CN116672279A - Fresh and stable high-multiple sun-screening emulsion and preparation method thereof - Google Patents
Fresh and stable high-multiple sun-screening emulsion and preparation method thereof Download PDFInfo
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- CN116672279A CN116672279A CN202310625258.XA CN202310625258A CN116672279A CN 116672279 A CN116672279 A CN 116672279A CN 202310625258 A CN202310625258 A CN 202310625258A CN 116672279 A CN116672279 A CN 116672279A
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- ZMPFVMSHKCGRFH-UHFFFAOYSA-N hexyl 3-(diethylamino)-2-hydroxybenzoate Chemical compound CCCCCCOC(=O)C1=CC=CC(N(CC)CC)=C1O ZMPFVMSHKCGRFH-UHFFFAOYSA-N 0.000 description 1
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- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
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Classifications
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/49—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
- A61K8/494—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with more than one nitrogen as the only hetero atom
- A61K8/496—Triazoles or their condensed derivatives, e.g. benzotriazoles
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- A—HUMAN NECESSITIES
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- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/27—Zinc; Compounds thereof
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/29—Titanium; Compounds thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/37—Esters of carboxylic acids
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- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/40—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
- A61K8/41—Amines
- A61K8/411—Aromatic amines, i.e. where the amino group is directly linked to the aromatic nucleus
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/49—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
- A61K8/494—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with more than one nitrogen as the only hetero atom
- A61K8/4946—Imidazoles or their condensed derivatives, e.g. benzimidazoles
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics 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
- A61K8/9706—Algae
- A61K8/9711—Phaeophycota or Phaeophyta [brown algae], e.g. Fucus
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q17/00—Barrier 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
- A61Q17/04—Topical preparations for affording protection against sunlight or other radiation; Topical sun tanning preparations
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/59—Mixtures
- A61K2800/592—Mixtures of compounds complementing their respective functions
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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
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Abstract
The application provides fresh and stable high-multiple sun-screening emulsion and a preparation method thereof, wherein the fresh and stable high-multiple sun-screening emulsion comprises chemical sun-screening agent, physical sun-screening agent, emulsifying agent, grease, humectant and deionized water; the chemical sun-screening agent is a combination of ethylhexyl methoxycinnamate, hexyl diethylin hydroxybenzoate and methylene bis-benzotriazole tetramethylbutylphenol. The components selected in the sun-screening emulsion are safe and non-irritating, and the physical sun-screening agent and the chemical sun-screening agent are combined to be used together, so that the skin barrier can be better strengthened, the facial skin can be protected from being affected by effective ultraviolet radiation, further, a remarkable sun-screening effect is achieved, and meanwhile, the grease, the emulsifying agent and the humectant are selected in the components of the sun-screening emulsion, so that the system compatibility is better, and the defending capability of the skin can be further improved.
Description
Technical Field
The application belongs to the field of cosmetics, and particularly relates to a fresh and stable high-multiple sun-screening emulsion and a preparation method thereof.
Background
Ultraviolet rays are important causes for accelerating skin aging, and proper sun-screening measures can effectively delay skin aging, and sun-screening cosmetics on the market at present mainly adopt a physical protection mode, a chemical protection mode or a physical and chemical protection mode to absorb ultraviolet rays. Consumers also tend to use high-fold sunscreen products more and more for better sun protection, so that to obtain high-fold sunscreen products, more and more products can effectively increase the sun protection factor by increasing the amount of sunscreen added to the composition.
CN109498474a discloses a refreshing three-phase emulsified sunscreen cosmetic and a preparation method thereof, wherein the components comprise grease, surfactant, polyalcohol, sunscreen agent, thickener and water. Wherein the grease comprises 7 substances including dioctyl carbonate and isononyl isononanoate, the surfactant comprises 4 substances including PEG-10 polydimethylsiloxane, the polyol comprises 6 substances including glycerin and sorbitol, the sun-screening agent comprises 6 substances including titanium dioxide and octocrylene, and the thickener comprises 3 substances including sodium polyacrylate.
CN108670890a discloses an organic sunscreen composition and application thereof, the organic sunscreen composition is prepared from the following raw materials: ethylhexyl methoxycinnamate, C12-15 alcohol benzoate, isopropyl lauroyl sarcosinate, octocrylene, bis-ethylhexyl oxyphenol methoxyphenyl triazine, octyl polymethylsiloxane, ethylhexyl triazone, hexyl diethylhydroxybenzoate, isodecyl pivalate, butyl methoxydibenzoyl methane. The organic sun-screening composition comprises ultraviolet absorbers with different wave bands, can achieve good sun-screening effect, has the characteristics of good compatibility and high refreshing degree, and can bring pleasant skin feel when comprehensively protecting skin. The organic sunscreen composition can be applied to cosmetics or skin care products, such as various formulations of prepared sun-proof gel, sun-proof spray, sun-proof cream, color cosmetics with sun-proof effect and the like.
However, excessive usage of the sun-screening agent in the product can cause oily skin feel, and on the other hand, the skin can be whitened to influence the sensory experience of the product, so that the sun-screening product with high index and refreshing effect has important market value.
Disclosure of Invention
Aiming at the defects of the prior art, the application aims to provide fresh and stable high-multiple sun-screening emulsion and a preparation method thereof, and the sun-screening emulsion not only can ensure the sun-screening effect of a product, but also can ensure that the product has fresh and non-greasy smearing feeling.
In order to achieve the aim of the application, the application adopts the following technical scheme:
in a first aspect, the application provides a fresh and stable high-multiple sun-screening emulsion, wherein the fresh and stable high-multiple sun-screening emulsion comprises chemical sun-screening agent, physical sun-screening agent, emulsifying agent, grease, humectant and deionized water;
the chemical sun-screening agent is a combination of ethylhexyl methoxycinnamate, hexyl diethylin hydroxybenzoate and methylenebis-benzotriazole tetramethylbutylphenol.
The components selected by the sun-screening emulsion are safe and non-irritating, the physical sun-screening agent and the chemical sun-screening agent are combined, the physical sun-screening agent and the chemical sun-screening agent are matched for use, skin barriers can be better strengthened, facial skin can be protected from being affected by effective ultraviolet radiation, and a remarkable sun-screening effect is achieved.
Preferably, the mass ratio of the ethylhexyl methoxycinnamate, the hexyl diethylaminohydroxybenzoate and the methylenebis-benzotriazole tetramethylbutylphenol is (1-10): 0.2-8): 0.5-10.
Wherein "1-10" may be 1.5, 2, 2.5, 3, 3.5, 4, 4.5, 5, 5.5, 6, 6.5, 7, 7.5, 8.5, 9 or 9.5, etc.;
"0.2-8" may be 0.5, 0.8, 1, 1.5, 2, 2.5, 3, 3.5, 4, 4.5, 5, 5.5, 6, 6.5, 7, 7.5, etc.;
"0.5-10" may be 1, 1.5, 2, 2.5, 3, 3.5, 4, 4.5, 5, 5.5, 6, 6.5, 7, 7.5, 8.5, 9, 9.5, or the like.
Preferably, the physical sunscreens comprise titanium dioxide and/or zinc oxide.
The physical sun-screening agent disclosed by the application is titanium dioxide and/or zinc oxide, and the titanium dioxide and/or zinc oxide have better reflection and scattering effects on ultraviolet rays, so that the effect of shielding ultraviolet rays is achieved.
Preferably, the emulsifier comprises any one or a combination of at least two of PEG-2 stearate, PEG-20 stearate, glycerol stearate, potassium laurylphosphate, sorbitan stearate, polyglycerol-3 isostearate, methyl gluceth-20, isocetyl polyether-20, cetostearyl alcohol or C20-22 alcohol phosphate.
Preferably, the grease comprises any one or a combination of at least two of cyclopentadimethicone, dimethicone, butanediol dicaprylate/dicaprate, neopentyl glycol diheptanoate, oleic acid/linoleic acid/linolenic acid polyglycerol esters, hydroxystearic acid or squalane.
Preferably, the humectant comprises any one or a combination of at least two of 1, 3-propanediol, diglycerol, glucose, 1, 2-hexanediol, sodium hyaluronate or butanediol.
Preferably, the fresh and stable high-fold sun protection milk further comprises a plant sunscreen.
Preferably, the plant sunscreen comprises a laminaria japonica extract and/or ergothioneine.
Preferably, the plant sunscreen is a combination of a laminaria japonica extract and ergothioneine.
As a preferable technical scheme of the application, the kelp wedge-based extract is used as an ultraviolet filter, can improve the tolerance of skin to ultraviolet rays, prevent photoaging, and simultaneously relieve sunburn skin and reduce wrinkles; the ergothioneine can remove free radicals, regulate oxidation-reduction reaction in cells, relieve the damage of ultraviolet rays to skin, participate in intracellular energy regulation and cell physiological protective agents, and can further improve the sun-screening capability of the sun-screening emulsion when being used as a plant sun-screening agent.
Preferably, the mass ratio of the laminaria japonica extract to the ergothioneine is 1 (1-2), and for example, the mass ratio can be 1:1.1, 1:1.2, 1:1.3, 1:1.4, 1:1.5, 1:1.6, 1:1.7, 1:1.8, 1:1.9, and the like.
Preferably, the fresh and stable high-fold sun protection milk further comprises a skin feel modifier.
Preferably, the skin feel modifier comprises any one or a combination of at least two of glycerol polymethacrylate, vinyl polydimethylsiloxane/polymethylsiloxane silsesquioxane cross-linked polymer, or silica.
Preferably, the skin feel modifier comprises a combination of glycerol polymethacrylate, vinyl polydimethylsiloxane/polymethylsiloxane silsesquioxane cross-linked polymer and silica.
As a preferable technical scheme of the application, the skin feel modifier is a combination of glycerol polymethacrylate, vinyl polydimethylsiloxane/polymethylsiloxane silsesquioxane cross-linked polymer and silica, and the three components are used together, so that the system stability of the sun-proof emulsion can be improved, and the fresh and non-greasy experience feel of the product after use can be further enhanced.
Preferably, the mass ratio of the glycerol polymethacrylate, the vinyl polydimethylsiloxane/polymethylsiloxane silsesquioxane cross-linked polymer and the silica is (1-3): 0.5-1.5): 0.1-1.
Wherein "1-3" may be 1.2, 1.5, 1.8, 2, 2.2, 2.5, 2.8, etc.;
"0.5-1.5" may be 0.6, 0.7, 0.8, 0.9, 1, 1.1, 1.2, 1.3, 1.4, 1.5, etc.;
"0.1-1" may be 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, etc.
Preferably, the fresh and stable high-fold sun protection milk further comprises a thickener and/or chelating agent.
Preferably, the thickener comprises a cross-linked polymer of acrylic acid (esters)/vinyl isodecanoate and/or xanthan gum.
Preferably, the chelating agent comprises disodium EDTA.
Preferably, the fresh and stable high-fold sun protection milk further comprises any one or a combination of at least two of a preservative, a pH regulator or a fragrance.
Preferably, the components of the fresh and stable high-multiple sun-screening emulsion comprise, by weight, 1-30 parts of a chemical sun-screening agent, 1-10 parts of a physical sun-screening agent, 1-10 parts of an emulsifying agent, 1-15 parts of grease, 1-15 parts of a humectant and 30-99 parts of deionized water.
The addition amount of the chemical sun-screening agent in the fresh and stable high-multiple sun-screening milk can be 3 parts, 6 parts, 9 parts, 10 parts, 12 parts, 15 parts, 18 parts, 20 parts, 23 parts, 25 parts or 28 parts and the like;
the addition amount of the physical sun-screening agent can be 2 parts, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts or 9 parts and the like;
the addition amount of the emulsifier can be 2 parts, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts or 9 parts, etc.;
the amount of the oil may be 2 parts, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, or the like;
the humectant can be added in an amount of 2 parts, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, 11 parts, 12 parts, 13 parts, 14 parts or the like;
the deionized water may be added in an amount of 35 parts, 40 parts, 45 parts, 50 parts, 55 parts, 60 parts, 65 parts, 70 parts, 75 parts, 80 parts, 85 parts, 90 parts, 95 parts, or the like.
Preferably, the components of the fresh and stable high-multiple sun-screening emulsion comprise, by weight, 1-20 parts of a chemical sun-screening agent, 1-8 parts of a physical sun-screening agent, 1-8 parts of a plant sun-screening agent, 1-8 parts of an emulsifying agent, 1-10 parts of grease, 1-10 parts of a humectant, 1-5 parts of a skin feel regulator, 0.1-1 part of a thickening agent, 0.05-0.2 part of a chelating agent and 30-99 parts of deionized water.
The addition amount of the skin feel modifier in the fresh and stable high-multiple sun-protection milk can be 1.5 parts, 2 parts, 2.5 parts, 3 parts, 3.5 parts, 4 parts or 4.5 parts and the like;
the thickener may be added in an amount of 0.2 parts, 0.3 parts, 0.4 parts, 0.5 parts, 0.6 parts, 0.7 parts, 0.8 parts, 0.9 parts, or the like;
the chelating agent may be added in an amount of 0.06 parts, 0.08 parts, 0.1 parts, 0.12 parts, 0.14 parts, 0.15 parts, 0.17 parts, 0.19 parts, or the like.
Other specific point values in the numerical ranges are selectable, and will not be described in detail herein.
In a second aspect, the application provides a preparation method of the fresh and stable high-multiple sun-screening milk, which comprises the steps of mixing and homogenizing a chemical sun-screening agent, a physical sun-screening agent, an emulsifying agent, grease, a humectant and deionized water to obtain the fresh and stable high-multiple sun-screening milk.
Preferably, the method comprises:
(1) Mixing part of chemical sunscreen agent, emulsifier, oil, part of skin feel regulator, and physical sunscreen agent, heating to 75-85deg.C (such as 75deg.C, 78deg.C, 80deg.C, 82 deg.C or 84deg.C) to obtain phase A;
(2) Mixing chelating agent, thickener, part of humectant, residual skin feel regulator, and half amount of water, heating to 75-85deg.C (such as 75deg.C, 78deg.C, 80deg.C, 82 deg.C or 84deg.C) to obtain phase B;
(3) Mixing the residual chemical sun-screening agent with the residual water to obtain a C phase;
(4) Mixing phase A and phase B, homogenizing, adding phase C, cooling to 45deg.C (such as 25deg.C, 28deg.C, 30deg.C, 32deg.C, 35deg.C or 38deg.C), adding the rest humectant and plant sunscreen agent, mixing, homogenizing to obtain sunscreen emulsion;
the steps (1), (2) and (3) do not distinguish the sequence.
Preferably, the step (4) further comprises adding any one or a combination of at least two of a preservative, a pH regulator or a fragrance after the addition of the plant sunscreen agent.
Other specific point values in the numerical ranges are selectable, and will not be described in detail herein.
Compared with the prior art, the application has the following beneficial effects:
(1) The components selected in the sun-screening emulsion are safe and non-irritating, and the physical sun-screening agent and the chemical sun-screening agent are combined to be used together, so that the skin barrier can be better strengthened, the facial skin can be protected from being affected by effective ultraviolet radiation, further, a remarkable sun-screening effect is achieved, and meanwhile, the grease, the emulsifying agent and the humectant are selected in the components of the sun-screening emulsion, so that the system compatibility is better, and the defending capability of the skin can be further improved.
(2) According to the chemical sun-screening agent, through the matched use of ethylhexyl methoxycinnamate, hexyl diethylin hydroxybenzoyl benzoate and methylene bis-benzotriazole tetramethylbutyl phenol, the three components have a synergistic effect, and the oily feel of sun-screening emulsion can be effectively reduced while high SPF value and PFA value are ensured, so that the product has a fresh and moist skin feel after being used.
(3) The preparation method of the sun-screening emulsion provided by the application is simple, is easy to operate in the production process, does not need complicated instruments and equipment, does not need harsh production conditions, and is easy for industrial production.
Detailed Description
The technical scheme of the application is further described by the following specific embodiments. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the application and are not to be construed as a specific limitation thereof.
The specification information of the partial raw materials involved in the following examples and comparative examples is as follows:
the remaining materials can be used as long as they are purchased from a regular dealer.
Example 1
The embodiment provides a fresh and stable high-multiple sun-protection emulsion, which comprises the following components in percentage by weight:
the preparation method of the fresh and stable high-multiple sun-proof emulsion comprises the following steps:
(1) Mixing potassium laurylphosphate, methyl glucitol polyether-20, isocetyl polyether-20, butanediol dicaprylate/dicaprate, polydimethylsiloxane, ethylhexyl methoxycinnamate, hexyl diethylaminobenzoyl benzoate, titanium dioxide, zinc oxide, vinyl polydimethylsiloxane/polymethylsiloxane silsesquioxane cross-linked polymer and silica, and heating to 80 ℃ to obtain phase A;
(2) Mixing EDTA disodium, acrylic acid (ester) vinyl ester/isodecanoate cross-linked polymer, glycerol polymethacrylate, 1,3 propylene glycol, diglycerol and half amount of water, and heating to 75 ℃ to obtain phase B;
(3) Mixing methylene bis-benzotriazole tetramethyl butyl phenol with the rest of water to obtain a C phase;
(4) Mixing phase A and phase B, homogenizing, adding phase C, cooling to 40deg.C, adding glycerol, herba Zosterae Marinae extract, and ergothioneine, mixing, homogenizing to obtain the sun-screening emulsion.
Example 2
The embodiment provides a fresh and stable high-multiple sun-protection emulsion, which comprises the following components in percentage by weight:
the preparation method of the fresh and stable high-multiple sun-proof emulsion comprises the following steps:
(1) Mixing PEG-2 stearate, PEG-20 stearate, sorbitan stearate, neopentyl glycol diheptanoate, cyclopentadimethicone, ethylhexyl methoxycinnamate, hexyl diethylcarbamoylbenzoate, titanium dioxide, zinc oxide, vinyl dimethicone/polymethylsilicone silsesquioxane cross-linked polymer, and silica, and heating to 75deg.C to obtain phase A;
(2) Mixing EDTA disodium, acrylic acid (esters) vinyl ester/isodecanoate crosslinked polymer, glycerol polymethacrylate, diglycerol, sodium hyaluronate and half of water, and heating to 85deg.C to obtain phase B;
(3) Mixing methylene bis-benzotriazole tetramethyl butyl phenol with the rest of water to obtain a C phase;
(4) Mixing phase A and phase B, homogenizing, adding phase C, cooling to 35deg.C, adding butanediol, herba Zosterae Marinae extract, and ergothioneine, mixing, homogenizing to obtain the sun-screening emulsion.
Example 3
The embodiment provides a fresh and stable high-multiple sun-protection emulsion, which comprises the following components in percentage by weight:
the preparation method of the fresh and stable high-multiple sun-proof emulsion comprises the following steps:
(1) Mixing ethylhexyl methoxycinnamate, diethylin hydroxybenzoyl benzoate, methyl glucitol polyether-20, sorbitan stearate, polyglycerol-3 isostearate, potassium laurylphosphate, squalane, polydimethylsiloxane, butanediol dicaprylate/dicaprate, vinyl polydimethylsiloxane/polymethylsiloxane silsesquioxane cross-linked polymer, silica and titanium dioxide, and heating to 75deg.C to obtain phase A;
(2) Mixing EDTA disodium, acrylic acid (ester) vinyl ester/isodecanoate cross-linked polymer, glycerol polymethacrylate, butanediol and half of water, and heating to 85 ℃ to obtain phase B;
(3) Mixing methylene bis-benzotriazole tetramethyl butyl phenol with water to obtain a C phase;
(4) Mixing phase A and phase B, homogenizing, adding phase C, cooling to 35deg.C, adding glycerol, 1,2 pentanediol, herba Zosterae Marinae extract, and ergothioneine, mixing, homogenizing to obtain the sun-screening emulsion.
Example 4
This example provides a refreshing stable high-fold sun block which differs from example 1 only in that the components do not contain plant sunscreens, the reduction of which is complemented by water, the remaining components remain unchanged, the preparation process being described with reference to example 1.
Example 5
This example provides a refreshing stable high-fold sun block which differs from example 1 only in that the plant sunscreen in the component is 5 parts of the laminaria cuneata extract, the remaining components remain unchanged, the preparation method being described with reference to example 1.
Example 6
This example provides a refreshing stable high-fold sun block which differs from example 1 only in that the plant sunscreen is 5 parts ergothioneine in the component, the remaining components remain unchanged, the preparation method being described with reference to example 1.
Example 7
This example provides a refreshing stable high-fold sun block which differs from example 1 only in that the components do not contain skin feel modifier, the content of which is complemented by water, the remaining components remain unchanged, the preparation method being described with reference to example 1.
Example 8
This example provides a fresh and stable high-fold sun block which differs from example 1 only in that the skin feel modifier does not include glycerol polymethacrylate in the components and the reduced amount of glycerol polymethacrylate is distributed in parts ratio to the vinyl dimethicone/polymethylsilicone silsesquioxane cross polymer and silica, the remaining components remaining unchanged, the preparation method described with reference to example 1.
Example 9
This example provides a fresh and stable high-fold sun block which differs from example 1 only in that the skin feel modifier in the component does not include a vinyl dimethicone/polymethylsilicone silsesquioxane cross polymer and the reduced amount of vinyl dimethicone/polymethylsilicone silsesquioxane cross polymer is apportioned in parts to glycerin polymethacrylate and silica, the remaining components remaining unchanged, the preparation method described with reference to example 1.
Example 10
This example provides a fresh and stable high-fold sun block which differs from example 1 only in that the skin feel modifier does not include silica in the components and the reduced amount of silica is apportioned in parts to the glycerol polymethacrylate and the vinyl dimethicone/dimethicone silsesquioxane cross polymer, the remaining components remaining unchanged, the preparation method described with reference to example 1.
Comparative example 1
This example provides a fresh and stable high-fold sun block which differs from example 1 only in that the components do not contain physical sunscreens, the reduction is complemented by chemical sunscreens, and the proportions of the components of the chemical sunscreens are kept unchanged, the remaining components remain unchanged, the preparation method being as described with reference to example 1.
Comparative example 2
This example provides a fresh and stable high-fold sun block which differs from example 1 only in that the components do not contain chemical sunscreens, the reduction is complemented by physical sunscreens, and the proportions of the components of the physical sunscreens are kept unchanged, the remaining components remain unchanged, the preparation method being as described with reference to example 1.
Comparative example 3
This example provides a refreshing stable high-fold sun block which differs from example 1 only in that the chemical sunscreen in the component does not include ethylhexyl methoxycinnamate, the reduced amounts are distributed in parts ratio to hexyl diethylhydroxybenzoate and methylenebis-benzotriazole tetramethylbutylphenol, the remaining components remaining unchanged, the preparation process described with reference to example 1.
Comparative example 4
This example provides a refreshing stable high-fold sun block which differs from example 1 only in that the chemical sunscreen in the component does not include hexyl diethylhydroxybenzoate, the reduced amount is apportioned in parts to ethylhexyl methoxycinnamate and methylenebis-benzotriazole-tetramethylbutylphenol, the remaining components remaining unchanged, the preparation process described with reference to example 1.
Comparative example 5
This example provides a refreshing stable high-fold sun block which differs from example 1 only in that the chemical sunscreen in the component does not include methylenebis-benzotriazole tetramethylbutylphenol, the reduced amount is apportioned in parts to ethylhexyl methoxycinnamate and hexyl diethylhydroxybenzoate, the remaining components remaining unchanged, the preparation process described with reference to example 1.
Test example 1 evaluation of sunscreening Effect
Evaluation tests of the sunscreen effects on the sunscreen emulsions prepared in examples 1 to 10 and comparative examples 1 to 5 were conducted, and the sunscreen effects of the products were tested according to the method for testing the sun protection index of sunscreen cosmetics (human body method) in the cosmetic safety Specification (2015 edition) using the sun protection index (SPF value) and the sun protection index of long wave ultraviolet (PFA value) of the sunscreen cosmetics as evaluation indexes.
SPF is also known as the sun protection factor, indicating the level of sun protection efficacy that a sunscreen product can perform. The greater the SPF value, the better the protection against UVB. It is determined based on the Minimum Erythema Dose (MED) of the skin. The minimum erythema dose of the skin increases after the sun protection product is used, and the sun protection factor SPF of the sun protection product is as follows:
SPF value = MED for skin protection/MED for unprotected skin using sunscreen cosmetics
PFA is also known as UVA protection index. UVA in sunlight irradiates the skin, and mainly generates physiological effects of skin blackening, wherein the effects are measured by minimum continuous blackening quantity (MPPD), the MPPD is minimum ultraviolet irradiation dose or minimum irradiation time required for generating slight blackening on the skin of the whole irradiation part 2-4 h after irradiation, and PFA of the sun protection product is:
PFA value = MPPD for skin protection using sunscreen cosmetics/MPPD for unprotected skin
The sunscreen effect test results are shown in table 1:
TABLE 1
Sample name | SPF value | PFA value |
Example 1 | 54 | 13 |
Example 2 | 52 | 11 |
Example 3 | 51 | 11 |
Example 4 | 39 | 6 |
Example 5 | 43 | 8 |
Example 6 | 44 | 7 |
Example 7 | 53 | 13 |
Example 8 | 54 | 12 |
Example 9 | 53 | 11 |
Example 10 | 53 | 12 |
Comparative example 1 | 48 | 10 |
Comparative example 2 | 52 | 12 |
Comparative example 3 | 42 | 11 |
Comparative example 4 | 53 | 7 |
Comparative example 5 | 39 | 6 |
As can be seen from Table 1, the SPF value of the sun-screening milk of examples 1-3 is 51-54, and the PFA value is 11-13, which shows that the sun-screening milk of the application has better sun-screening effect; in example 4, the SPF and PFA values of the sun block were reduced in the absence of plant sunscreens; in examples 5-6, the kelp extract and ergothioneine have synergistic effects, and the lack of either one of them reduces the sun protection effect of the sun protection milk; in the case of the comparative examples 1 to 2 lacking a chemical sunscreen agent or a physical sunscreen agent, although the decrease in the sunscreen ability of the sunscreen emulsion is not remarkable, the high addition amount of the chemical sunscreen agent has a strong greasy feel, and the dry feel after absorption is remarkable, which is not conducive to subsequent make-up; however, high levels of physical sunscreens can make the body difficult to spread and the whitening is severe, affecting consumer sensory acceptability. This can be seen in the skin feel evaluation below; as is evident from comparative examples 3-5, the synergistic effect between the components of the chemical sunscreen can be achieved to better increase the sun protection factor of the sunscreen.
Test example 2 evaluation of skin feel
100 healthy female volunteers were selected and randomly divided into 10 groups of 10 persons each, and the sun protection emulsions of examples 1 to 4, 7 to 10 and comparative examples 1 to 2 were tried out, respectively.
Volunteer inclusion criteria: 1) Healthy, without any history of skin disease or systemic disease; 2) The male and female are not limited, and the ages are 18-65 years old; 3) The attitude is serious, and the product can be used continuously; the excluded population is pregnant or lactating women, and sensitive skin.
The using method comprises the following steps: after cleansing, the sun block was used at a concentration of 2mg/cm 2 The coating density is uniformly applied to the face part once a day, and the product is continuously used for 7 days.
The efficacy evaluation method was completed in the form of a questionnaire.
The main evaluation index is as follows:
skin feel index: very dislike (sticky, non-absorbing, heavy, etc., poor spreadability), general (slightly sticky, poor absorbing, general spreadability), very good (no greasy feel, fresh, easy absorbing, good spreadability).
The test results are shown in table 2 by using the preference percentages of the users as a comparison basis.
TABLE 2
From the data in Table 2, the skin feel experience of the sun protection milk of the application in examples 1-3 is better, the volunteer is fresh and free from greasy feel after using, and the use effect of the sun protection milk is better after adding the skin feel modifier as seen in example 7; from examples 8 to 10, it is known that the user satisfaction of the sun-screening milk can be better improved by mutually matching the components in the skin feel modifier; from comparative examples 1-2, it is seen that the skin feel experience of sun-blocks using pure sunscreens or physical sunscreens is relatively poor; in comparative example 1, only the chemical sunscreen agent is an oil-soluble material, and although the oily material can provide a certain moist feeling, the excessive dosage of the chemical sunscreen agent can bring a certain negative effect (such as greasy feeling) to the use feeling of volunteers; in comparative example 2, the sun-screening agent is only a physical sun-screening agent, and most of the physical sun-screening agent is powder, and the powder has certain oil absorption. In the absence of oily sunscreens, the addition of high powders resulted in a dry skin feel and was difficult to spread, thus the skin feel of comparative example 2 was significantly worse than the other examples.
Test example 3 safety evaluation:
the safety test was carried out on the sun protection emulsions prepared in examples 1 to 10 by the following method:
chorioallantoic membrane (CAM) is a respiratory membrane that surrounds the chick embryo. Because the surface blood vessels of the chick embryo allantois are rich and can be regarded as a complete organism, the test utilizes the characteristics of complete, clear and transparent chorioallantoic membrane vascular system in the medium-term chick embryo hatched, a certain amount of test objects are directly contacted with the chick embryo allantois, the change of chorioallantoic membrane toxic effect indexes (such as bleeding, coagulation and vascular thawing) is observed after a specified time of action, the grading is given, and the mathematical average value is calculated for evaluating the irritation of the test objects.
(1) Preparing chicken embryo: fertilized chick embryo of Bai Laihang chick (White Leghorn chicken) and other breeds, wherein the chick embryo weight is 50g-60g, SPF chick embryo is preferably selected to be placed in an incubator for hatching, the temperature is controlled at 37.5+/-0.5 ℃, the relative humidity is 55% -70%, and the egg turning frequency is 3 times/h-6 times/h. And (5) hatching to an 8 th day egg candler for checking by candling, discarding unfertilized and inactive chick embryos, selecting chick embryos with good vascular development, and marking the positions of air chambers on the surfaces of eggshells.
(2) The testing process comprises the following steps: at least 6 chick embryos per group, negative and positive controls were set for each trial. The test was started on day 9. The air chamber eggshell part is carefully stripped by the dental curved forceps, a few drops of physiological saline are dripped on the surface of the eggshell membrane to fully wet the eggshell membrane, and after the eggshell membrane is poured out, the eggshell membrane is carefully removed by the forceps, so that the exposed allantoic membrane is ensured to be intact and not damaged. 0.3ml/0.3g of the test substance was directly applied to the CAM. Coating is carried out as much as possible, and the coverage area is ensured to reach at least 50%. After 3min of action, the CAM surface was gently rinsed with double distilled water, the rinsing was completed within 30s, the liquid was decanted, and immediately the extent of each toxic effect was observed under a stereoscopic microscope, and a score (ES) was given based on capillary bleeding, clotting, and vascular thawing.
(3) And (3) observing results:
bleeding: blood flows from the blood vessels or capillaries of the CAM. And judging 0, 1,2 and 3 points according to no bleeding, mild bleeding, moderate bleeding and severe bleeding.
Coagulation: the protein denaturation inside and outside the blood vessel is manifested by thrombus, tube wall swelling, blood coagulation points inside and outside the blood vessel, opacification turbidity outside the blood vessel, and the like. The blood coagulation was judged to be 0, 1,2 and 3 points based on no blood coagulation, mild blood coagulation, moderate blood coagulation and severe blood coagulation, respectively.
Vascular thawing: refers to vascular ablation on the CAM membrane. And respectively judging 0, 1,2 and 3 points according to the non-vascular thawing, the mild vascular thawing, the moderate vascular thawing and the severe vascular thawing.
(4) Calculation and evaluation of results
The ES average score was calculated according to the following formula and the stimulus classification was judged as shown in table 3.
Table 3 evaluation of results
Endpoint scoring | Irritation classification |
ES≤12 | No/light irritation |
12<ES<16 | Moderate irritation |
ES≥16 | Severe irritation |
The statistics of the test results are shown in table 4 below:
TABLE 4 Table 4
Group of | Irritation evaluation index ES | Irritation classification |
Example 1 | 2 | No/light irritation |
Example 2 | 3 | No/light irritation |
Example 3 | 5 | No/light irritation |
Example 4 | 3 | No/light irritation |
Example 5 | 4 | No/light irritation |
Example 6 | 4 | No/light irritation |
Example 7 | 5 | No/light irritation |
Example 8 | 2 | No/light irritation |
Example 9 | 6 | No/light irritation |
Example 10 | 5 | No/light irritation |
As can be seen from the data in table 4: the sun-proof emulsion obtained by the specific components of the application has no hemolysis phenomenon, and is safe and non-irritating. The product of the application has no adverse reaction to human body and high safety.
The applicant states that the present application is illustrated by the above examples as a refreshing stable high-fold sun block and a method for preparing the same, but the present application is not limited to the above detailed method, i.e. it does not mean that the present application must be carried out depending on the above detailed method. It should be apparent to those skilled in the art that any modification of the present application, equivalent substitution of raw materials for the product of the present application, addition of auxiliary components, selection of specific modes, etc., falls within the scope of the present application and the scope of disclosure.
Claims (10)
1. The fresh and stable high-multiple sun-screening emulsion is characterized in that the fresh and stable high-multiple sun-screening emulsion comprises chemical sun-screening agent, physical sun-screening agent, emulsifying agent, grease, humectant and deionized water;
the chemical sun-screening agent is a combination of ethylhexyl methoxycinnamate, hexyl diethylin hydroxybenzoate and methylenebis-benzotriazole tetramethylbutylphenol.
2. The fresh and stable high-magnification sun protection milk according to claim 1, wherein the mass ratio of ethylhexyl methoxycinnamate, hexyl diethylhydroxybenzoate and methylenebis-benzotriazole-tetramethylbutylphenol is (1-10): 0.2-8): 0.5-10.
3. The fresh stable high-fold sun block according to claim 1 or 2, wherein the physical sunscreens comprise titanium dioxide and/or zinc oxide;
the emulsifier comprises any one or a combination of at least two of PEG-2 stearate, PEG-20 stearate, glycerol stearate, potassium laurylphosphate, sorbitan stearate, polyglycerol-3 isostearate, methyl glucitol polyether-20, isocetyl polyether-20, cetostearyl alcohol or C20-22 alcohol phosphate.
4. A fresh stable high-fold sun emulsion according to any one of claims 1 to 3, wherein the oil comprises any one or a combination of at least two of cyclopentadimethicone, dimethicone, butanediol dicaprylate/dicaprate, neopentyl glycol diheptanoate, oleic acid/linoleic acid/linolenic acid polyglycerol esters, hydroxystearic acid or squalane;
preferably, the humectant comprises any one or a combination of at least two of 1, 3-propanediol, diglycerol, glucose, 1, 2-hexanediol, sodium hyaluronate or butanediol.
5. The fresh stable high-fold sun milk according to any one of claims 1 to 4, further comprising a plant sunscreen agent;
preferably, the plant sunscreen comprises a laminaria japonica extract and/or ergothioneine;
preferably, the plant sunscreen is a combination of a laminaria japonica extract and ergothioneine;
preferably, the mass ratio of the kelp wedge-based extract to the ergothioneine is 1 (1-2).
6. The fresh stable high-fold sun milk according to any one of claims 1 to 5, further comprising a skin feel modifier;
preferably, the skin feel modifier comprises any one or a combination of at least two of glycerol polymethacrylate, vinyl polydimethylsiloxane/polymethylsiloxane silsesquioxane cross-linked polymer or silica;
preferably, the skin feel modifier comprises a combination of glycerol polymethacrylate, vinyl polydimethylsiloxane/polymethylsiloxane silsesquioxane cross-linked polymer and silica;
preferably, the mass ratio of the glycerol polymethacrylate, the vinyl polydimethylsiloxane/polymethylsiloxane silsesquioxane cross-linked polymer and the silica is (1-3): (0.5-1.5): (0.1-1).
7. The fresh stable high-fold sun milk according to any one of claims 1 to 6, further comprising a thickener and/or chelating agent;
preferably, the thickener comprises a cross-linked polymer of acrylic acid (esters) and/or vinyl isodecanoate and/or xanthan gum;
preferably, the chelating agent comprises disodium EDTA;
preferably, the fresh and stable high-fold sun protection milk further comprises any one or a combination of at least two of a preservative, a pH regulator or a fragrance.
8. The fresh stable high-fold sun-protection milk according to any one of claims 1 to 7, wherein the fresh stable high-fold sun-protection milk comprises, by weight, 1 to 30 parts of a chemical sun-protection agent, 1 to 10 parts of a physical sun-protection agent, 1 to 10 parts of an emulsifier, 1 to 15 parts of grease, 1 to 15 parts of a humectant, and 30 to 99 parts of deionized water;
preferably, the components of the fresh and stable high-multiple sun-screening emulsion comprise, by weight, 1-20 parts of a chemical sun-screening agent, 1-8 parts of a physical sun-screening agent, 1-8 parts of a plant sun-screening agent, 1-8 parts of an emulsifying agent, 1-10 parts of grease, 1-10 parts of a humectant, 1-5 parts of a skin feel regulator, 0.1-1 part of a thickening agent, 0.05-0.2 part of a chelating agent and 30-99 parts of deionized water.
9. The method for preparing the fresh and stable high-fold sun-proof milk according to any one of claims 1 to 8, wherein the preparation method comprises the steps of mixing and homogenizing a chemical sun-proof agent, a physical sun-proof agent, an emulsifying agent, grease, a humectant and deionized water to obtain the fresh and stable high-fold sun-proof milk.
10. The method for preparing a fresh and stable high-fold sun protection milk according to claim 9, characterized in that it comprises:
(1) Mixing part of chemical sunscreen agent, emulsifier, oil, part of skin feel regulator and physical sunscreen agent, heating to 75-85deg.C to obtain phase A;
(2) Mixing chelating agent, thickener, partial humectant, residual skin feel regulator and half of water, heating to 75-85deg.C to obtain phase B;
(3) Mixing the residual chemical sun-screening agent with the residual water to obtain a C phase;
(4) Mixing phase A and phase B, homogenizing, adding phase C, cooling to 45deg.C, adding the rest humectant and plant sunscreen agent, mixing, and homogenizing to obtain sunscreen emulsion;
the steps (1), (2) and (3) do not distinguish the sequence;
preferably, the step (4) further comprises adding any one or a combination of at least two of a preservative, a pH regulator or a fragrance after the addition of the plant sunscreen agent.
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CN117598932B (en) * | 2023-11-29 | 2024-05-10 | 追光生物科技有限公司 | Sun-screening synergistic composition, water-in-oil type high-power sun-screening composition and preparation method thereof |
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