CN115252510B - Sunscreen composition and application thereof - Google Patents

Sunscreen composition and application thereof Download PDF

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CN115252510B
CN115252510B CN202211194796.XA CN202211194796A CN115252510B CN 115252510 B CN115252510 B CN 115252510B CN 202211194796 A CN202211194796 A CN 202211194796A CN 115252510 B CN115252510 B CN 115252510B
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sunscreen
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ascorbic acid
sun
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CN115252510A (en
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卢智慧
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Guangdong Xuanyuan Biotechnology Co ltd
Huangpu Institute of Materials
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Huangpu Institute of Materials
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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
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/84Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
    • A61K8/88Polyamides
    • 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
    • A61K8/27Zinc; 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
    • A61K8/19Cosmetics 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
    • A61K8/58Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing atoms other than carbon, hydrogen, halogen, oxygen, nitrogen, sulfur or phosphorus
    • 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
    • A61K8/676Ascorbic acid, i.e. vitamin C
    • 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
    • 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
    • A61K2800/41Particular ingredients further characterized by their size
    • A61K2800/413Nanosized, i.e. having sizes below 100 nm
    • 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 discloses a sunscreen composition and application thereof, and relates to the technical field of sunscreen skin care products. The invention provides a sunscreen composition which comprises the following components in parts by weight: 0.1-5 parts of polyglutamic acid, 2-5.5 parts of sophora flower extract, 20-40 parts of physical sun-screening agent, 0.5-5 parts of ascorbic acid and/or ascorbic acid derivative and 0.1-0.3 part of sodium copper chlorophyllin; the physical sun-screening agent is at least one of nano titanium dioxide and nano zinc oxide. When the polyglutamic acid, the sophora flower extract, the physical sun-screening agent, the ascorbic acid and/or ascorbic acid derivatives and the sodium copper chlorophyllin are synergistically acted, the prepared sun-screening composition has good ultraviolet UVA (320-400 nm), UVB (290-320 nm) resistance and good blue light protection effects, and the light protection range of the product is further expanded.

Description

Sunscreen composition and application thereof
Technical Field
The invention relates to the technical field of sunscreen skin care products, in particular to a sunscreen composition and application thereof.
Background
With the development of modern science and technology and the continuous improvement of the living standard of people, on one hand, the work and life rhythm is faster and faster, and the skin burden is larger and larger due to irregular daily work and rest, severe environmental problems and incorrect skin care habits. On the other hand, after the ozone layer is largely depleted due to the destruction of the ozone layer, the ability to absorb ultraviolet radiation is greatly weakened, resulting in a significant increase in the ultraviolet B (UVB) reaching the earth's surface. According to research and investigation, eighty percent of skin aging comes from ultraviolet irradiation, the harm of ultraviolet rays to the skin attracts people's extensive attention, and sun protection becomes a necessary step for daily skin care. The ultraviolet rays are divided into UVA (320-420 nm), UVB (275-320 nm) and UVC (200-275 nm). The UVA has slow and lasting effect, has strong penetrating power which can directly reach the dermis, can damage elastic fibers and collagen fibers to cause skin aging, and can tan the skin; UVB has rapid action on skin, causes skin photosensitive reaction, can cause skin damage such as erythema, inflammation and the like, and is a root cause of skin sunburn; the penetration of UVC is the weakest, only reaches the horny layer of the skin, most of the UVC is blocked by the atmosphere, but the irradiation easily burns the skin, and skin cancer can be caused by long-time irradiation. The sunscreen products on the market at present are various in types, the formula difference is large, the physical sunscreen agent has no irritation to the skin, but the absorption, the air permeability and the transparency are poor, the chemical sunscreen agent has certain irritation to the skin and can possibly cause irritation and allergic reaction of sensitive skin, and meanwhile, part of the chemical sunscreen agent is low in light stability and oxidation resistance and is easy to lose efficacy by photodegradation. In this regard, for preparing sunscreen cosmetics, the safety, stability, and continuous sunscreen ability of the product and sunscreen effect need to be improved.
Plant sunscreens are more and more favored by people due to the characteristics of safety, naturalness, remarkable efficacy and the like, and are also hot spots developed by sunscreen cosmetic producers. The existing research shows that chlorophyll has double sunscreen effects, can absorb and reflect ultraviolet rays at the same time, is one of natural plant sunscreens, contains a porphyrin ring capable of absorbing light in the chlorophyll structure, and a conjugated system of the porphyrin ring can absorb part of visible light, but a complex formed by the porphyrin ring and magnesium ions in the chlorophyll is unstable, so that the chlorophyll copper sodium salt is adopted as a sunscreen component, and the stability of a product is improved. Patent CN 106420471A discloses a skin care product with sun protection and after-sun repair functions and a preparation method thereof, the skin care product is prepared from sodium copper chlorophyllin, cytokine complex liposome, asparagus extract, flos lonicerae extract, ash bark extract, dipotassium glycyrrhizinate, shea butter, butanediol, beta-glucan, sodium hyaluronate, xanthan gum, trehalose, hydrogenated jojoba oil, squalane, cyclopentadimethylsiloxane, cetearyl glucoside, cetearyl alcohol, PEG-100 stearate, tocopheryl acetate, bisabolol, preservative, essence and deionized water, the skin care product has a remarkable sun protection effect and a better protection effect on UVA, but the skin care product as a cytokine with a repair effect cannot be used as a cosmetic raw material according to new regulations, so a new substitute is needed to be found. Patent CN 103211731B discloses a sunscreen skin care product containing chlorophyll, plant extract, sunscreen agent, oil, emulsifier, humectant, deionized water and antibacterial peptide, which improves the sunscreen effect of chlorophyll in combination with physical sunscreen agent and enhances the skin repairing effect, but the problems of poor stability of chlorophyll a and easy decomposition in light are not solved well, and in addition, the oil component and emulsifier content in the formula are high, and the skin feel is heavy and the skin feel is not easy to be smeared to affect the appearance. Patent CN 107854339B discloses a sunscreen skin care cream with high stability and a preparation method thereof, wherein a chlorophyll liposome is prepared from lecithin, tween-80, luo's quercus seed oil, chlorophyll and lutein, the stability of the chlorophyll can be improved by the inclusion of the chlorophyll in the liposome, but the sunscreen effect is not ideal because the chlorophyll and the lutein are hindered due to the inclusion of active substances in the liposome.
In addition, when people pay attention to damage of ultraviolet rays in sunlight to human skins, people also pay attention to damage of blue light in visible light to the skins, compared with the ultraviolet rays, the penetrating power of the blue light is stronger, and unlike the ultraviolet rays, the blue light exists not only in sunlight, but also in a large amount of light emitted by computer displays, televisions, mobile phones, automobile lamps, neon lamps and the like. Through research, mitochondria in cells can generate active oxygen free radicals under long-term blue light irradiation, and the active oxygen free radicals can generate oxidation reaction with the mitochondria, DNA and organelles containing lipid to damage the mitochondria and the DNA, and the blue light can also damage skin barriers, so that the skin is dehydrated, relaxed, and elastic, and the pigmentation and the aging of the skin are accelerated, therefore, the blue light prevention is one of the large research directions of modern skin care products. Chinese patent CN 109939058A discloses a blue-light-proof cosmetic composition which is prepared from citrus extract, lespedeza capitata leaf/stem extract, cerium oxide, flos Buddlejae extract, rhizoma Zingiberis recens rhizoma root extract, and rutin compound. The effect of the nano cerium oxide can keep the balance of circadian rhythm of skin and reduce the oxidative damage of the skin, but the inhalation of the nano cerium oxide can influence the health of respiratory tract and seriously can cause the fibrosis of lung. However, the chlorophyll-containing sunscreen products on the market are mainly protected against ultraviolet UVA and UVB, do not protect against blue light, and have no relevant research on the synergistic effects thereof.
Disclosure of Invention
Based on the above, the invention aims to overcome the defects of the prior art and provide a sunscreen composition and application thereof.
In order to realize the purpose, the technical scheme adopted by the invention is as follows: a sunscreen composition comprises the following components in parts by weight: 0.1-5.5 parts of polyglutamic acid, 2-5 parts of sophora flower extract, 20-40 parts of physical sun-screening agent, 0.5-5 parts of ascorbic acid and/or ascorbic acid derivative and 0.1-0.3 part of sodium copper chlorophyllin; the physical sun-screening agent is at least one of nano titanium dioxide and nano zinc oxide.
The inventor finds that in the practical experimental process, when polyglutamic acid, sophora flower extract, a physical sun-screening agent, ascorbic acid and/or ascorbic acid derivatives and sodium copper chlorophyllin are synergistically acted, the prepared sun-screening composition has good ultraviolet UVA (320-400 nm), UVB (290-320 nm) and good blue light protection effects, and the light protection range of the product is further expanded. In addition, the inventor finds that the compound use of the polyglutamic acid, the ascorbic acid and/or the ascorbic acid derivative not only greatly improves the sun-screening effect, but also greatly contributes to the stability of the sodium copper chlorophyllin. The polyglutamic acid not only has stronger antioxidation in cooperation with ascorbic acid and/or ascorbic acid derivatives, but also has the whitening effect of inhibiting the activity of tyrosinase of the skin, the synergistic ascorbic acid and the derivatives thereof can further improve the stability of sodium copper chlorophyllin, and the chlorophyll chelated by copper ions can be complexed with the polyglutamic acid, so that the antioxidation activity of the tetrapyrrole compound is enhanced, and the repairing effect after sunburn is well promoted. When polyglutamic acid, sophora flower extract, physical sun-screening agent, ascorbic acid and/or ascorbic acid derivative and sodium copper chlorophyllin are synergistically acted, the prepared sun-screening composition is excellent in stability, the appearance of the product is light green after illumination for 30 days, and the product is uniform, fine and unchanged.
Preferably, the sunscreen composition comprises the following components in parts by weight: 1-3 parts of polyglutamic acid, 3-5 parts of sophora flower extract, 25-30 parts of physical sun-screening agent, 1-2 parts of ascorbic acid and/or ascorbic acid derivative and 0.12-0.15 part of sodium copper chlorophyllin.
The inventor finds that when polyglutamic acid, sophora flower extract, physical sunscreen agent, ascorbic acid and/or ascorbic acid derivative and sodium copper chlorophyllin act synergistically, the sunscreen effect and stability of the prepared sunscreen composition are greatly affected by the weight parts of the components, and under the selection of the specific weight parts, the prepared sunscreen composition is excellent in stability, the appearance of the product is light green after illumination for 30 days, and the product is uniform, fine and unchanged; the sun-proof product has a sun-proof index SPF value of more than 40, a PFA value of more than 15 and a PA grade PA + + + +, has a certain absorption and protection effect on light in ultraviolet UVA and UVB wave bands, and also has a blue light resistance effect and a certain absorption and protection effect on blue light with a wavelength of 400-500 nm.
Preferably, the weight average molecular weight of the polyglutamic acid is 70 to 110 ten thousand; the grain diameter D50 of the nano titanium dioxide is 30-100 nm, and the grain diameter D50 of the nano zinc oxide is 10-100 nm.
The inventor finds that the prepared sun-screening composition has proper viscosity and good body feeling when the weight-average molecular weight of the polyglutamic acid is 70-110 ten thousand in the practical experimental process. When the particle diameter D50 of the nano titanium dioxide is 30-100 nm and the particle diameter D50 of the nano zinc oxide is 10-100 nm, the sun-screening effect is better.
Preferably, the ascorbic acid derivative is at least one of sodium ascorbyl phosphate, magnesium ascorbyl phosphate, ascorbyl palmitate, ascorbyl glucoside, ascorbyl tetraisopalmitate and 2-o-ethyl ascorbic acid.
In addition, the invention provides application of the sun-screening composition in sun-screening products and after-sun repair products. Preferably, the sunscreen product is sunscreen emulsion, sunscreen cream, sunscreen base product and the like; the dosage form of the sun-proof product is water-in-oil type, oil-in-water type or full oil type.
Further, the invention provides a sunscreen product comprising the sunscreen composition.
Preferably, the sunscreen product further comprises the following components in parts by weight: 1-30 parts of humectant, 5-40 parts of emollient oil, 0.1-10 parts of emulsifier, 0.1-5 parts of antioxidant and 0.01-3 parts of thickener
The sunscreen product can comprehensively protect the skin from being damaged by ultraviolet and blue light, has better market prospect and economic benefit, and has reasonable formula, simple process and obvious effect.
Preferably, the following (a) to (e):
(a) The humectant is at least one of sodium hyaluronate, glycerol, ethylhexyl glycerol, propylene glycol, dimethiconol, glycerin acrylate/acrylic acid copolymer, butanediol, urea, betaine, dextran, magnesium stearate, polyethylene glycol, sorbitol, 1, 2-hexanediol, caprylyl glycol, panthenol, algae extract, and trehalose;
(b) The emollient oil is at least one of liquid paraffin, petrolatum, hydrogenated polyisobutene, caprylic/capric triglyceride, tri (ethyl acetate) glyceride, cyclopentadimethylsiloxane, cyclohexasiloxane, polydimethylsiloxane, phenyl trimethicone, cetostearyl alcohol, jojoba seed oil, squalane, olive oil, camellia seed oil, hydrogenated coconut oil glyceride, caprylic/capric triglyceride, macadamia nut (MACADAMI atrenifolia) seed oil, MORINGA pterocarpa (MORINGA PTERYGOSPERMA) seed oil, grape (VITIS VINIFERA) seed oil, meadowfoam (LIMNANTHES ALBA) seed oil, hydrogenated sunflower seed oil, and shea butter (butyrosperm PARKII) fruit fat;
(c) The emulsifier is at least one of glyceryl stearate, sorbitan stearate, methylglucose sesquistearate, cetyl PEG/PPG-10/1 polydimethylsiloxane, PEG-10 polydimethylsiloxane, bis-PEG/PPG-14/14 polydimethylsiloxane, polyglyceryl-4 isostearate, sodium acrylate copolymer, lecithin, polyglyceryl-6 polyhydroxystearate, ethylhexyl palmitate, sorbitan isostearate, sorbitan olive oleate, polyacrylate-13, polyisobutylene, polysorbate-20, cetearyl olive oleate, sodium stearoyl glutamate, PEG-40 stearate, sucrose cocoate, C9-15 alcohol phosphate, coco glucoside and butanediol cocoate;
(d) The antioxidant is at least one of tocopherol acetate, rosemary extract, curcumin, coffee cherry and coffee bean extract, astaxanthin, resveratrol, butylated hydroxytoluene, yeast extract, schizosaccharomyces cerevisiae fermentation product lysate, corn oil, GELIDIELLA ACEROSA (GELIDIELLA ACEROSA) extract, wild soybean (GLYCINE SOJA) seed extract, sesame (sesaminum INDICUM) seed oil, alfalfa (mediciago SATIVA) seed powder, chamomile flos (ANTHEMIS NOBILIS) flower extract, white birch (BETULA ALBA) bark/leaf extract, and wild soybean (GLYCINE SOJA) protein;
(e) The thickener is at least one of xanthan gum, carbomer 940, acrylic acid (ester)/C10-C30 alkanol acrylate cross-linked polymer, hydroxyethyl cellulose, microcrystalline wax, dextrin palmitate, magnesium aluminum silicate, silica dimethyl silylate, distearyl dimethyl ammonium hectorite and quaternary ammonium salt-18 hectorite.
Preferably, the sunscreen product further comprises at least one of a fragrance, a preservative, and an efficacy ingredient; the effective component is at least one of boscalid, palmitoyl tripeptide-1, palmitoyl pentapeptide-4, palmitoyl tetrapeptide-7, palmitoyl tripeptide-8, tripeptide-32, acetyl hexapeptide-8, RNA sodium, asiaticoside, bisabolol, phytosphingosine, carnosine, nicotinamide, flos Nymphaeae (NYMHAEA ALBA) extract, and dipotassium glycyrrhizinate.
Preferably, the preservative is at least one of menthone, 1, 2-hexanediol, phenoxyethanol, methyl hydroxybenzoate, butyl hydroxybenzoate, ethyl hydroxybenzoate, propyl hydroxybenzoate and methylisothiazolinone.
In addition, the invention provides a preparation method of the sunscreen product, which comprises the following steps:
(1) Sequentially adding the skin moistening oil, the emulsifier and the physical sun-screening agent into an emulsifying pot, stirring and mixing uniformly, stirring and heating to 75-85 ℃, preserving heat for 10-25 minutes, carrying out homogenizing emulsification at the stirring rotation speed of 2000-3000r/min for 5 minutes, and carrying out vacuum defoaming to obtain a phase A material;
(2) Sequentially adding polyglutamic acid, ascorbic acid and/or derivatives, flos Sophorae Immaturus extract, sodium copper chlorophyllin, humectant, antioxidant and thickener into a water kettle, uniformly stirring and heating to 80-85 deg.C, and keeping the temperature for 10-15 min to obtain B phase material;
(3) Adding the B-phase material into the A-phase material, stirring and homogenizing for 10 minutes, stirring and cooling to 40 ℃, adding the aromatic, the preservative and the functional components, stirring for 20 minutes, cooling to room temperature, sampling and detecting to be qualified, and discharging to obtain the sunscreen product.
Compared with the prior art, the invention has the beneficial effects that: the invention provides a sunscreen composition, when the synergistic effect of polyglutamic acid, sophora flower extract, a physical sunscreen agent, ascorbic acid and/or ascorbic acid derivatives and sodium copper chlorophyllin is realized, the prepared sunscreen composition has good ultraviolet UVA (320-400 nm), UVB (290-320 nm) and blue light protection effects, and the light protection range of the product is further expanded. In addition, the inventor finds that the compound use of the polyglutamic acid and the ascorbic acid and/or the ascorbic acid derivative not only greatly improves the sun-screening effect, but also greatly helps the stability of the sodium copper chlorophyllin, and when the polyglutamic acid, the sophora flower extract, the physical sun-screening agent, the ascorbic acid and/or the ascorbic acid derivative and the sodium copper chlorophyllin act synergistically, the prepared sun-screening composition has excellent stability, the product is still light green in appearance after being illuminated for 30 days, and the product is uniform, fine and unchanged.
Drawings
FIG. 1 is a graph showing the effects of the samples of example 1 and comparative example 4 after being applied to a body surface.
Detailed Description
To better illustrate the objects, technical solutions and advantages of the present invention, the present invention will be further described with reference to the accompanying drawings and specific embodiments. In the examples, the experimental methods used were all conventional methods unless otherwise specified, and the materials, reagents and the like used were commercially available without otherwise specified.
Examples 1 to 6 and comparative examples 1 to 4
The components and parts by weight of the sunscreen product of examples 1-6 and comparative examples 1-4 of the present invention are selected as shown in tables 1 and 2, based on 100 parts by weight; the preparation of a sunscreen product of the examples and comparative examples comprises the following steps:
(1) Sequentially adding emollient oil, emulsifier and physical sun-screening agent into an emulsifying pot, stirring and mixing uniformly, stirring and heating to 80 ℃, keeping the temperature for 20 minutes, homogenizing and emulsifying at the stirring speed of 2500r/min for 5 minutes, and defoaming in vacuum to obtain a phase A material;
(2) Sequentially adding polyglutamic acid, ascorbic acid and/or derivatives, flos Sophorae Immaturus extract, sodium copper chlorophyllin, humectant, antioxidant and thickener into a water kettle, uniformly stirring, heating to 82 deg.C, and keeping the temperature for 15 min to obtain phase B material;
(3) Adding the B phase material into the A phase material, stirring and homogenizing for 10 minutes, stirring and cooling to 40 ℃, adding the aromatic, the preservative and the functional components, stirring for 20 minutes, cooling to room temperature, sampling and detecting to be qualified, and discharging to obtain the sunscreen product.
Table 1: component content (parts by weight) of the sunscreen products provided in examples 1-6 are shown in the table
Figure 226676DEST_PATH_IMAGE001
Figure 49139DEST_PATH_IMAGE002
Table 2: comparative examples 1-4 provide sunscreen products having component contents (parts by weight) shown in the table
Figure 253855DEST_PATH_IMAGE003
Figure 452755DEST_PATH_IMAGE004
The performance tests on the product are shown in runs 1-5.
Test 1: safety test
The test process comprises the following steps: the sunscreen products prepared in examples 1-6 of the present invention were tested for skin irritation and allergy by a homeostatic self-comparison method. 30 volunteers are divided into 6 groups, 5 volunteers are in each group, the composition product is directly smeared on a preparation part of the skin of a volunteer subject and is covered and fixed by dressing, the pasting time is at least 4 hours, a plurality of skin irritation tests are continuously administrated on the same part, the administration time is the same each time, and the skin injury degree in the skin injury test is limited by the injured epidermis layer. The skin reaction was visually observed under natural light or full spectrum light.
The observation time points of the skin irritation test are 30-60min, 24h, 48 h and 72h after the medicament is removed. The skin irritation test was performed several times, and the application was continued after 1 hour of each drug removal.
And (3) test results: the results prove that the product has no irritation, sensitization and other adverse reactions to human bodies.
Test 2: evaluation of sunscreen Effect
The test process comprises the following steps: the Sun Protection effect of a sunscreen product is mainly expressed in terms of the Sun Protection Factor (SPF) value and the PFA (Protection factor of UVA) value. The SPF value is primarily the ability of the sunscreen to protect against mid-wave ultraviolet UVB, while the PFA value is primarily indicative of the ability of the sunscreen to protect against long-wave ultraviolet UVA.
The SPF and PFA values of the sunscreen products of examples 1-6 and comparative examples 1-4, respectively, were determined in the present invention primarily by means of a Sun protection factor tester, wherein the Sun protection factor SPF value is the ratio of the minimum amount of erythema MED required to produce erythema on skin protected with a sunscreen cosmetic to the MED required to produce erythema on unprotected skin. Where MED refers to the lowest dose or minimum time of uv irradiation required to cause a clearly visible erythema of the skin ranging to the majority of the area of the irradiation spot. The higher the SPF value, the greater the skin protection, and the PFA protection is PA +, PA + + +. When the PFA value is less than 2, the UVA protection effect cannot be marked, and when the PFA value is 2-3, PA + is marked; when the PFA value is 4-7, PA + +; when the PFA value is 8-15, PA + + + +; when the PFA value is equal to or greater than 16, PA + + + + +. The more the "+" sign, the better the protection against UVA and the longer the effective protection time.
And (3) test results: as shown in table 3.
Table 3: tables showing the results of evaluating the sunscreen effects of the sunscreen products prepared in examples 1 to 6 and comparative examples 1 to 4
Figure 308585DEST_PATH_IMAGE005
As can be seen from the table, the sunscreen products prepared in the embodiments 1-6 of the present invention have the SPF value of more than 35, the PFA value of more than 10, and the PA + + + grade and above, and have very good sunscreen effects. Comparative examples 1-2 although the parts of the sunscreen composition were the same as in example 1, one of the components was absent and was significantly reduced from the viewpoint of sunscreen effect. Comparative examples 3-4 the parts of the sunscreen composition are outside the specified range of the present invention and are significantly reduced from the viewpoint of sunscreen effect.
Test 3: evaluation of anti-blue light Effect
The test process comprises the following steps: reactive Oxygen Species (ROS) are chemically Reactive Oxygen-containing molecules produced by Oxygen metabolism, including peroxides, superoxides, hydroxyl radicals, singlet Oxygen, and alpha-Oxygen. In the biological context, the formation of ROS plays an important role in cell signaling and homeostasis. The blue light can induce the generation of Reactive Oxygen Species (ROS) and other substances, so that the skin generates oxidative stress to cause skin aging, skin diseases and other problems. According to the method for detecting the active oxygen by using the fluorescent probe, DCFH-DA without fluorescence is hydrolyzed into DCFH after penetrating through cell membranes, the DCFH can not penetrate through the cell membranes, so that the probe can be easily loaded into cells, and ROS generated by induction can be used for producing fluorescent DCF through the DCFH of oxide fluorescence under the irradiation of blue light, so that the generation amount of the ROS in the cells can be reacted through the fluorescence intensity of the DCF.
The experimental steps are as follows: 1) Cell preparation: and (3) performing cell plating one day before detection to ensure that the confluence degree of the cells reaches 50-70% during detection.
2) Inducing a sample: the cell culture solution was removed, and the cells of examples 1-6 and comparative examples 1-4, diluted to working concentration with appropriate buffer or serum-free medium, were incubated at 37 ℃ in a cell culture chamber for an induction time determined according to their characteristics and cell type.
3) Preparing a probe: DCFH-DA was diluted in serum-free medium to a final concentration of 10. Mu.M according to 1.
4) Probe loading: the sample for induction was aspirated and the appropriate volume of diluted DCFH-DA working solution was added.
5) Cell washing: washing the cells for 1 to 2 times by using a serum-free culture solution, and fully removing DCFH-DA which does not enter the cells.
6) The relative fluorescence intensity of the examples 1-6, the comparative examples 1-4 and the blank before and after the blue light irradiation stimulation was measured by a fluorescence spectrophotometer using an excitation wavelength of 488 nm and an emission wavelength of 525 nm.
And (3) test results: as shown in table 4.
Table 4: anti-blue light effect evaluation results of the sunscreen products prepared in examples 1-6 and comparative examples 1-4 and the blank
Figure 301949DEST_PATH_IMAGE006
As can be seen from the above table, the sunscreen products prepared in the embodiments 1-6 of the present invention can effectively reduce the generation amount of ROS, and compared with the blank group, the reduction range is more than 18.6%. Comparative examples 1-2 although the parts of the sunscreen composition were the same as in example 1, one of the components was absent, and the effect of reducing the amount of ROS produced was remarkably reduced. Comparative examples 3 to 4 the number of parts of the sunscreen composition outside the specified range of the present invention was significantly reduced from the effect of reducing the amount of ROS produced.
Test 4: evaluation of stability
The test process comprises the following steps: the products prepared in the examples and the comparative examples are heated in a water bath kettle at 100 ℃ for 30min, the color change condition of the products is observed, the absorbance is measured and recorded, the absorbance value is increased, the stability of the pigment is protected to a certain extent, the change rate of the absorbance value is higher, the stability of the pigment is protected to a better extent, and the calculation method of the change rate is as follows: change rate = (absorbance after heating-absorbance before heating) ÷ absorbance before heating × 100%.
And (3) test results: as shown in table 5.
Table 5: table of evaluation results of stability of sunscreen products prepared in examples 1 to 6 and comparative examples 1 to 4
Figure 993961DEST_PATH_IMAGE007
As can be seen from the above table, the light absorption values of examples 1 to 6 are significantly increased before and after heating, and the amplification is more than 10.7%; the composition has obvious protective effect on the stability of the pigment.
Test 5: sunscreen product and illumination stability test
The test process comprises the following steps: the products prepared in the examples and the comparative examples are placed in the sunlight irradiation place, and after 24h, 7d and 30d, the change of the sample is observed at room temperature to judge the illumination stability of the sample.
And (3) test results: as shown in table 6.
Table 6: the appearance and light stability test results of the sunscreen products prepared in examples 1-6 and comparative examples 1-4 are shown in the table
Figure 730973DEST_PATH_IMAGE008
As can be seen from the above table, the sunscreen products prepared in all the examples of the present invention have uniform and fine appearance, and the tissue morphology of the sunscreen product has no obvious change after the light stability test, which indicates that the sunscreen product provided by the present invention has good stability; wherein the effect of the samples of example 1 and comparative example 4 after being applied on the body surface is shown in fig. 1, the left side [1] of fig. 1 shows that the sample of example 1 is applied, and the right side [2] shows that the sample of comparative example 4 is applied, it can be seen from the figure that comparative example 4 is darker and darker green in color, poor skin feel due to too high content of 2-o-ethyl ascorbic acid, fine skin feel of example 1, and whitish and greenish in color.
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 (8)

1. The sun-screening composition is characterized by comprising the following components in parts by weight: 0.1-5 parts of polyglutamic acid, 2-5.5 parts of sophora flower extract, 20-40 parts of physical sun-screening agent, 0.5-5 parts of ascorbic acid and/or ascorbic acid derivative and 0.1-0.3 part of sodium copper chlorophyllin; the physical sun-screening agent is at least one of nano titanium dioxide and nano zinc oxide;
the weight average molecular weight of the polyglutamic acid is 70-110 ten thousand; the grain diameter D50 of the nano titanium dioxide is 30-100 nm, and the grain diameter D50 of the nano zinc oxide is 10-100 nm.
2. The sunscreen composition of claim 1 comprising the following components in parts by weight: 1-3 parts of polyglutamic acid, 3-5 parts of sophora flower extract, 25-30 parts of physical sun-screening agent, 1-2 parts of ascorbic acid and/or ascorbic acid derivative and 0.12-0.15 part of sodium copper chlorophyllin.
3. Use of a sunscreen composition according to claim 1 or 2 in sunscreen products and after-sun products.
4. A sunscreen product comprising the sunscreen composition of claim 1 or 2.
5. The sunscreen product of claim 4, further comprising the following components in parts by weight: 1-30 parts of humectant, 5-40 parts of emollient grease, 0.1-10 parts of emulsifier, 0.1-5 parts of antioxidant and 0.01-3 parts of thickener.
6. The sunscreen product of claim 5,
the humectant is at least one of sodium hyaluronate, glycerol, ethylhexyl glycerol, propylene glycol, dimethiconol, glycerin acrylate/acrylic acid copolymer, butanediol, urea, betaine, dextran, magnesium stearate, polyethylene glycol, sorbitol, 1, 2-hexanediol, caprylyl glycol, panthenol, algae extract, and trehalose;
the skin moistening oil is at least one of liquid paraffin, petrolatum, hydrogenated polyisobutene, triglyceride (ethyl acetate), cyclopentadimethylsiloxane, cyclohexasiloxane, polydimethylsiloxane, phenyl trimethicone, cetostearyl alcohol, jojoba seed oil, squalane, olive oil, camellia seed oil, hydrogenated coconut oil glycerides, caprylic/capric triglyceride, macadamia nut seed oil, pterocarya pterocarpum seed oil, grape seed oil, meadowfoam seed oil, hydrogenated sunflower seed oil and shea butter;
the emulsifier is at least one of glyceryl stearate, sorbitan stearate, methylglucamine sesquistearate, cetyl PEG/PPG-10/1 polydimethylsiloxane, PEG-10 polydimethylsiloxane, bis-PEG/PPG-14/14 polydimethylsiloxane, polyglyceryl-4 isostearate, acrylic acid (ester) copolymer sodium, lecithin, polyglyceryl-6 polyhydroxystearate, ethylhexyl palmitate, sorbitan isostearate, sorbitan olivate, polyacrylate-13, polyisobutylene, polysorbate-20, cetearyl olivate, sodium stearyl glutamate, PEG-40 stearate, sucrose cocoate, C9-15 alcohol phosphate, coco glucoside and butanediol cocoate;
the antioxidant is at least one of tocopherol acetate, rosemary extract, curcumin, coffee cherokee and coffee bean extract, astaxanthin, resveratrol, butylated hydroxytoluene, yeast extract, schizosaccharomyces cerevisiae fermentation product lysate, corn oil, lithospermum extract, soybean seed extract, sesame seed oil, alfalfa seed powder, chamomile extract, white birch bark/leaf extract and wild soybean protein;
the thickener is at least one of xanthan gum, carbomer 940, acrylic acid (ester)/C10-C30 alkanol acrylate cross-linked polymer, hydroxyethyl cellulose, microcrystalline wax, dextrin palmitate, magnesium aluminum silicate, silica dimethyl silylate, distearyl dimethyl ammonium hectorite and quaternary ammonium salt-18 hectorite.
7. The sunscreen product of any one of claims 4-6, further comprising at least one of a fragrance, a preservative, and a performance ingredient; the functional components are at least one of boscalid, palmitoyl tripeptide-1, palmitoyl pentapeptide-4, palmitoyl tetrapeptide-7, palmitoyl tripeptide-8, tripeptide-32, acetyl hexapeptide-8, RNA sodium, asiaticoside, bisabolol, phytosphingosine, carnosine, nicotinamide, flos Nymphaeae alba extract and dipotassium glycyrrhizinate.
8. A process for the preparation of a sunscreen product as claimed in any one of claims 4 to 6 comprising the steps of:
(1) Sequentially adding skin moistening oil, emulsifier and physical sun-screening agent into an emulsifying pot, stirring and mixing uniformly, stirring and heating to 75-85 deg.C, keeping the temperature for 10-25 min, homogenizing and emulsifying at a stirring speed of 2000-3000r/min for 5min, and vacuum defoaming to obtain phase A material;
(2) Sequentially adding polyglutamic acid, ascorbic acid and/or derivatives, flos Sophorae Immaturus extract, sodium copper chlorophyllin, humectant, antioxidant and thickener into a water kettle, uniformly stirring and heating to 80-85 deg.C, and keeping the temperature for 10-15 min to obtain B phase material;
(3) Adding the B phase material into the A phase material, stirring and homogenizing for 10 minutes, stirring and cooling to 40 ℃, adding the aromatic, the preservative and the functional components, stirring for 20 minutes, cooling to room temperature, sampling and detecting to be qualified, and discharging to obtain the sunscreen product.
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