot, heating to 80-90 ℃ to ensure that the raw material is dissolved until no particles exist, and adding the pretreated raw material of the phase B, and uniformly stirring for later use;
s5: starting vacuum, pumping A, B phase raw materials into a main pot, homogenizing and emulsifying at a high speed for 5-8 minutes, fully stirring uniformly, taking a dotted material body, observing whether the appearance and the texture of the material body are uniform, if particles exist, properly prolonging the homogenizing time, ensuring that the emulsification is complete, stirring at a constant temperature and low speed for defoaming for 10-15 minutes, and then cooling;
s6: when the temperature is reduced to 60-70 ℃, adding the pretreated D-phase raw material, fully and uniformly stirring, and continuously reducing the temperature;
s7: when the temperature is reduced to 40-50 ℃, adding the pretreated raw material in the E phase, the pretreated raw material in the F phase and the pretreated raw material in the G phase, and fully and uniformly stirring;
s8: cooling to 35-40 ℃, taking materials for self-inspection, discharging through 80-120 mesh filter cloth after the self-inspection is qualified, and filling after the self-inspection is qualified;
s9: and (5) after filling, carrying out spot inspection, and warehousing after qualified detection.
Preferably, the specific steps in S1 are as follows: cleaning and sterilizing colloid mill equipment, uniformly mixing and stirring the weighed B-phase raw materials, grinding for three to five times by using a colloid mill, and comparing the fineness of sample plate powder, and grinding for three times by using a three-roller grinder if the fineness is insufficient; uniformly mixing D phases D1 and D2 in advance for later use; and uniformly mixing the E phases E1 and E2 in advance for later use.
Advantageous effects
1. According to the invention, the sun-proof synergist is added to improve the sun-proof performance of the sun-proof agent by synergistic effect with other substances in the sun-proof agent, so that the sun-proof value of the sun-proof product is improved.
2. In the invention, troxerutin, extract of flos verrucae rugosae, acrylic ester copolymer and microcrystalline cellulose are added, so that the use feeling of the sun-screening agent is improved.
3. According to the invention, by adding the polyglyceryl-6 stearate and polyglyceryl-behenate composition, the lipid emulsifying agents such as cetyl phosphate potassium, inulin lauryl carbamate and the like to compound with microcrystalline cellulose and acrylic ester copolymers, the waterproof property of the sunscreen agent is improved.
4. The sun-screening agent added with the sun-screening synergistic agent has the functions of moisturizing and relieving, and has a high sun-screening function.
5. The sun-screening agent has certain high sun-screening effect, small irritation and certain effects of moisturizing and repairing red areas.
Drawings
Figure 1 is a graph of the process of human SPF, PA value testing with a portion of the sunscreens of the examples and comparative examples (12 samples were not measured by one person).
FIG. 2 is a process diagram of a sensory evaluation test; the left is a process recipe graph for testing the smear feel of the product of example 1; the right is a process chart for testing the greasy feel of the product of example 1.
FIG. 3 is a detailed view of the sensory evaluation scores of experimental example 1 and comparative examples 1 to 11.
Detailed Description
Example 1
The embodiment provides a high-efficiency sun-screening synergistic agent which comprises, by weight, 1 part of troxerutin, 1 part of flos mori extract, 1.5 parts of acrylic ester copolymer and 1.5 parts of microcrystalline cellulose.
This example provides a sunscreen formulation comprising a high efficiency sunscreen enhancer, prepared as shown in table 1.
TABLE 1
The polyglycerol-6 stearate and polyglycerol-6 behenate compositions were purchased from Evonik Operations GmbHCare PBS 6 MB。
The ethylhexyl isononanoate was purchased from Isopure IPN of Chevron Phillips Chemical Company LP.
The ethylhexyl methoxycinnamate was purchased from basf (china) limited.
The bis-ethylhexyloxyphenol methoxyphenyl triazine was purchased from basf (china) limitedS。
The potassium cetyl phosphate was purchased from AMPHISOL K of DSM Nutritional Products China.
The glycerol, inulin lauryl carbamate, was purchased from INUTEC SL1, a trade company, inc. of Ceramium.
The dibutyl adipate was purchased from Cetiol B of Basoff (China) Inc.
The behenyl alcohol was purchased from Lanete 22, a company of Basiff (China).
The cyclopentadimethicone was purchased from KF-995, believed to be the more silicone internationally trade.
The vinyl polydimethylsiloxane/polymethylsiloxane silsesquioxane cross-linked polymer was purchased from BT-9102, new materials science and technology, inc.
The octyl polymethylsiloxane is SIL ZP-034 octyl silicone oil from Guangdong Heterol New Material Co.
The acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer is purchased from Pemulen of Shanghai, inc. of Libo specialty chemical industry TM TR-2 Polymer。
The titanium dioxide and triethoxyoctylsilane compositions are available from Micro TiO2 035 AS of k.s. pearl co., ltd.
The glycerol is purchased from refined glycerol of the Fengyi oil technology (Dongguan) limited company.
Said carbomers are available from Lubrizol Advanced Materials, inc980 Polymer。
The p-hydroxyacetophenone was purchased from Symrise Shanghai LTDH(672096)。
The 1, 2-hexanediol is available from Symrise Shanghai LTD6O。
The methylenebis-benzotriazole-tetramethylbutylphenol, water, decyl glucoside, propylene glycol, and xanthan gum composition was purchased from basf (chinese) limitedM。
The arginine was purchased from BINACTI AR, shanghai Violet biological medicine Co.
The troxerutin is purchased from the Xian green biotechnology company; the extract of flos Wallichii (Magnolia Biondii) flowers is purchased from Uygur, shanghai Jia Kai Biotechnology Co., ltd; the acrylic copolymer was obtained from AvoBrite of Hallstar Beauty and Personal care Solutions Company TM The method comprises the steps of carrying out a first treatment on the surface of the The microcrystalline cellulose was purchased from SunSpheres of THE DOW CHEMICAL COMPANY TM BIO SPF Booster。
The preparation method of the sun-screening agent containing the efficient sun-screening synergistic agent comprises the following steps of:
s1: cleaning and sterilizing colloid mill equipment, mixing and stirring the weighed B1, B2, B3 and B4 of the B phase raw materials uniformly, grinding three to five times by using a colloid mill (reserving A7 washing grinder), comparing the fineness of sample plate powder, and grinding three times by using a three-roller grinder if the fineness is insufficient for later use; evenly mixing the D phases D1 and D2 in advance for later use; uniformly mixing F phase F1 and F2 in advance for later use;
s2: accurately weighing various raw materials in the formula, and placing the raw materials in a clean and sterilized vessel;
s3: adding C1, C2, C3, C4, C5 and C6 in the phase C into a main pot, heating to 80 ℃, homogenizing at high speed for 2 minutes, and ensuring that the mixture is dissolved until no particles are needed;
s4: adding A phases A1, A2, A3, A4, A5, A6, A7 and A8 into a main pot, heating to 80 ℃ to ensure that the B phases are dissolved until no particles exist, adding B1, B2, B3 and B4 of the pretreated B phase raw materials, and uniformly stirring for later use;
s5: starting vacuum, pumping the phase A and phase B raw materials into a main pot, homogenizing and emulsifying at a high speed for 5 minutes, fully stirring uniformly, taking a dotted material body, observing whether the appearance and the texture of the material body are uniform, if particles exist, properly prolonging the homogenizing time, ensuring that the emulsification is complete, stirring at a constant temperature and low speed for defoaming for 10 minutes, and then cooling;
s6: when the temperature is reduced to 65+/-2 ℃, adding the pretreated D phases D1 and D2, fully and uniformly stirring, and continuously reducing the temperature;
s7: and cooling to 43+/-2 ℃, and adding G1, G2, G3 and G4 of the E1, E2 and F1 and G phases in the pretreated E phase. Fully and uniformly stirring;
s8: cooling to 38+/-2 ℃, taking materials for self-inspection, discharging through a 100-mesh filter cloth after the self-inspection is qualified, and filling after the self-inspection is qualified;
s9: and (5) after filling, carrying out spot inspection, and warehousing after qualified detection.
Comparative example 1
The embodiment of comparative example 1 is the same as example 1, except that the sunscreen synergist is absent from the sunscreen agent.
Comparative example 2
The embodiment of comparative example 2 is the same as in example 1 except that the sun-screening synergist is 1 part of a flower extract of flos Hemerocallis (Magnoliabiodii), 1.5 parts of an acrylic copolymer, and 1.5 parts of microcrystalline cellulose.
Comparative example 3
The embodiment of comparative example 3 is the same as example 1 except that the sun-screening synergist is 2 parts of flos Hemerocallis (Magnoliabiodii) flower extract, 3 parts of acrylic copolymer, and 3 parts of microcrystalline cellulose.
Comparative example 4
The embodiment of comparative example 4 is the same as in example 1, except that the sunscreen synergist is 0.5 parts of troxerutin, 1.5 parts of acrylic copolymer, and 3 parts of microcrystalline cellulose.
Comparative example 5
The embodiment of comparative example 5 is the same as in example 1, except that the sun-screening synergist is 0.5 part of troxerutin, 1 part of flos Hemerocallis (Magnoliabindii) flower extract, and 3 parts of acrylic copolymer.
Comparative example 6
The embodiment of comparative example 6 is the same as in example 1 except that the sun-screening synergist is 0.5 parts of troxerutin, 2 parts of flos Hemerocallis (Magnoliabindii) flower extract, and 1.5 parts of microcrystalline cellulose.
Comparative example 7
The specific embodiment of comparative example 7 is the same as in example 1, except that the sunscreen synergist is 1 part of troxerutin, 3 parts of acrylic ester copolymer, and 1.5 parts of microcrystalline cellulose.
Comparative example 8
The embodiment of comparative example 8 is the same as in example 1, except that the sunscreen synergist is 1 part of troxerutin, 1 part of flos Hederae sinensis (Magnoliabiodii) flower extract, and 3 parts of microcrystalline cellulose.
Comparative example 9
The specific embodiment of comparative example 9 is the same as example 1, except that the sunscreen synergist is 1 part of troxerutin, 2 parts of flos Hederae sinensis (Magnoliabiodii) flower extract, and 1.5 parts of acrylic copolymer.
Comparative example 10
The embodiment of comparative example 10 is the same as in example 1, except that the sunscreen synergist is 0.5 parts of troxerutin, 1 part of argania spinosa (ARGANIASPINOSA) kernel oil, a tocopherol acetate and bisabolol composition, and 3 parts of acrylic copolymer.
The argania spinosa (ARGANIASPINOSA) kernel oil, tocopheryl acetate, and bisabolol compositions were purchased from supboost ATB, a company of the open-euro trade, shanghai, co.
Comparative example 11
The embodiment of comparative example 11 is the same as in example 1, except that the sunscreen synergist is 0.5 parts of troxerutin, 0.1 parts of bisabolol and ginger (ZINGIBER OFFICINALE) root extract composition, 3 parts of acrylic copolymer.
The bisabolol and ginger (ZINGIBER OFFICINALE) root extract composition is available from Dendropanne fragrance (Nantong) Inc100。
Performance testing
1. And screening out the subjects with skin types I, II and III (sensitive to sunlight or ultraviolet irradiation reaction, and being easy to generate sunburn and difficult to generate pigmentation) to test SPF values by using an Antera multifunctional 3D skin imaging analyzer, and selecting the subjects with skin types III and IV to test PA values. According to the requirements of cosmetic safety technical Specification (2015 edition), a manual simulation sun meter is used for measuring human SPF and PA values of example 1, comparative examples 1-11 and commercial products (SPF50+PA++ of Miranona clear sunscreen cream), a test chart is shown in figure 1, and meanwhile, machine tests are carried out on experimental examples and comparative examples, mainly a quantitative detection method of sun-screening products of Hallstar patent (US 20180313694A 1) is adopted, and a matched instrument is SolasureTM Sunscreen Testing Platform. The machine test flow is as follows:
A. and repeatedly coating the sun-proof sample on the quartz sheet with accurate thickness by using a full-automatic coating platform and a coater to obtain a plurality of sun-proof sample coatings with good reproducibility and accurate coating film thickness. The comparative thickness of the film was 5 microns.
B. The absorption curve of the film sample was measured with an ultraviolet-visible spectrophotometer and the absorption value between 290 nm and 400 nm was recorded.
C. The film sample was irradiated with simulated sunlight using an HPA skin-beautifying lamp with a lamp power of 6.7 mW/square
The irradiation dose corresponds to the sunlight irradiation dose of 31 DEG in North latitude and 1 hour in noon in summer.
D. After irradiation, the absorption curve of the sample coating film is measured by an ultraviolet-visible spectrophotometer, and the measured value is substituted into an ISO24443 calculation formula to calculate the SPF value and the PA value measured by an experimental example machine. And its cost was calculated, and the results are shown in table 2.
TABLE 2
2. Sensory evaluation test
30 testers with ages between 18 and 55 are screened for healthy skin types using skin care products at ordinary times. The volunteers were scored separately for each of the experimental examples (test article was example 1, comparative examples 1 to 11, commercially available products), and the test subjects scored according to the evaluation form (table 3) and filled in the evaluation form for data arrangement analysis. The results are reported in Table 4, table 5; table 5 is the sensory test scoring results for volunteers using the product in example 1. The method of testing is shown in FIG. 2. A comparison of the overall details of the examples and comparative examples is shown in FIG. 3.
TABLE 3 Sun protection sensory evaluation scoring criteria specification sheet
TABLE 4 Table 4
TABLE 5
3. Moisture content of stratum corneum
The detection method comprises the following steps: 30 volunteers were selected, and the test areas were marked on the inner sides of the forearms of both hands of the subject, with the test areas being 3X 3cm, and each test area being spaced at least 1cm apart. The product obtained in example 1 and commercially available product 1 were combined in an amount of (2.0.+ -. 0.1) mg/cm 2 The method comprises the steps of (1) carrying out single coating on the dosage of the skin tester, uniformly coating a sample in a test area by using a latex fingerstall, recording the actual sample coating quantity, and carrying out measurement of each area after adjusting the instrument according to the use instruction of the skin tester by a capacitance method, wherein each area is measured for 3 times in parallel; initial values of the test areas were measured first, and then skin moisture contents of the areas after 1h, 4h, 6h, and 8h were measured, respectively. Descriptive statistics were performed on the measurements for each test area, and the average, maximum, and rate of change were recorded and the results are reported in table 6.
The results of the comparison data of the moisture content of the horny layer are shown in Table 6; higher values of the water content of the stratum corneum indicate better moisturizing effect.
TABLE 6
4. Percutaneous moisture loss test
The detection method comprises the following steps: selecting 30 volunteers, cleaning the tested part with warm water and wiping the tested part with a chipless paper towel before starting a test; measurement area markers were made on the inside of the forearms of the subject's hands, the test areas were 3X 3cm in area, and each test area was spaced at least 1cm apart. Using the product obtained in example 1 and commercially available product 1, the ratio of mg/cm was (2.0.+ -. 0.1) 2 The amount of the composition is coated for one time, test areas of a subject are respectively coated, initial values of the test areas of the subject are measured firstly, the test areas are measured in parallel for 3 times, and then the test areas are measured by a percutaneous water loss rate testerThe transepidermal water loss rates of subjects 1h, 4h, 6h, 8h using different products were determined 3 times in parallel and descriptive statistics were performed on the measurements for each test area, and the average, maximum, and rate of change were recorded and the results are reported in table 7.
The results of the comparison of the percutaneous moisture loss rate and the data are shown in Table 7. The lower the percutaneous water loss rate is, the better the water locking effect is.
TABLE 7
4. Skin redness a value test
The detection method comprises the following steps: 31 volunteers were selected, and the products prepared in example 1 and the commercial products were used on the random sides of the left and right faces of the subjects, and VISI-CR photographing was performed before trial (D0), after trial for 14 days (D14) and after trial for 28 days (D28), and the red area a values of the facial skin were analyzed by IPP image analysis software, and were counted, and the mean, standard deviation, standard error, minimum, maximum were recorded, and the results were recorded in Table 8.
The skin red area a value test value describes the statistics and the results are recorded in a table 8; the greater the value of the a-value of the red area of the skin, the more severe the Pi Fufan red.
The results of the percent change before and after use of the skin red area a values are reported in Table 9. As is clear from tables 8 and 9, the sunscreens prepared in example 1 were used to improve the redness of the skin.
TABLE 8
TABLE 9
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Claims (10)

1. A high-efficiency sun-screening synergistic agent is characterized by comprising the following components of a flavone compound, a plant extract, a copolymer and cellulose.
2. The high-efficiency sunscreen synergistic agent of claim 1, wherein the flavone compound comprises one of troxerutin, quercetin, rotenone and catechin.
3. The high-efficiency sunscreen synergistic agent of claim 1, wherein the plant extract comprises one or two of a flower extract of hopanax hopefully (Magnolia Biondii) and a bark extract of hopanax hopefully (Magnolia Biondii).
4. The high efficiency sunscreen synergist of claim 1 wherein the copolymer is an acrylic copolymer.
5. The high efficiency sunscreen booster according to claim 1, wherein the cellulose comprises one or more of microcrystalline cellulose, ethylcellulose, and ecteinascidin cellulose.
6. The efficient sunscreen synergistic agent according to claim 1, wherein the weight ratio of flavone compound, plant extract, copolymer and cellulose is (1-3): (1-3): (2-4): (2-4).
7. A sunscreen comprising the high-potency sunscreen potentiator of any one of claims 1 to 6, characterized in that its composition comprises phase a, phase B, phase C and phase D;
the phase A comprises, by weight, 1 to 2 parts of a polyglycerol-6 stearate and polyglycerol-6 behenate composition, 4 to 7 parts of ethylhexyl isononanoate, 6 to 9 parts of ethylhexyl methoxycinnamate, 0.5 to 1.5 parts of bis-ethylhexyl oxyphenol methoxyphenyl triazine, 1 to 3 parts of cetyl alcohol phosphate potassium, 0.1 to 10 parts of a glycerol and inulin lauryl carbamate composition, 0.5 to 1.5 parts of dibutyl adipate, and 0.5 to 1.5 parts of behenyl alcohol;
the phase B comprises 1 to 3 parts of cyclopentadimethicone, 0.5 to 1.5 parts of vinyl dimethicone/polymethylsilicone silsesquioxane cross-linked polymer, 1 to 3 parts of octyl polymethylsilicone, 1 to 3 parts of titanium dioxide and triethoxy octyl silane composition and 1 to 3 parts of deionized water;
the phase C comprises 50 to 65 parts of deionized water, 4 to 7 parts of glycerol, 0.05 to 0.5 part of carbomer, 0.05 to 0.5 part of acrylic acid (ester) or C10-30 alkanol acrylate crosslinked polymer, 0.1 to 1 part of p-hydroxyacetophenone and 0.1 to 1 part of 1, 2-hexanediol;
the phase D comprises 0.5 to 1.5 parts of methylenebis-benzotriazole tetramethylbutylphenol, deionized water, decyl glucoside, a composition of propylene glycol and xanthan gum, and 0.5 to 1.5 parts of deionized water;
the sun-screening agent also comprises a G phase, wherein the G phase comprises the sun-screening synergistic agent.
8. The sunscreen comprising a high efficiency sunscreen booster according to claim 7, wherein said sunscreen further comprises an E phase comprising from 0.1 to 1 part amino acid and from 0.1 to 10 parts deionized water.
9. The sunscreen comprising a high efficiency sunscreen booster according to claim 8, wherein said sunscreen further comprises an F phase comprising 0.1 to 1.0 parts of perfume.
10. The method of preparing a sunscreen comprising a high efficiency sunscreen booster according to claim 9, wherein the preparation process comprises: pretreating part of raw materials, accurately weighing various raw materials, mixing A, B, C, D, E, F, G phase raw materials, stirring uniformly, keeping no particle state, filtering, filling, and warehousing.
CN202310462255.9A 2023-04-25 2023-04-25 Efficient sun-screening synergistic agent, sun-screening agent and preparation method of sun-screening synergistic agent Pending CN116549349A (en)

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