CN113730269B - Mild gel with sun-screening effect and preparation method thereof - Google Patents

Mild gel with sun-screening effect and preparation method thereof Download PDF

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CN113730269B
CN113730269B CN202111156152.7A CN202111156152A CN113730269B CN 113730269 B CN113730269 B CN 113730269B CN 202111156152 A CN202111156152 A CN 202111156152A CN 113730269 B CN113730269 B CN 113730269B
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gel
skin feel
phase
sun
stirring
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CN113730269A (en
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陈佳龄
孟潇
陈庆生
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Guangzhou Huanya Cosmetic Science and Technology Co Ltd
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Guangzhou Huanya Cosmetic Science and Technology Co Ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/04Dispersions; Emulsions
    • A61K8/042Gels
    • 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
    • A61K8/25Silicon; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/34Alcohols
    • A61K8/345Alcohols containing more than one hydroxy group
    • 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
    • A61K8/37Esters of carboxylic acids
    • 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
    • A61K8/40Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
    • A61K8/41Amines
    • A61K8/411Aromatic amines, i.e. where the amino group is directly linked to the aromatic nucleus
    • 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
    • A61K8/494Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with more than one nitrogen as the only hetero atom
    • A61K8/4966Triazines or their condensed 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
    • A61K8/30Cosmetics 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
    • A61K8/585Organosilicon compounds
    • 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
    • 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
    • A61K8/89Polysiloxanes
    • A61K8/891Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone
    • 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
    • A61K8/89Polysiloxanes
    • A61K8/895Polysiloxanes containing silicon bound to unsaturated aliphatic groups, e.g. vinyl dimethicone
    • 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
    • A61K2800/20Chemical, physico-chemical or functional or structural properties of the composition as a whole
    • A61K2800/30Characterized by the absence of a particular group of ingredients
    • 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

Abstract

The invention belongs to the technical field of cosmetics and discloses a mild sunscreen gel and a preparation method thereof. The gel comprises the following components: sunscreens, silicone elastomers and skin feel modifiers; the silicone elastomer accounts for 20-65% of the gel by mass, and the skin feel modifier accounts for 2-25% of the gel by mass; and the gel does not contain preservatives and surfactants. The gel contains the sun-screening agent, the organic silicon elastomer and the skin feel regulator, the content of the organic silicon elastomer and the skin feel regulator is controlled, and under the condition that the gel does not contain preservatives and surfactants, the gel is mild and non-irritant, the skin feel is fresh and cool and not sticky, the gel has good system stability and excellent sun-screening effect, the SPF can reach 51, and the PFA can reach 17; meanwhile, the preparation method is simple, does not need an emulsification step, and can be prepared by simple heating and mixing steps.

Description

Mild gel with sun-screening effect and preparation method thereof
Technical Field
The invention belongs to the technical field of cosmetics, and particularly relates to a mild sunscreen gel and a preparation method thereof.
Background
Scientific research proves that the excessive irradiation of ultraviolet rays can damage the immune system of a human body, cause sunburn and suntan of the skin, accelerate the aging of the skin and cause various skin diseases and even skin cancer. The use of sunscreen products to prevent sunburn, tanning and aging has become a common recognition. As the sun-screening products gradually become necessary daily products, people have increasing appeal to the sun-screening products, and the sun-screening products are mild and safe, have high sun-screening index, are waterproof and sweat-resistant, and have good skin feel and use feel as the basic selection standards.
The sun protection gels on the market today mainly have two types: the sun protection oil gel of the water-in-oil system and the sun protection hydrogel of the oil-in-water system have higher sun protection index and better waterproof and sweat-resistant performance, but the skin feel is oily, sticky and has certain irritation.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art described above. Therefore, compared with the traditional sun-screening oil gel, the gel provided by the invention is fresh and cool in skin feel and is not sticky.
In a first aspect of the invention, there is provided a mild sunscreen gel comprising the following components: sunscreens, silicone elastomers and skin feel modifiers; the silicone elastomer accounts for 20-65% of the gel by mass, and the skin feel modifier accounts for 2-25% of the gel by mass; and the gel is free of preservatives and surfactants.
The preservative-free agent does not contain conventional preservatives in the field such as phenoxyethanol, methyl p-hydroxybenzoate, glyceryl caprylate, methylisothiazolinone or imidazolidinyl urea and the like; the absence of surfactant in the present invention means that the surfactant is conventional in the art, such as lecithin, PEG-10 polydimethylsiloxane, isododecane/polydimethylsiloxane/diisobutyl PPG-20 crosspolymer, etc.
The gel with the sun-screening effect is a sun-screening oil gel of a water-in-oil system, contains a sun-screening agent, an organic silicon elastomer and a skin-feel regulator, and controls the content of the organic silicon elastomer and the skin-feel regulator, meanwhile, the gel does not contain a preservative and a surfactant, the preservative is a factor causing skin allergy, and the surfactant can also influence the mildness of the product, so the gel is mild and non-irritant, the skin feel is fresh and cool without being sticky, and the gel has good sun-screening effect, the SPF (sun-screening factor) can reach 51, and the PFA (ultraviolet A protection index) can reach 17. The traditional sun protection oil gel is usually added with a surfactant and a preservative, if the surfactant is not added, the product system is unstable, and the surfactant has certain irritation, so that the product mildness is influenced. How to avoid the stimulation of the surfactant and still keep the good stability of a product system on the basis of not adding the surfactant is very difficult for a person skilled in the art. The sunscreen oil gel disclosed by the invention still has good system stability on the basis of not containing a surfactant by adjusting the contents of the organic silicon elastomer and the skin feel regulator, and meanwhile, the skin feel is fresh and not sticky.
The gel disclosed by the invention has the advantages that pores are hidden after the gel is used, so that fine lines of skin are smoothed immediately, and the effects of skin beautification are achieved; the emulsion can also be used as a sun-screening makeup isolation emulsion before makeup, so that fine lines are smoothed, the fitting degree and the makeup effect of a subsequent makeup product are improved, and the subsequent makeup and mud rubbing cannot be caused.
Preferably, the silicone elastomer accounts for 20-40% of the gel by mass, and the skin feel modifier accounts for 16-25% of the gel by mass.
Preferably, the gel further comprises a polyol, a peony extract, a peppermint extract and an oil.
According to the gel, the peony extract and the mentha piperita extract are added, the peony extract is preferably peony flower water, the mentha piperita extract is preferably mentha piperita leaf water, and the peony flower water and the mentha piperita leaf water have synergistic effects, so that the capability of resisting light injury of skin can be remarkably improved, and the sun-screening effect can be remarkably improved.
Preferably, the gel comprises the following components in percentage by mass: 16-21% of sun-screening agent, 20-40% of organic silicon elastomer, 16-25% of skin feel regulator, 1-10% of polyalcohol, 0.5-1% of peony extract, 0.5-1% of peppermint extract and 10-30% of grease.
Preferably, the sunscreen comprises at least two of bis-ethylhexyloxyphenol methoxyphenyl triazine, diethylamino hydroxybenzoyl hexyl benzoate, ethylhexyl triazone, polysiloxane-15, ethylhexyl salicylate, isoamyl p-methoxycinnamate, ethylhexyl methoxycinnamate.
The invention preferably uses chemical sunscreens, which can achieve higher sun protection indices than physical sunscreens such as titanium dioxide and zinc oxide, without the problems of whitening and heavy skin feel.
Preferably, the silicone elastomer comprises at least one of dimethicone/vinyl dimethicone crosspolymer/cyclopentadimethicone, dimethicone/vinyl dimethicone crosspolymer/dimethicone.
Preferably, the skin feel modifier comprises at least one of silica, methyl methacrylate crosspolymer, polymethylsilsesquioxane, vinyl dimethicone/polymethylsilsesquioxane crosspolymer, dimethicone/vinyl dimethicone crosspolymer/silica.
Preferably, the polyhydric alcohol comprises at least one of glycerol, butylene glycol, propylene glycol, dipropylene glycol, sorbitol, 1, 2-pentanediol, 1, 3-propanediol, 1, 2-hexanediol.
Preferably, the grease comprises at least one of dioctyl carbonate, C12-15 alcohol benzoate, isohexadecane, isododecane, undecane/tridecane, phenyl trimethicone, octyl methicone, polydimethylsiloxane, isononyl isononanoate, butanediol dicaprylate/dicaprate, and butyl octanol salicylate.
The second aspect of the present invention provides a preparation method of the mild sunscreen gel, which comprises the following steps:
and mixing the components to prepare the mild sunscreen gel.
Preferably, the preparation method specifically comprises the following steps:
putting the sun-screening agent and the grease into an oil phase pot, heating to 75-85 ℃, uniformly stirring and dispersing, and cooling to 30-40 ℃ to obtain a phase A;
putting the organic silicon elastomer into an emulsifying pot, uniformly stirring and dispersing, slowly pumping the phase A into the emulsifying pot, stirring for 15-20min, putting the skin feel regulator into the emulsifying pot, and stirring for 5-10min to obtain a phase B;
mixing the peony extract, the peppermint extract and the polyhydric alcohol, uniformly dispersing, adding into the emulsifying pot, stirring for 5-10min, vacuumizing and defoaming, discharging at 30-40 ℃, and standing to obtain the mild sunscreen gel.
Preferably, the peony extract is peony water, and the mentha piperita extract is mentha piperita leaf water; the preparation method of the peony flower water or the peppermint leaf water comprises the following steps:
1) drying plant materials (peony or peppermint leaf), pulverizing, and sieving with 80-200 mesh sieve to obtain plant coarse powder;
2) mixing the plant coarse powder with deionized water according to the mass ratio of 1 (5-10), and soaking at 55-65 ℃ for 60-90 minutes to obtain an extracting solution;
3) filtering the extracting solution by adopting a 0.22-micron microfiltration membrane, performing rotary evaporation concentration, freeze-drying, then adding deionized water according to the mass ratio of 1 (1-3), and stirring and dispersing uniformly to obtain the peony flower water or the peppermint leaf water.
Compared with the prior art, the invention has the following beneficial effects:
the gel disclosed by the invention contains the sunscreen agent, the organic silicon elastomer and the skin feel regulator, the content of the organic silicon elastomer and the skin feel regulator is controlled, and the gel does not contain a preservative and a surfactant, so that the gel is mild and non-irritant, the skin feel is fresh and cool without being sticky, the gel has good system stability and excellent sunscreen effect, the SPF can reach 51, and the PFA can reach 17.
The preparation method of the gel is simple, does not need an emulsification step, and can be prepared by simple heating and mixing steps.
Detailed Description
In order to make the technical solutions of the present invention more apparent to those skilled in the art, the following examples are given for illustration. It should be noted that the following examples are not intended to limit the scope of the claimed invention.
The starting materials, reagents or apparatuses used in the following examples are conventionally commercially available or can be obtained by conventionally known methods, unless otherwise specified.
Example 1
A mild sunscreen gel has the components shown in Table 1.
TABLE 1
Figure BDA0003287727200000041
Figure BDA0003287727200000051
The preparation method of the peony flower water or the peppermint leaf water comprises the following steps:
1) drying plant materials (peony or peppermint leaf), pulverizing, and sieving with 80 mesh sieve to obtain plant coarse powder;
2) mixing the plant coarse powder and deionized water according to the mass ratio of 1:5, and soaking for 60 minutes at 60 ℃ to obtain an extracting solution;
3) filtering the extracting solution by adopting a 0.22-micron microfiltration membrane, performing rotary evaporation concentration, freeze-drying, adding deionized water according to the mass ratio of 1:3, and uniformly stirring and dispersing to obtain the peony flower water or the peppermint leaf water.
The preparation method of the gel of the embodiment comprises the following steps:
1) dispersing cosmetic additives with polyalcohol uniformly in advance;
2) adding sunscreen agent and oil into oil phase pan, heating to 80 deg.C, stirring, dispersing, and cooling to 30 deg.C to obtain phase A;
3) putting the organic silicon elastomer into an emulsifying pot, keeping the temperature at 30 ℃, stirring and dispersing uniformly, slowly pumping the phase A into the emulsifying pot at a constant speed, stirring for 20 minutes, putting the skin feel regulator into the emulsifying pot, and stirring for 10 minutes to obtain a phase B;
4) adding the cosmetic additive and the polyalcohol dispersed in the step 1) into an emulsifying pot, stirring for 10 minutes, vacuumizing and defoaming, discharging at 30 ℃, and standing to obtain gel.
Example 2
A mild sunscreen gel having the composition shown in Table 2.
TABLE 2
Figure BDA0003287727200000052
Figure BDA0003287727200000061
The preparation method of the peony flower water or the peppermint leaf water comprises the following steps:
1) drying plant materials (peony or peppermint leaf), pulverizing, and sieving with 100 mesh sieve to obtain plant coarse powder;
2) mixing the plant coarse powder and deionized water according to the mass ratio of 1:8, and soaking for 70 minutes at 60 ℃ to obtain an extracting solution;
3) filtering the extracting solution by adopting a microfiltration membrane of 0.22 mu m, performing rotary evaporation concentration, freeze drying, adding deionized water according to the mass ratio of 1:2, and uniformly stirring and dispersing to obtain the peony water or the peppermint leaf water.
The preparation method of the gel of the embodiment comprises the following steps:
1) dispersing cosmetic additives with polyalcohol uniformly in advance;
2) adding sunscreen agent and oil into oil phase pan, heating to 75 deg.C, stirring, dispersing, and cooling to 35 deg.C to obtain phase A;
3) putting the organic silicon elastomer into an emulsifying pot, keeping the temperature at 35 ℃, stirring and dispersing uniformly, slowly pumping the phase A into the emulsifying pot at a constant speed, stirring for 15 minutes, putting the skin feel regulator into the emulsifying pot, and stirring for 5 minutes to obtain a phase B;
4) adding the cosmetic additive and the polyalcohol dispersed in the step 1) into an emulsifying pot, stirring for 8 minutes, vacuumizing and defoaming, discharging at 35 ℃, and standing to obtain gel.
Example 3
A mild sunscreen gel having the composition shown in Table 3.
TABLE 3
Figure BDA0003287727200000071
The preparation method of the peony flower water or the peppermint leaf water comprises the following steps:
1) drying plant materials (peony or peppermint leaf), pulverizing, and sieving with 200 mesh sieve to obtain plant coarse powder;
2) mixing the plant coarse powder and deionized water according to the mass ratio of 1:10, and soaking for 90 minutes at 65 ℃ to obtain an extracting solution;
3) filtering the extracting solution by adopting a 0.22-micron microfiltration membrane, performing rotary evaporation concentration, freeze-drying, adding deionized water according to the mass ratio of 1:1, and uniformly stirring and dispersing to obtain the peony water or the peppermint leaf water.
The preparation method of the gel of the embodiment comprises the following steps:
1) dispersing cosmetic additives with polyalcohol uniformly in advance;
2) adding sunscreen agent and oil into oil phase pan, heating to 85 deg.C, stirring, dispersing, and cooling to 40 deg.C to obtain phase A;
3) putting the organic silicon elastomer into an emulsifying pot, keeping the temperature at 40 ℃, stirring and dispersing uniformly, slowly pumping the phase A into the emulsifying pot at a constant speed, stirring for 15 minutes, putting the skin feel regulator into the emulsifying pot, and stirring for 10 minutes to obtain a phase B;
4) adding the cosmetic additive and the polyalcohol dispersed in the step 1) into an emulsifying pot, stirring for 5 minutes, vacuumizing and defoaming, discharging at 40 ℃, and standing to obtain gel.
Example 4
A mild sunscreen gel having the composition shown in Table 4.
TABLE 4
Figure BDA0003287727200000081
Figure BDA0003287727200000091
The preparation method of the peony flower water or the peppermint leaf water comprises the following steps:
1) drying plant materials (peony or peppermint leaf), pulverizing, and sieving with 100 mesh sieve to obtain plant coarse powder;
2) mixing the plant coarse powder and deionized water according to the mass ratio of 1:7, and soaking for 80 minutes at 60 ℃ to obtain an extracting solution;
3) filtering the extracting solution by adopting a microfiltration membrane of 0.22 mu m, performing rotary evaporation concentration, freeze drying, adding deionized water according to the mass ratio of 1:2, and uniformly stirring and dispersing to obtain the peony water or the peppermint leaf water.
The preparation method of the gel of the embodiment comprises the following steps:
1) dispersing cosmetic additives with polyalcohol uniformly in advance;
2) adding sunscreen agent and oil into oil phase pan, heating to 80 deg.C, stirring, dispersing, and cooling to 32 deg.C to obtain phase A;
3) putting the organic silicon elastomer into an emulsifying pot, keeping the temperature at 32 ℃, stirring and dispersing uniformly, slowly pumping the phase A into the emulsifying pot at a constant speed, stirring for 20 minutes, putting the skin feel regulator into the emulsifying pot, and stirring for 8 minutes to obtain a phase B;
4) adding the cosmetic additive and the polyalcohol dispersed in the step 1) into an emulsifying pot, stirring for 8 minutes, vacuumizing and defoaming, discharging at 32 ℃, and standing to obtain gel.
Example 5
A mild sunscreen gel having the composition shown in Table 5.
TABLE 5
Figure BDA0003287727200000092
Figure BDA0003287727200000101
The preparation method of the peony flower water or the peppermint leaf water comprises the following steps:
1) drying plant materials (peony or peppermint leaf), pulverizing, and sieving with 100 mesh sieve to obtain plant coarse powder;
2) mixing the plant coarse powder and deionized water according to the mass ratio of 1:8, and soaking for 70 minutes at 55 ℃ to obtain an extracting solution;
3) filtering the extracting solution by adopting a microfiltration membrane of 0.22 mu m, performing rotary evaporation concentration, freeze drying, adding deionized water according to the mass ratio of 1:2, and uniformly stirring and dispersing to obtain the peony water or the peppermint leaf water.
The preparation method of the gel of the embodiment comprises the following steps:
1) dispersing cosmetic additives with polyalcohol uniformly in advance;
2) adding sunscreen agent and oil into oil phase pan, heating to 80 deg.C, stirring, dispersing, and cooling to 30 deg.C to obtain phase A;
3) putting the organic silicon elastomer into an emulsifying pot, keeping the temperature at 30 ℃, stirring and dispersing uniformly, slowly pumping the phase A into the emulsifying pot at a constant speed, stirring for 18 minutes, putting the skin feel regulator into the emulsifying pot, and stirring for 10 minutes to obtain a phase B;
4) adding the cosmetic additive and the polyalcohol dispersed in the step 1) into an emulsifying pot, stirring for 8 minutes, vacuumizing and defoaming, discharging at 30 ℃, and standing to obtain gel.
Example 6
The difference from the example 2 is that the peony flower water and the peppermint leaf water are not contained, the difference is supplemented by the polyhydric alcohol, and the other components and the preparation method are the same as the example 2.
Example 7
The difference from the example 2 is that the peony flower water is not contained, the difference is supplemented by the polyhydric alcohol, and the other components and the preparation method are the same as the example 2.
Example 8
The difference from the example 2 is that the peppermint leaf water is not contained, the difference is supplemented by the polyhydric alcohol, and the other components and the preparation method are the same as the example 2.
Example 9
The difference from the example 2 is that the peony flower water is replaced by the rose flower water with similar efficacy, and other components and the preparation method are the same as the example 2.
Example 10
The difference from the example 2 is that the peppermint leaf water is replaced by rosemary leaf water with similar efficacy, and other components and the preparation method are the same as the example 2.
Comparative example 1
The difference from example 3 is that the content of silicone elastomer is 15 wt%, the missing content is supplemented by grease, and other components and preparation method are the same as example 3.
Comparative example 2
The difference from example 4 is that the content of the silicone elastomer is 70 wt%, the excess content is reduced from grease, and other components and preparation method are the same as example 4.
Comparative example 3
The difference from example 3 is that the content of the skin feel modifier is 30 wt%, the excess content is reduced from the amount of the grease, and other components and the preparation method are the same as example 3.
Comparative example 4
The difference from example 4 is that the content of the skin feel modifier is 1 wt%, the lack of the content is supplemented by the oil, and other components and the preparation method are the same as example 4.
Comparative example 5
The difference from example 3 is that a preservative and a surfactant were contained, and the components of this comparative example are shown in table 6.
TABLE 6
Figure BDA0003287727200000121
The preparation method of the comparative example gel comprises the following steps:
1) dispersing cosmetic additives with polyalcohol uniformly in advance;
2) adding sunscreen agent, oil and surfactant into oil phase pan, heating to 85 deg.C, stirring, dispersing, and cooling to 40 deg.C to obtain phase A;
3) putting the organic silicon elastomer into an emulsifying pot, keeping the temperature at 40 ℃, stirring and dispersing uniformly, slowly pumping the phase A into the emulsifying pot at a constant speed, stirring for 15 minutes, putting the skin feel regulator into the emulsifying pot, and stirring for 10 minutes to obtain a phase B;
4) adding the cosmetic additive, the polyalcohol and the preservative which are dispersed in the step 1) into an emulsifying pot, stirring for 5 minutes, vacuumizing and defoaming, discharging at 40 ℃, and standing to obtain gel.
Comparative example 6
The comparative example is a conventional sunscreen gel having the components shown in table 7.
TABLE 7
Figure BDA0003287727200000131
Figure BDA0003287727200000141
The preparation method of the comparative gel comprises the following steps:
1) adding a surfactant into a humectant, stirring at normal temperature to dissolve uniformly to serve as a water phase for later use;
2) heating and dissolving the organic sun-screening agent and the grease uniformly, and cooling to room temperature to be used as an oil phase for later use;
3) slowly adding the oil phase into the water phase at a constant speed under the conditions of normal temperature and stirring until the oil phase and the water phase are uniformly mixed;
4) slowly adding deionized water into the paste at a constant speed under the conditions of normal temperature and stirring until the paste is transparent and uniform;
5) and adding the rest components in the formula into the paste, and performing vacuum defoaming to prepare the sunscreen oil gel.
Test example 1 System stability test
The examples 1 to 10 and comparative examples 1 to 4 were subjected to stability tests, and 30mL of each sample was placed in a transparent sealed vial, and the stability was observed after 30 days at-15, 25, 40 and 48 ℃ and the results are shown in Table 8.
TABLE 8
Figure BDA0003287727200000142
Figure BDA0003287727200000151
From the test results in table 8, it can be seen that comparative examples 1-4 show the instability of the system, etc., indicating that the silicone elastomer and skin feel modifier are stable only within the limits of the present invention without the addition of surfactant.
Test example 2 Patch test
The products of examples 1-5 were selected as test samples and used as blank controls to test their potential for causing adverse skin reactions in humans.
The test was carried out according to the method of technical Specification for safety of cosmetics (2015 edition) -test for skin spots on human body. 30 volunteers 18-60 years old who meet the requirements of the test were selected as subjects (15 each for male and female). The sample (test substance) is added into a spot tester in an amount of 0.020-0.025 g. Control wells were blank (without any material). The spot test device with the tested object is applied to the flexed side of the forearm of the tested object by using a non-irritating adhesive tape, and is lightly pressed by hands and palms to be uniformly applied to the skin. The test site is marked for easy observation. The patch is applied every 24h, 30min after the patch is uncovered, and skin reaction is observed after the indentation disappears. If the reaction is suspicious or positive, stopping the spot test of the subject; if the reaction is negative, the spot-pasting test is continuously carried out on the same tested part of the subject, and the spot-pasting test is repeatedly carried out for 6 times. The test population response results are recorded as in table 9. The test results are shown in table 10.
TABLE 9 grading Standard of adverse skin reactions
Grade of (symbol) Identification criteria
0 - Negative reaction: has no irritation and erythema
1 ± And (3) suspicious reaction: mild erythema
2 + Weak positive reaction: erythema
3 ++ Strong positive reaction: erythema, papules, blisters
4 +++ Extremely strong positive reaction: severe edema and bulla
TABLE 10 Patch test results
Figure BDA0003287727200000152
Figure BDA0003287727200000161
As can be seen from Table 10, the sunscreen oil gel prepared by the present invention has no allergy or irritation to the skin, indicating that the sunscreen oil gel of the present invention has good mildness.
Test example 3 sunscreen Effect human body test
(1) Sun Protection Factor (SPF): also known as the solar protection factor, indicates how high the sunscreen product can exert the sunscreen effect. The larger the SPF value, the better the sunscreen effect. It is determined based on the Minimum Erythemal Dose (MED) of the skin. When the sunscreen is used, the minimum erythema dose of the skin increases, and the sun protection factor SPF of the sunscreen is:
Figure BDA0003287727200000162
the SPF index is useful for evaluating the protection against UVB.
(2) Long-wave ultraviolet protection index (PFA value) of sunscreen cosmetic: also known as the UVA protection index. UVA in sunlight strikes the skin, primarily producing the physiological effects of skin darkening, measured as the minimum sustained amount of darkening (MPPD). MPPD is the minimum ultraviolet irradiation dose or the minimum irradiation time required for 2-4h after irradiation to produce slight blackening on the skin at the whole irradiation site.
Figure BDA0003287727200000163
The sunscreen effectiveness test was not performed because the product systems prepared in comparative examples 1-4 were unstable. The products of examples 1-10 were selected as test samples and tested for sunscreen efficacy according to the sunscreen cosmetic sun protection index test method (human method) in technical Specification for cosmetic safety (2015 edition), the test results are shown in Table 11.
TABLE 11
Figure BDA0003287727200000164
Figure BDA0003287727200000171
As can be seen from Table 11, the SPF values of examples 1-5 were 46 or more, the PFA values were 14 or more, the SPF values of examples 1, 4 and 5 were 50 or more, and the PFA values were 16 or more, indicating that the sunscreen oil gels of the present invention have excellent sunscreen effects. The SPF value and the PFA value of example 2 are obviously higher than those of examples 6-10, and the sun-screening effect of examples 6-10 is obviously poor because the peony flower water and the peppermint leaf water are not added, or only single peony flower water or peppermint leaf water is added, or the peony flower water or peppermint leaf water is replaced by other substances with similar efficacy, so that the peony flower water and peppermint leaf water have a synergistic effect and can obviously improve the sun-screening effect.
Test example 4 test of UV damage resistance
Scientific studies have shown that, following UV irradiation, the transdermal Water Loss (TEW L) of the skin increases, the barrier function is impaired and the skin becomes dry. The samples prepared in example 2 and examples 7-10 were selected as test samples for testing, and example 6 was used as a blank sample.
Selecting 30 volunteers 23-34 years old for human body test, firstly selecting skin at thigh parts for testing TEWL, then respectively using a test sample and a blank control sample twice a day, once in the morning and at noon, using 15d, carrying out full spectrum irradiation on the thigh skin for 6h according to the lowest erythema dose of the volunteer skin, testing the TEWL, taking the blank control as a reference, and calculating the TEWL rising value reduction rate according to the formula (1), wherein the results are shown in Table 12.
The TEWL rise decrease rate (%) - (difference in TEWL values in blank sample-difference in TEWL values in test sample)/difference in TEWL values in blank sample X100% (1)
TABLE 12
Experimental group TEWL rise decrease rate (%)
Example 2 78.4
Example 7 31.9
Example 8 37.7
Example 9 58.3
Example 10 59.6
As can be seen from table 12, the TEWL increase reduction rate of example 2 is significantly higher than that of examples 7 to 10, and the UV damage resistance of examples 7 to 10 is significantly reduced in examples 7 to 10 due to the addition of only a single peony flower water or peppermint leaf water, or the substitution of the peony flower water or peppermint leaf water with other substances having similar efficacy, which indicates that the peony flower water and peppermint leaf water of the present invention have a synergistic effect, and can significantly improve the UV damage resistance and further improve the sunscreen effect.
Test example 5 sensory evaluation test
1. Pore hiding and fine line smoothing test
The samples prepared in examples 1-5 and comparative example 6 were selected for testing. 30 female volunteers with the age of 28-35 years who meet the requirements of the test were selected as subjects. The left face and the right face of a subject are respectively smeared with different test samples with the same amount, and the change of pores and wrinkles of the left face and the right face is observed.
Testing a grading rule: 5 points, 5 points-very effective; 4 min-very effective; 3 min-effective; 2 min-has a little effect; 1 minute-no effect at all. The subjects were scored according to the above scoring criteria and finally counted for all scores to calculate the mean.
2. Pre-makeup foundation effect test
The samples prepared in examples 1-5 and comparative example 6 were selected for testing. 30 female volunteers with the age of 28-35 years who meet the requirements of the test were selected as subjects. The left face and the right face of a subject are respectively coated with the same amount of different test samples, after the samples to be tested are filmed, the left face and the right face are respectively coated with the same amount of commercially available foundation liquid, and the makeup observation is carried out after 4 hours.
Testing a grading rule: 5, comprehensively scoring according to the difficulty of applying the foundation liquid during makeup, the makeup effect of the foundation liquid after makeup and the makeup effect after 4 hours: score 5-very satisfactory; score 4-satisfactory; 3 min-general; score 2-unsatisfied; score 1-very unsatisfactory. The subjects were scored according to the above scoring criteria and finally counted for all scores to calculate the mean.
The results of the above pore hiding and fine line smoothing tests, as well as the pre-makeup foundation effect, are shown in table 13.
Watch 13
Figure BDA0003287727200000181
Figure BDA0003287727200000191
From the test results in table 13, it can be seen that the samples of examples 1 to 5 of the present invention have significant effects of hiding pores and smoothing fine lines compared to the common sunscreen gel sample of comparative example 6, and when used as a makeup pre-emulsion, make up for subsequent color makeup is easy, and exhibit better makeup effects and longer lasting makeup-sustaining effects.
3. Irritation evaluation test
Examples 1-5, comparative example 5, and comparative example 6 were selected for irritation testing. 40 volunteers 23 to 34 years old were selected for the test, the test subjects of example 1 were subjected to the full face test, the test subjects of examples 2 to 4 and comparative examples 5 to 6 were subjected to the half face test, the test subjects were subjected to the evaluation 2 weeks later using the test samples for the full face in the morning or using different test samples for the left and right faces, and the evaluation results are shown in Table 14.
Irritation scoring rules: score 5, score 1-mild irritation; 2 min-the toxic stimulus is tolerable; 3 points-moderate stimulation fruit; 4 points-moderate to severe stimulation; score 5-severe irritation.
TABLE 14
Test sample Mean value of scores
Example 1 0
Example 2 0
Example 3 0
Example 4 0
Example 5 0
Comparative example 5 0.15
Comparative example 6 0.3
As can be seen from table 14, examples 1 to 5 of the present invention, which all scored 0 points, show that the mildness of the present invention is good, while comparative example 5, which has a mean of 0.15 points, and comparative example 6, which has a mean of 0.3 points, shows that comparative example 5 and comparative example 6 have some irritativeness due to the addition of preservatives and surfactants.
While the preferred embodiments of the present invention have been illustrated and described, it will be understood by those skilled in the art that the present invention is not limited to the details of the embodiments shown and described, but is capable of numerous equivalents and substitutions without departing from the spirit of the invention as set forth in the claims appended hereto.

Claims (5)

1. The gel is characterized by comprising the following components in percentage by mass: 16-21% of sun-screening agent, 20-65% of organic silicon elastomer, 2-25% of skin feel regulator, 1-10% of polyalcohol, 0.5-1% of peony flower water, 0.5-1% of peppermint leaf water and 10-30% of grease; the gel is free of preservatives and surfactants;
the organic silicon elastomer comprises at least one of polydimethylsiloxane/vinyl polydimethylsiloxane cross-linked polymer/cyclopentadimethylsiloxane, polydimethylsiloxane/vinyl polydimethylsiloxane cross-linked polymer/polydimethylsiloxane;
the skin feel modifier comprises at least one of silica, methyl methacrylate crosspolymer, polymethylsilsesquioxane, vinyl dimethicone/polymethylsilsesquioxane crosspolymer, dimethicone/vinyl dimethicone crosspolymer/silica.
2. The gel of claim 1, wherein said sunscreen agent comprises at least two of bis-ethylhexyloxyphenol methoxyphenyl triazine, diethylamino hydroxybenzoyl hexyl benzoate, ethylhexyl triazone, silicone-15, ethylhexyl salicylate, isoamyl p-methoxycinnamate, ethylhexyl methoxycinnamate.
3. The gel of claim 1, wherein said polyhydric alcohol comprises at least one of glycerol, butylene glycol, propylene glycol, dipropylene glycol, sorbitol, 1, 2-pentanediol, 1, 3-propanediol, 1, 2-hexanediol.
4. The gel of claim 1, wherein said oil comprises at least one of dioctyl carbonate, C12-15 alcohol benzoate, isohexadecane, isododecane, undecane/tridecane, phenyl trimethicone, octyl methicone, dimethicone, isononyl isononanoate, butanediol dicaprylate/dicaprate, butyl octanol salicylate.
5. A process for the preparation of a gel as claimed in any one of claims 1 to 4, characterized in that it comprises the following steps:
mixing the sun-screening agent and the grease, and heating to obtain a phase A;
mixing the organic silicon elastomer, the phase A and the skin feel modifier, and stirring to obtain a phase B;
mixing the peony flower water, the peppermint leaf water and the polyhydric alcohol, mixing the mixture with the phase A and the phase B, and stirring to obtain the gel.
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