CN118178228A - Application of cerium oxide in preparation of relieving, repairing and/or brightening products - Google Patents
Application of cerium oxide in preparation of relieving, repairing and/or brightening products Download PDFInfo
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- CN118178228A CN118178228A CN202410299876.4A CN202410299876A CN118178228A CN 118178228 A CN118178228 A CN 118178228A CN 202410299876 A CN202410299876 A CN 202410299876A CN 118178228 A CN118178228 A CN 118178228A
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- Prior art keywords
- cerium oxide
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- soothing
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- stirring
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- 229910000420 cerium oxide Inorganic materials 0.000 title claims abstract description 77
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 title claims abstract description 77
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 238000005282 brightening Methods 0.000 title abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 88
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000003974 emollient agent Substances 0.000 claims abstract description 35
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 34
- 239000003906 humectant Substances 0.000 claims abstract description 30
- 239000002562 thickening agent Substances 0.000 claims abstract description 27
- 239000002738 chelating agent Substances 0.000 claims abstract description 24
- 239000002537 cosmetic Substances 0.000 claims abstract description 21
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 49
- 238000010438 heat treatment Methods 0.000 claims description 44
- 238000003756 stirring Methods 0.000 claims description 38
- 238000000034 method Methods 0.000 claims description 32
- 238000002156 mixing Methods 0.000 claims description 26
- 238000004321 preservation Methods 0.000 claims description 25
- 239000003755 preservative agent Substances 0.000 claims description 25
- 230000002335 preservative effect Effects 0.000 claims description 25
- -1 polyol ester Chemical class 0.000 claims description 24
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 21
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- 230000008569 process Effects 0.000 claims description 19
- 239000002245 particle Substances 0.000 claims description 16
- 239000002243 precursor Substances 0.000 claims description 14
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- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 12
- GJQLBGWSDGMZKM-UHFFFAOYSA-N ethylhexyl palmitate Chemical compound CCCCCCCCCCCCCCCC(=O)OC(CC)CCCCC GJQLBGWSDGMZKM-UHFFFAOYSA-N 0.000 claims description 12
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- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 12
- FSEJJKIPRNUIFL-UHFFFAOYSA-N [2,2-bis(hydroxymethyl)-3-octadecanoyloxypropyl] octadecanoate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(CO)(CO)COC(=O)CCCCCCCCCCCCCCCCC FSEJJKIPRNUIFL-UHFFFAOYSA-N 0.000 claims description 11
- 229940082500 cetostearyl alcohol Drugs 0.000 claims description 11
- 229920001577 copolymer Polymers 0.000 claims description 11
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 claims description 11
- 230000035484 reaction time Effects 0.000 claims description 11
- 230000008439 repair process Effects 0.000 claims description 11
- OULAJFUGPPVRBK-UHFFFAOYSA-N tetratriacontyl alcohol Natural products CCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCO OULAJFUGPPVRBK-UHFFFAOYSA-N 0.000 claims description 11
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- BXWNKGSJHAJOGX-UHFFFAOYSA-N hexadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCO BXWNKGSJHAJOGX-UHFFFAOYSA-N 0.000 claims description 10
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 8
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- SZYSLWCAWVWFLT-UTGHZIEOSA-N [(2s,3s,4s,5r)-3,4-dihydroxy-5-(hydroxymethyl)-2-[(2r,3r,4s,5s,6r)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxyoxolan-2-yl]methyl octadecanoate Chemical compound O([C@@H]1[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O1)O)[C@]1(COC(=O)CCCCCCCCCCCCCCCCC)O[C@H](CO)[C@@H](O)[C@@H]1O SZYSLWCAWVWFLT-UTGHZIEOSA-N 0.000 claims description 6
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- QPJVMBTYPHYUOC-UHFFFAOYSA-N methyl benzoate Chemical compound COC(=O)C1=CC=CC=C1 QPJVMBTYPHYUOC-UHFFFAOYSA-N 0.000 claims description 4
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
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- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 claims description 2
- IYFATESGLOUGBX-YVNJGZBMSA-N Sorbitan monopalmitate Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O IYFATESGLOUGBX-YVNJGZBMSA-N 0.000 claims description 2
- HVUMOYIDDBPOLL-XWVZOOPGSA-N Sorbitan monostearate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O HVUMOYIDDBPOLL-XWVZOOPGSA-N 0.000 claims description 2
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- LWZFANDGMFTDAV-BURFUSLBSA-N [(2r)-2-[(2r,3r,4s)-3,4-dihydroxyoxolan-2-yl]-2-hydroxyethyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O LWZFANDGMFTDAV-BURFUSLBSA-N 0.000 claims description 2
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Abstract
The application discloses application of cerium oxide in preparation of a soothing, repairing and/or brightening product, and belongs to the technical field of cosmetics. The application provides a soothing and repairing composition which comprises the following components in parts by mass: 0.05 to 2 parts of cerium oxide, 1 to 10 parts of emulsifying agent, 1 to 10 parts of thickening agent, 5 to 50 parts of emollient, 0.1 to 20 parts of humectant, 0.01 to 2 parts of chelating agent and 1 to 95 parts of water. Experiments prove that the cerium oxide is added into the formula, so that the effects of relieving, repairing and brightening the composition can be obviously improved. The soothing and repairing composition can be widely applied to the field of cosmetics, and is suitable for preparing various cosmetic formulations such as emulsion, face cream, essence, facial mask and the like. The application fills the blank of cerium oxide in the preparation of cosmetics which are used for relieving, repairing and brightening.
Description
Technical Field
The application belongs to the technical field of cosmetics, and particularly relates to application of cerium oxide in preparation of a soothing, repairing and/or brightening product.
Background
The skin of human body is exposed in ultraviolet environment for a long time, so that the surface barrier is easily damaged, allergic reaction is easily generated, and the problems of skin redness, pain, itching and the like are caused. Moreover, due to the external pollution and the stimulation of living habits, skin problems such as dark complexion, dark yellow complexion, pigmentation, lack of luster and the like exist in a large group. These problems have led to increasing importance of skin care and finer product efficacy requirements. Based on the above, developing a skin care composition with soothing and repairing effects and with lightening effects is a technical problem to be solved by those skilled in the art.
In recent years, cerium oxide (CeO 2) has a wide development prospect in the field of cosmetics because of its ability to eliminate various active oxygen species and good biosafety. However, cerium oxide is currently used as a light-screening agent, an ultraviolet-resistant agent, etc. in the cosmetic field to achieve the effects of sun protection, photoprotection, etc. Few people have studied their efficacy in soothing inflammatory stimuli, photodamage repair or lightening products.
Disclosure of Invention
In order to overcome the defects in the prior art, the application provides application of cerium oxide in preparing a relieving, repairing and/or brightening product, and the relieving and repairing composition is added with cerium oxide, so that the composition has remarkable relieving and repairing effects and also has remarkable skin brightening effects.
In order to achieve the above object, the present application provides the following technical solutions:
in one aspect, the present application provides the use of cerium oxide for the preparation of a soothing, repairing and/or lightening product.
Optionally, the cerium oxide is spherical;
the particle size of the cerium oxide is 0.1-20 mu m;
the cerium oxide is prepared by a water/solvent thermal method.
Optionally, the cerium oxide has a particle size of 0.2 to 0.5 μm.
Alternatively, the cerium oxide has a particle size of 0.3 μm.
Optionally, the preparation process of the cerium oxide comprises the following steps: mixing cerium nitrate with water to obtain a precursor solution; adding acetic acid into the precursor solution to obtain a first solution; adding ethylene glycol into the first solution, and uniformly mixing to obtain a second solution; and heating the second solution to react to obtain the cerium oxide.
Optionally, the temperature of the heating reaction is 160-170 ℃;
the heating reaction time is 155-165 min;
the pressure of the heating reaction is 0.4-0.6 Mpa.
Optionally, the temperature of the heating reaction is 165 ℃;
the heating reaction time is 160min;
The pressure of the heating reaction is 0.5Mpa.
Optionally, the product comprises a cosmetic.
Optionally, the addition amount of cerium oxide is 0.05-2% in the application process.
Optionally, the addition amount of cerium oxide is 0.5-1.5% in the application process.
Alternatively, the cerium oxide is added in an amount of 1% during the application.
In a second aspect, the application provides a soothing and repairing composition comprising the following components in parts by mass: 0.05 to 2 parts of cerium oxide, 1 to 10 parts of emulsifying agent, 1 to 10 parts of thickening agent, 5 to 50 parts of emollient, 0.1 to 20 parts of humectant, 0.01 to 2 parts of chelating agent and 1 to 95 parts of water.
Optionally, the composition comprises the following components in parts by mass: 0.2 to 1 part of cerium oxide, 1 to 5 parts of emulsifying agent, 1 to 5 parts of thickening agent, 5 to 10 parts of emollient, 5 to 10 parts of humectant, 0.01 to 0.05 part of chelating agent and 60 to 90 parts of water.
Optionally, the cerium oxide is spherical;
the particle size of the cerium oxide is 0.1-20 mu m;
the cerium oxide is prepared by a water/solvent thermal method.
Optionally, the cerium oxide has a particle size of 0.2 to 0.5 μm.
Alternatively, the cerium oxide has a particle size of 0.3 μm.
Optionally, the preparation process of the cerium oxide comprises the following steps: mixing cerium nitrate with water to obtain a precursor solution; adding acetic acid into the precursor solution to obtain a first solution; adding ethylene glycol into the first solution, and uniformly mixing to obtain a second solution; and heating the second solution to react to obtain the cerium oxide.
Optionally, the temperature of the heating reaction is 160-170 ℃;
the heating reaction time is 155-165 min;
the pressure of the heating reaction is 0.4-0.6 Mpa.
Optionally, the temperature of the heating reaction is 165 ℃;
the heating reaction time is 160min;
The pressure of the heating reaction is 0.5Mpa.
Optionally, the emulsifier comprises at least one of polyol ester type emulsifier, alkyl glycoside type emulsifier, span and tween type emulsifier, phosphate ester type emulsifier, fatty alcohol polyether type emulsifier, polyglycerol type emulsifier and high polymer type emulsifier.
Optionally, the emulsifier comprises at least one of cetyl alcohol/cetostearyl glucoside/sucrose stearate, span 20, span 40, span 60, span 80, tween 120, polyglycerol-10 stearate, sorbitan fatty acid ester, polyoxyethylene sorbitan fatty acid ester.
Preferably, the emulsifier is EC-FIX SE (cetyl/cetostearyl glucoside/sucrose stearate).
Optionally, the thickener comprises at least one of polyacrylic acid, fatty alcohol and fatty acid, cellulose, natural gum and its modified substance, esters, inorganic macromolecule and its modified substance.
Optionally, the thickener comprises at least one of cetostearyl alcohol, pentaerythritol distearate, ammonium acryloyldimethyl taurate/VP copolymer, starch, acacia, pectin, agar, gelatin, seaweed gel, carrageenan, dextrin.
Alternatively, the thickener is a combination of cetostearyl alcohol, pentaerythritol distearate, AVC (ammonium acryloyldimethyl taurate/VP copolymer).
Optionally, the mass ratio of cetostearyl alcohol, pentaerythritol distearate, AVC (ammonium acryloyldimethyl taurate/VP copolymer) in the composition is 1-2:0.5-1:0.1-0.5.
Alternatively, the mass ratio of cetostearyl alcohol, pentaerythritol distearate, AVC (ammonium acryloyldimethyl taurate/VP copolymer) in the composition is 1.5:0.8:0.3. In the practical operation process, the application discovers that when the three components are combined, the proportion of the three components is critical to the stability and the overall form of the system, and the system state and the texture under the proportion are optimal, so that the viscosity of an external phase can be improved, the obstruction to the movement of an internal phase is caused, and the liquid drops are kept separate and are not aggregated.
Optionally, the emollient comprises at least one of high molecular polymers, vegetable oils, animal oils, mineral oils, synthetic oils.
Optionally, the emollient comprises at least one of polydimethylsiloxane, hydrogenated polyisobutene, ethylhexyl palmitate, coconut oil, olive oil, palm oil, lanolin, beeswax, jojoba oil, mineral oil, petrolatum.
Alternatively, the emollient is a combination of polydimethylsiloxane, hydrogenated polyisobutene, ethylhexyl palmitate.
Optionally, the mass ratio of the polydimethylsiloxane, the hydrogenated polyisobutene and the ethylhexyl palmitate in the composition is 1-3:4:1-3.
Optionally, the mass ratio of polydimethylsiloxane, hydrogenated polyisobutene, and ethylhexyl palmitate in the composition is 2:4:2.
In the present application, the selection of emollients has an important impact on the lightening effect of the final product. Experiments prove that the obvious brightening effect can be achieved only by adopting the emollient combination of the application to be compounded with other components.
Optionally, the humectant comprises at least one of natural moisturizing factor, polyalcohol humectant, polymer biochemical humectant and amino acid humectant.
Optionally, the humectant comprises at least one of glycerin, butylene glycol, glycerin polyether-26, trehalose.
Optionally, the humectant is a combination of glycerin and butylene glycol.
Optionally, the mass ratio of glycerin to butanediol in the composition is 3-5:3.
Optionally, the mass ratio of glycerin to butylene glycol in the composition is 4:3.
Optionally, the chelating agent comprises a hydroxy acid chelating agent and/or an amino acid derivative chelating agent.
Optionally, the chelating agent comprises at least one of disodium EDTA, ethylenediamine tetraacetic acid tetrasodium salt, and disodium nitrilotriacetate.
Preferably, the chelating agent is disodium EDTA.
Optionally, 0.1 to 5 parts of preservative is also included in the composition.
Optionally, 0.5 to 1 part of preservative is also included in the composition.
Optionally, the preservative comprises at least one of an alcohol preservative, a paraben preservative, methyl chloroisothiazolinone and methyl isothiazolinone, a formaldehyde releaser preservative, and an acid preservative.
Optionally, the preservative comprises at least one of phenoxyethanol/ethylhexyl glycerol, methyl benzoate, ethyl benzoate, propyl benzoate, sorbic acid, benzoic acid, dehydroacetic acid.
Preferably, the preservative is PEHG (phenoxyethanol/ethylhexyl glycerol).
In a third aspect, the present application provides a method for preparing the above-described soothing repair composition, comprising the steps of:
And uniformly mixing a mixture containing cerium oxide, water, a humectant, a chelating agent, an emulsifying agent, a thickening agent and an emollient to obtain the soothing and repairing composition.
Optionally, the method comprises the following steps:
(1) Mixing cerium oxide with water, heating to 80-85 ℃, homogenizing, adding a humectant and a chelating agent, and stirring under heat preservation to obtain a mixture 1;
(2) Mixing an emulsifying agent, a thickening agent and an emollient, heating to 80-85 ℃, and preserving heat to obtain a mixture 2;
(3) Homogenizing the mixture 1, adding the mixture 2 in the homogenizing process, and carrying out heat preservation and stirring after homogenizing to obtain a mixture 3;
(4) And (3) cooling the mixture 3 to 30-40 ℃, adding a preservative, and stirring uniformly to obtain the relief repair composition.
Optionally, in the step (1), the homogenizing rotation speed is 3000-4000 rpm;
the homogenizing time is 1-5 min;
the rotation speed of the heat preservation stirring is 50-150 rpm;
The time of heat preservation and stirring is 25-35 min.
Optionally, in the step (1), the homogenizing rotation speed is 3000-3500 rpm;
the homogenizing time is 2-4 min;
The rotation speed of the heat preservation stirring is 80-120 rpm;
The time of heat preservation and stirring is 28-32 min.
Optionally, in step (1), the homogenized rotation speed is independently selected from any value of 3000rpm, 3200rpm, 3400rpm, 3500rpm, 3600rpm, 3800rpm, 4000rpm or a range value between any two.
Optionally, in step (1), the time of homogenization is independently selected from any value or range of values between any two of 1min, 2min, 3min, 4min, 5 min.
Optionally, in step (1), the rotational speed of the incubation agitation is independently selected from any value or range of values between any two of 50rpm, 80rpm, 100rpm, 120rpm, 150 rpm.
Optionally, in step (1), the time of incubation and stirring is independently selected from any value or range of values between any two of 25min, 28min, 30min, 32min, 35 min.
Optionally, in the step (3), the homogenizing rotation speed is 3000-4000 rpm;
The homogenizing time is 5-15 min;
the rotation speed of the heat preservation stirring is 50-150 rpm;
The time of heat preservation and stirring is 25-35 min.
Optionally, in the step (3), the homogenizing rotation speed is 3400-3600 rpm;
the homogenizing time is 8-12 min;
The rotation speed of the heat preservation stirring is 80-120 rpm;
The time of heat preservation and stirring is 28-32 min.
Optionally, in step (3), the homogenized rotation speed is independently selected from any value of 3000rpm, 3200rpm, 3400rpm, 3500rpm, 3600rpm, 3800rpm, 4000rpm or a range value between any two.
Optionally, in step (3), the time of homogenization is independently selected from any value or range of values between any two of 5min, 8min, 10min, 12min, 15 min.
Optionally, in step (3), the rotational speed of the incubation agitation is independently selected from any value or range of values between any two of 50rpm, 80rpm, 100rpm, 120rpm, 150 rpm.
Optionally, in step (3), the time of incubation and stirring is independently selected from any value or range of values between any two of 25min, 28min, 30min, 32min, 35 min.
In a fourth aspect, the present application provides the use of a soothing composition as described above in the preparation of a cosmetic.
Optionally, the formulation of the cosmetic comprises at least one of emulsion, face cream, essence and facial mask.
Compared with the prior art, the application has the following beneficial effects:
(1) The research of the application shows that the cerium oxide is applied to the formula of the cosmetic, not only can remarkably enhance the relieving and repairing effects of the cosmetic, but also can make the cosmetic have the effect of brightening; the application fills the blank of cerium oxide in the preparation of cosmetics which are used for relieving, repairing and brightening.
(2) According to the soothing and repairing composition provided by the application, the cerium oxide microspheres are added in the formula, and after verification of a single-time and high-dose human body photoaging model, the skin injury caused by illumination can be effectively repaired after the cerium oxide is added, redness and sensitivity after illumination are obviously improved, and the water loss is obviously reduced, so that the product provided by the application has obvious effects of light protection and barrier repair. Based on 3D epidermis skin modelCompared with a control group, the product has obviously reduced contents of inflammatory factors (IL-1 alpha) and nuclear transcription factors (NF-kB), which indicates that the product can down regulate the contents of inflammatory factors (IL-1 alpha) and nuclear transcription factors (NF-kB) and has a relieving effect. Based on 3D epidermal skin model/>Compared with a control group, the content of the transglutaminase 1 (TGM 1) of the product is obviously increased, the content of the DNA damaged Cyclobutane Pyrimidine Dimer (CPD) is obviously reduced, and the product is capable of increasing the content of the transglutaminase 1 (TGM 1) and reducing the content of the DNA damaged Cyclobutane Pyrimidine Dimer (CPD) and has a repairing effect. The change of the L-value and the ITA-value of the skin color before and after the product is used is tested, so that the product can be used for remarkably improving the skin color and the brightness after 21 days and 28 days, and has remarkable brightening effect.
(3) The preparation method of the soothing and repairing composition provided by the application adopts a batch feeding mode and a reasonable process, improves the uniformity and stability of the whole system, can combine the components together to the maximum extent, and realizes the synergistic effect of the components. Meanwhile, the whole preparation process is simple and easy to operate, raw materials are easy to obtain, the cost is low, and the preparation method is suitable for industrial production.
(4) The soothing and repairing composition provided by the application can be widely applied to the field of cosmetics, and is suitable for preparing various cosmetic formulations such as emulsion, face cream, essence, facial mask and the like; the application fills the blank of cerium oxide in the preparation of cosmetics which are used for relieving, repairing and brightening.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present application and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a graph showing the trend of heme EI change in example 1, example 2 and comparative example 1 of the present application (note: X represents a significant difference (P.ltoreq.0.05) from before use), and # represents a significant difference (P < 0.05) from the product of comparative example 1);
Fig. 2 is a graph showing the trend of change in skin color a values for example 1, example 2 and comparative example 1 of the present application (note: indicating significant difference (p.ltoreq.0.05) from before use), and # indicating significant difference (P < 0.05) from the product of comparative example 1);
FIG. 3 is a graph showing the variation trend of the percutaneous water loss TEWL of the present application in example 1, example 2 and comparative example 1 (note: showing a significant difference (P.ltoreq.0.05) from before use), and # showing a significant difference (P < 0.05) from the product of comparative example 1);
FIG. 4 is a TiVi-index trend graph of examples 1, 2 and comparative example 1 (note: indicating significant difference (P.ltoreq.0.05) from before use, # indicating significant difference (P < 0.05) from the product of comparative example 1);
FIG. 5 is an example TiVi-index images of example 1, example 2, and comparative example 1 of the present application;
Fig. 6 is a bar graph of IL-lα content detection results (note: significance is represented by # for the BC group, P-value <0.01 is represented by # #, and significance is represented by x for the NC group, P-value <0.01 is represented by x);
FIG. 7 is a graph of TGM1 immunofluorescence results;
FIG. 8 is a bar graph of TGM1 relative Integrated Optical Density (IOD) values (note: significance is represented by # for the BC group, P-value <0.01 is represented by # #, and significance is represented by x for the NC group, P-value <0.01 is represented by x);
FIG. 9 is a graph of NF-kB immunofluorescence results;
FIG. 10 is a histogram of NF-kB relative Integrated Optical Density (IOD) values (note: significance is indicated by # for the BC group, P-value <0.01 is indicated by # #, and significance is indicated by x for the NC group, P-value <0.01 is indicated by x);
FIG. 11 is a graph showing the result of DNA damage CPD immunohistochemistry;
Fig. 12 is a bar graph of DNA damage CPD detection results (note: significance is represented by # for the BC group, P-value <0.01 is represented by # #, and significance is represented by x for the NC group, P-value <0.05 is represented by x, and P-value <0.01 is represented by x);
Fig. 13 is a graph showing the change rate of the skin color L (note: shows a significant difference (p.ltoreq.0.05) from before use; # shows a significant difference (P < 0.05) from comparative examples 1, 2, 3, and 6);
Fig. 14 is a graph showing the change rate of the skin color ITA ° value (note: x represents a significant difference (p.ltoreq.0.05) from before use; and # represents a significant difference (P < 0.05) from comparative example 1, comparative example 2, comparative example 3, and example 6).
Detailed Description
The application will be further illustrated with reference to specific examples. The following description is given of several embodiments of the present application and is not intended to limit the application in any way, and although the application is disclosed in the preferred embodiments, it is not intended to limit the application, and any person skilled in the art will make some changes or modifications with the technical content disclosed in the above description equivalent to the equivalent embodiments without departing from the scope of the technical solution of the present application.
Unless otherwise indicated, all starting materials in the examples of the present application were purchased commercially and used without any particular treatment.
Unless otherwise indicated, the analytical methods in the examples all employed conventional arrangements of instruments or equipment and conventional analytical methods.
The cerium oxide in the following examples 1 to 3 was self-made by the present company laboratory, and the preparation process was: weighing 20g of cerium nitrate hexahydrate, and mixing the cerium nitrate hexahydrate with 10mL of deionized water to prepare a precursor solution; adding 20mL of acetic acid into the precursor solution to prepare a first solution; adding 600mL of ethylene glycol into the first solution, and uniformly mixing to prepare a second solution; wherein, the mass ratio of the cerium nitrate hexahydrate in the second solution is 3 percent; transferring the second solution into a 1L hastelloy pressure-resistant reaction kettle for heating reaction, wherein the reaction temperature is 165 ℃, the reaction time is 160min, and the reaction pressure is 0.5Mpa; filtering and heating the reaction product by adopting a ceramic filter membrane with the average pore diameter of 500nm, washing the filtered filtrate to be neutral by adopting water, and drying at room temperature for 24 hours; sterilizing, and packaging to obtain cerium oxide microsphere (average particle diameter of 0.3 μm).
Example 1
A preparation method of a soothing and repairing composition comprises the following steps:
(1) Weighing the following raw materials in parts by weight: cerium oxide 0.5 parts, EC-FIX SE (cetyl alcohol/cetostearyl glucoside/sucrose stearate) (emulsifier) 3 parts, cetostearyl alcohol (thickener) 1.5 parts, 0.8 Part of PES pentaerythritol distearate (thickener), 0.3 part of AVC (ammonium acryloyldimethyl taurate/VP copolymer) (thickener), 2 parts of DM100 polydimethylsiloxane (emollient), 4 parts of synthesized squalane (hydrogenated polyisobutene) (emollient), 2 parts of Crodamol OP-LQ ethylhexyl palmitate (emollient), 4 parts of glycerol (humectant), 3 parts of butanediol (humectant), 0.03 part of EDTA disodium (chelating agent), PEHG (phenoxyethanol/ethylhexyl glycerol) (preservative), 0.7 part of deionized water and 78.17 parts of deionized water;
(2) Mixing cerium oxide with deionized water, heating to 80 ℃, homogenizing for 3min under 3000rpm, adding humectant and chelating agent, and stirring for 30min under 100rpm to obtain a mixture 1;
(3) Mixing an emulsifying agent, a thickening agent and an emollient, heating to 80 ℃, and preserving heat to obtain a mixture 2;
(4) Adding the mixture 1 into a main pot, starting homogenization (the homogenization rotating speed is 3500 rpm), slowly adding the mixture 2 in the homogenization process, homogenizing for 10min, and then carrying out heat preservation and stirring for 30min under the condition of 100rpm to obtain a mixture 3;
(5) Continuously stirring and cooling, adding preservative when the temperature of the mixture 3 is reduced to 40 ℃, stirring uniformly, and discharging when the temperature is reduced to 38 ℃ to obtain the soothing and repairing composition.
Example 2
A preparation method of a soothing and repairing composition comprises the following steps:
(1) Weighing the following raw materials in parts by weight: cerium oxide 1 part, EC-FIX SE (cetyl alcohol/cetostearyl glucoside/sucrose stearate) (emulsifier) 3 parts, cetostearyl alcohol (thickener) 1.5 parts, 0.8 Part of PES pentaerythritol distearate (thickener), 0.3 part of AVC (ammonium acryloyldimethyl taurate/VP copolymer) (thickener), 2 parts of DM100 polydimethylsiloxane (emollient), 4 parts of synthesized squalane (hydrogenated polyisobutene) (emollient), 2 parts of Crodamol OP-LQ ethylhexyl palmitate (emollient), 4 parts of glycerol (humectant), 3 parts of butanediol (humectant), 0.03 part of EDTA disodium (chelating agent), PEHG (phenoxyethanol/ethylhexyl glycerol) (preservative), 0.7 part of deionized water 77.67 parts;
(2) Mixing cerium oxide with deionized water, heating to 80 ℃, homogenizing for 3min under 3000rpm, adding humectant and chelating agent, and stirring for 30min under 100rpm to obtain a mixture 1;
(3) Mixing an emulsifying agent, a thickening agent and an emollient, heating to 80 ℃, and preserving heat to obtain a mixture 2;
(4) Adding the mixture 1 into a main pot, starting homogenization (the homogenization rotating speed is 3500 rpm), slowly adding the mixture 2 in the homogenization process, homogenizing for 10min, and then carrying out heat preservation and stirring for 30min under the condition of 100rpm to obtain a mixture 3;
(5) Continuously stirring and cooling, adding preservative when the temperature of the mixture 3 is reduced to 40 ℃, stirring uniformly, and discharging when the temperature is reduced to 38 ℃ to obtain the soothing and repairing composition.
Example 3
A preparation method of a soothing and repairing composition comprises the following steps:
(1) Weighing the following raw materials in parts by weight: cerium oxide 0.2 parts, EC-FIX SE (cetyl alcohol/cetostearyl glucoside/sucrose stearate) (emulsifier) 3 parts, cetostearyl alcohol (thickener) 1.5 parts, 0.8 Part of PES pentaerythritol distearate (thickener), 0.3 part of AVC (ammonium acryloyldimethyl taurate/VP copolymer) (thickener), 2 parts of DM100 polydimethylsiloxane (emollient), 4 parts of synthesized squalane (hydrogenated polyisobutene) (emollient), 2 parts of Crodamol OP-LQ ethylhexyl palmitate (emollient), 4 parts of glycerol (humectant), 3 parts of butanediol (humectant), 0.03 part of EDTA disodium (chelating agent), PEHG (phenoxyethanol/ethylhexyl glycerol) (preservative), 0.7 part of deionized water and 78.47 parts of deionized water;
(2) Mixing cerium oxide with deionized water, heating to 80 ℃, homogenizing for 3min under 3000rpm, adding humectant and chelating agent, and stirring for 30min under 100rpm to obtain a mixture 1;
(3) Mixing an emulsifying agent, a thickening agent and an emollient, heating to 80 ℃, and preserving heat to obtain a mixture 2;
(4) Adding the mixture 1 into a main pot, starting homogenization (the homogenization rotating speed is 3500 rpm), slowly adding the mixture 2 in the homogenization process, homogenizing for 10min, and then carrying out heat preservation and stirring for 30min under the condition of 100rpm to obtain a mixture 3;
(5) Continuously stirring and cooling, adding preservative when the temperature of the mixture 3 is reduced to 40 ℃, stirring uniformly, and discharging when the temperature is reduced to 38 ℃ to obtain the soothing and repairing composition.
Example 4
The other components and the step conditions were the same as in example 2 except for the cerium oxide preparation process.
The cerium oxide in this embodiment is self-made by the laboratory of the company, and the preparation process is as follows: weighing 20g of cerium nitrate hexahydrate, and mixing the cerium nitrate hexahydrate with 10mL of deionized water to prepare a precursor solution; adding 20mL of acetic acid into the precursor solution to prepare a first solution; adding 600mL of ethylene glycol into the first solution, and uniformly mixing to prepare a second solution; wherein, the mass ratio of the cerium nitrate hexahydrate in the second solution is 3 percent; transferring the second solution into a 1L hastelloy pressure-resistant reaction kettle for heating reaction, wherein the reaction temperature is 160 ℃, the reaction time is 155min, and the reaction pressure is 0.4Mpa; filtering and heating the reaction product by adopting a ceramic filter membrane with the average pore diameter of 500nm, washing the filtered filtrate to be neutral by adopting water, and drying at room temperature for 24 hours; sterilizing, and packaging to obtain cerium oxide microsphere (average particle diameter of 0.1 μm).
Example 5
The other components and the step conditions were the same as in example 2 except for the cerium oxide preparation process.
The cerium oxide in this embodiment is self-made by the laboratory of the company, and the preparation process is as follows: weighing 20g of cerium nitrate hexahydrate, and mixing the cerium nitrate hexahydrate with 10mL of deionized water to prepare a precursor solution; adding 20mL of acetic acid into the precursor solution to prepare a first solution; adding 600mL of ethylene glycol into the first solution, and uniformly mixing to prepare a second solution; wherein, the mass ratio of the cerium nitrate hexahydrate in the second solution is 3 percent; transferring the second solution into a 1L hastelloy pressure-resistant reaction kettle for heating reaction, wherein the reaction temperature is 170 ℃, the reaction time is 165min, and the reaction pressure is 0.6Mpa; filtering and heating a reaction product by using a filter membrane, washing the filtered filtrate to be neutral by using water, and drying the filtrate at room temperature for 24 hours; sterilizing, and packaging to obtain cerium oxide microsphere (average particle diameter of 20 μm).
Example 6
The remaining components and process conditions were the same as in example 2 except that the source of cerium oxide was common commercial (purchased from Yangrun technologies (Guangdong) Co., ltd., average particle size of 0.3 μm).
Comparative example 1
The other components and process conditions were the same as in example 2 except that no cerium oxide was added.
Comparative example 2
The remaining components and process conditions were identical to those of example 2 except that 2 parts of "DM100 polydimethylsiloxane (emollient) (hydrogenated polyisobutene) (emollient) was replaced with 2 parts of" polypropylene glycol (emollient) 2 parts of Crodamol OP-LQ ethylhexyl palmitate (emollient) ", 4 parts of sea buckthorn oil (emollient) and 2 parts of rose hip oil (emollient)".
Comparative example 3
The other components and the conditions of the steps were the same as in example 2 except that the processes of steps (4) and (5) were different.
The steps (4) and (5) in this comparative example are:
(4) Adding the mixture 1 into a main pot, adding the mixture 2, starting homogenizing (the homogenizing rotating speed is 3500 rpm), homogenizing for 10min, and then carrying out heat preservation and stirring for 30min under the condition of 100rpm to obtain a mixture 3;
(5) Adding antiseptic into the mixture 3, stirring, cooling to 38deg.C, and discharging to obtain the final product.
Experimental example 1
Establishing a single and high-dose human body photoaging model, and evaluating the repairing effect of different test samples on photodamage:
1. test sample:
example 1 product, example 2 product, comparative example 1 product, before use
2. And (3) test design:
Volunteers who were screened for compliance were tested with the back area. The minimal erythema dose MED was determined for each volunteer by shining the Solar Light601-300 Solar ultraviolet Light module on the back prior to testing. The test area was irradiated with high dose ultraviolet rays (1.5 MED) a single time, and the measured value 24 hours after irradiation was used as an initial value (T0), after which the test sample was applied twice daily for 2 consecutive days, and skin data was collected after using the sample, and the effect of the sample of the example was evaluated by comparing with the product of comparative example 1 applied and the area before use.
3. Volunteer requirements:
1. volunteer enrollment criteria:
1) Age 18-60 years, healthy men or women;
2) Skin type II-III populations (test site skin tone ITA ° values above 28 °);
3) No allergic diseases, no allergic history of cosmetics or other external preparations;
4) No medicine affecting the light sensitivity is used in the recent history of no light-sensitive disease;
5) Skin at the tested part should be free of pigmentation, inflammation, scar, pigmented nevus, and hair;
6) A person capable of receiving the skin of the test area for tanning using an artificial light source;
7) The test procedure can be understood, voluntarily taking part in the test and signing a written informed consent.
2. Volunteer exclusion criteria:
1) Pregnant or lactating women, or those who have a pregnancy preparation plan recently;
2) Skin history patients with psoriasis, eczema, atopic dermatitis, severe acne, etc.;
3) For the last 1 month, anti-inflammatory drugs such as corticosteroids, etc. are orally taken or externally used;
4) For about 2 months, orally or topically applying any product or drug that affects skin color (e.g., hydroquinone-based formulations);
5) The skin blackening marks of the test parts do not completely fade after the similar tests are carried out in 3 months or before 3 months;
6) Other clinical trials were enrolled in approximately 2 months;
7) Other clinical evaluations were considered unsuitable for the participants.
4. Sample size:
ensuring 24-30 persons of effective data.
5. Test area:
And (3) a back. The sample application area of each test area should be not less than 6cm 2 and the interval between each test area should be not less than 1.0cm. The UV irradiation zone should be located within each of the application zones. Solar Light 601-300 Solar ultraviolet Light system (Solar Light Company, inc), long wave Ultraviolet (UVA) and medium wave Ultraviolet (UVB) filter specifications, irradiating to form square spots with sides of 8mm, and irradiating at a dose of 1.5 times MED.
6. Sample application mode:
In the test period, a worker smears the test object according to a random table corresponding to the test area, smears 1 sample according to a sample distribution table in the test area of the volunteer every morning and afternoon, and uses the sample according to the sample application amount of 2.00+/-0.05 mg/cm 2 each time every time with the time interval of not less than 4 hours.
7. The testing process comprises the following steps:
(1) Day1: volunteer screening; registering group entering information and informed consent; testing ITA degree value, and fumbling MED by ultraviolet irradiation;
(2) Day2: 1) Determining a subject MED;
2) Skin background value acquisition (BL);
3) Setting the irradiation dose to be 1.5 times of MED, and carrying out single irradiation;
(3) After irradiation: 1) Day3 (T0, 24h after UV irradiation), day4 (Td 1), day5 (Td 2) interviews, collecting skin data for each test area;
2) Day3 to Day5 were used once each Day in the afternoon (after data collection).
1. Visual assessment: the two researchers independently carried out subjective assessment of skin condition (redness, color shift, desquamation or other manifestations respectively);
2. TiVi image acquisition (TiVi, 700, wheelsBridge, sweden), one for each region, analysis TiVi-index;
3. skin color a value (Chroma Meters CR-700D), 1 acquisition in parallel;
4. Skin heme index EI (skin red melanin tester Mexameter MX, 18), collected 3 times in parallel;
5. Percutaneous water loss (percutaneous water loss tester, BIOXAquaflux) was collected in parallel 1 time.
8. Test period:
For 5 days.
9. Test time point:
Background value: BL (before irradiation);
initial value: 24h (T0) after UV irradiation;
Within 7 days after sample use: 48h (Td 1), 72h (Td 2), td7 after UV irradiation.
10. Image analysis:
1. Each region is cut TiVi and 700 to collect polarized light patterns and TiVi analysis patterns, and the images are analyzed TiVi-index;
2. each region provides a VC98 picture, which suggests analysis of the sels, SEsc.
11. Data analysis:
intra-group analysis: after use (Td 1-2) vs T0;
Inter-group variance analysis: example 1/2 product vs. comparative example 1 product.
12. The specific experimental results are as follows:
1. the results of the heme EI test are shown in tables 1, 2 and FIG. 1.
TABLE 1 heme EI test results
TABLE 2 heme EI significance analysis results
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Note that: n=30, based on human back test, results using T test, # indicating significant difference (p.ltoreq.0.05) compared to pre-use and # indicating significant difference (P < 0.05) compared to cream base; the rate of change (%) = (after-use-before-use)/100% before use shown in fig. 1.
2. The results of the skin color a values are shown in table 3, table 4 and fig. 2.
Table 3 skin color a value test results
Table 4 skin color a value significance analysis results
Note that: n=30, based on human back test, results using T test, # indicating significant difference (p.ltoreq.0.05) compared to pre-use and # indicating significant difference (P < 0.05) compared to cream base; the rate of change (%) = (after-use-before-use)/100% before use shown in fig. 2.
3. The results of the percutaneous water loss test are shown in tables 5, 6 and 3.
TABLE 5 percutaneous moisture loss TEWL test results
TABLE 6 results of the percutaneous moisture loss TEWL significance analysis
Note that: n=30, based on human back test, results using T test, # indicating significant difference (p.ltoreq.0.05) compared to pre-use and # indicating significant difference (P < 0.05) compared to cream base; the rate of change (%) = (after-use-before-use)/100% before use shown in fig. 3.
4. The test results of Tivi700,700 are shown in tables 7, 8 and figures 4 and 5.
Table 7Tivi test results 700
Table 8Tivi700,700 significance analysis results
Note that: n=30, based on human back test, results using T test, # indicating significant difference (p.ltoreq.0.05) compared to pre-use and # indicating significant difference (P < 0.05) compared to cream base; the rate of change (%) = (after-use-before-use)/100% before use shown in fig. 4.
From the above experimental results, compared with the matrix product group in comparative example 1, the cerium oxide product of the embodiment of the application can effectively repair skin damage caused by illumination on human skin, remarkably improve redness and sensitivity after illumination, and remarkably reduce water loss, thus indicating that the product of the application has remarkable light protection and barrier repair effects.
Experimental example 2
3D epidermal skin model using UVB irradiationEvaluating the relief efficacy of different samples to be tested by detecting the changes in the content of inflammatory factors (IL-lα) and nuclear transcription factors (NF-kB); the repair efficacy of different test samples was evaluated by detecting changes in the levels of transglutaminase 1 (TGM 1) and DNA damaging Cyclobutane Pyrimidine Dimers (CPD):
1. Test materials
1. And (3) a testing system:
3D epidermis skin model for this test Lot number: ES231106, available from guangdong bosch biotechnology limited.
2. The main reagent comprises:
EpiGrowth culture (Guangdong Boxi organism), PBS (Solebao), IL-lα ELISA kit (Abcam), dexamethasone (Medium), WY14643 (Sigma), vitamin E (VE, sigma), TGM1 antibody (Abcam), CPD antibody (CosMo Bio Co. LTD.), paraformaldehyde (Biosharp), NF-kB antibody (Abcam).
3. The main equipment comprises:
CO 2 incubator (Thermo, 150I), ultra clean bench (Sujingtai, SW-CJ-IF), microplate reader (BioTek, epoch), UVB irradiation instrument (Philips), fluorescence microscope (Leica, DM 2500).
4. Sample information:
TABLE 9 sample information
| Sample name | Quantity of | Specification of specification | Color and physical state |
| Example 3 product | 1 Bottle | 30 G/bottle | Pale yellow emulsion |
2. Test method
1. Test packets:
table 10 test packets
Note that: PC1 (dexamethasone) was used for positive control of IL-lα; PC2 (WY 14643) was used for a positive control of TGM1, NF-kB; PC3 (VE) was used as a positive control for DNA damage CPD.
2. Administration and irradiation:
1) According to the test group, the model was transferred to a 6-well plate (EpiGrowth culture broth added in advance with 0.9mL of the corresponding group), and the test group number was marked on the 6-well plate.
2) And adding working solution with corresponding concentration under PC group liquid, uniformly smearing the sample stock solution on the surface of a model by the sample group, and placing the model in a CO 2 incubator (37 ℃ C., 5% CO 2) for 24h of incubation.
3) After 24h incubation, the groups requiring UVB irradiation were subjected to UVB irradiation (irradiation dose 600mJ/cm 2) in a CO 2 incubator (37 ℃, 5% CO 2) for a further 24h incubation, according to the test group (Table 1).
4) After the incubation, the sample remaining on the surface of the model was washed with sterile PBS, and the inner and outer residual liquids of the model were wiped off with a sterile cotton swab.
3. ELISA detection:
After 24h incubation, collecting the culture solution of the 3D epidermis skin model in a centrifuge tube, and after collection, placing the sample for ELISA detection in a refrigerator at-80 ℃ for freezing preservation, and carrying out detection analysis according to the operation instruction of an ELISA kit.
4. Immunofluorescence test:
Taking out the model for detection, performing fixation treatment by using 4% paraformaldehyde, performing immunofluorescence detection after 24 hours of fixation, photographing and observing under a microscope, and collecting and analyzing pictures.
5. Immunohistochemical test:
taking out the model for detection, performing fixation treatment by using 4% paraformaldehyde, performing immunohistochemical detection after 24 hours fixation, photographing and observing under a microscope, and collecting and analyzing pictures.
6. Lifting rate and inhibition rate calculation:
7. Results statistical analysis:
The results are expressed as mean±sd using GRAPHPAD PRISM plots. Comparisons between groups were performed using t-test statistical analysis. Statistical analysis was double tailed. P <0.05 was considered to have significant differences and P <0.01 was considered to have very significant differences.
3. Test results
1. Inflammatory factor (IL-lα) test results are shown in Table 11 and FIG. 6.
TABLE 11 results of IL-lα content detection
Note that: when the statistical analysis is performed by the t-test method, compared with the BC group, the significance is expressed as # and the P-value <0.05 is expressed as # and the P-value <0.01 is expressed as #; compared to NC groups, significance is expressed as x, P-value <0.05 is expressed as x, and P-value <0.01 is expressed as x.
As can be seen from table 11 and fig. 6, the IL-lα content of NC group was significantly increased compared to BC group, indicating that the stimulation conditions of this test were effective; compared with the NC group, the IL-lα content of the PC1 group is obviously reduced, which proves that the positive control of the test is effective; compared with NC group, the IL-lα content of the product of example 3 of the application is obviously reduced, and the inhibition rate is 8.66%.
2. The results of the transglutaminase 1 (TGM 1) test are shown in table 12 and fig. 7 and 8.
TABLE 12 summary of TGM1 immunofluorescence analysis results
Note that: integrated Optical Density (IOD), whose value reflects the content of TGM 1. When the statistical analysis is performed by the t-test method, compared with the BC group, the significance is expressed as # and the P-value <0.05 is expressed as # and the P-value <0.01 is expressed as #; compared to NC groups, significance is expressed as x, P-value <0.05 is expressed as x, and P-value <0.01 is expressed as x.
As can be seen from table 12, fig. 7 and fig. 8, the TGM1 content of NC group is significantly reduced compared with BC group, indicating that the test stimulus condition is effective; compared with the NC group, the TGM1 content of the PC2 group is obviously increased, which proves that the positive control of the test is effective; compared with NC group, the TGM1 content of the product of the embodiment 3 of the application is obviously increased, and the increase rate is 158.49%.
3. The results of nuclear transcription factor (NF-kB) test are shown in Table 13 and FIGS. 9 and 10.
TABLE 13NF-kB immunofluorescence analysis results summary table
Note that: integrated Optical Density (IOD), a value reflecting the NF-kB content. When the statistical analysis is performed by the t-test method, compared with the BC group, the significance is expressed as # and the P-value <0.05 is expressed as # and the P-value <0.01 is expressed as #; compared to NC groups, significance is expressed as x, P-value <0.05 is expressed as x, and P-value <0.01 is expressed as x.
As can be seen from table 13, fig. 9 and fig. 10, the NF-kB content of NC group is significantly increased compared to BC group, indicating that the stimulus condition of this test is effective; compared with the NC group, the NF-kB content of the PC2 group is obviously reduced, which proves that the positive control of the test is effective; compared with NC group, the NF-kB content of the product of the embodiment 3 of the application is obviously reduced, and the inhibition rate is 89.71 percent.
4. The results of the DNA damage Cyclobutane Pyrimidine Dimer (CPD) test are shown in table 14 and fig. 11, 12.
TABLE 14DNA damage CPD immunohistochemical analysis results summary
Note that: the difference analysis is carried out by a t-test method, compared with the BC group, the significance is expressed as # and the P-value <0.05 is expressed as # and the P-value <0.01 is expressed as #; compared to NC groups, significance is expressed as x, P-value <0.05 is expressed as x, and P-value <0.01 is expressed as x.
As can be seen from table 14, fig. 11 and fig. 12, the IOD/positive cell number in NC group significantly increased compared to BC group, indicating that the stimulation conditions of this test were valid; compared with the NC group, the IOD/positive cell value of the PC3 group is obviously reduced, which indicates that the positive control of the test is effective; compared with NC group, the IOD/positive cell number of the product of the application example 3 is obviously reduced, and the inhibition rate is 14.84%.
To sum up, based on the 3D epidermis modelCompared with a control group, the product of the embodiment 3 of the application has obviously reduced contents of inflammatory factors (IL-1 alpha) and nuclear transcription factors (NF-kB), the inhibition rates are 8.66 percent and 89.71 percent respectively, which indicates that the product can down regulate the contents of inflammatory factors (IL-1 alpha) and nuclear transcription factors (NF-kB) and has a relieving effect. Based on 3D epidermal skin model/>Compared with a control group, the content of the transglutaminase 1 (TGM 1) of the product in the embodiment 3 is obviously increased, the increasing rate is 158.49%, the content of the DNA damaged Cyclobutane Pyrimidine Dimer (CPD) is obviously reduced, and the inhibition rate is 14.84%, which indicates that the product can increase the content of the transglutaminase 1 (TGM 1) and lower the content of the DNA damaged Cyclobutane Pyrimidine Dimer (CPD) and has a repairing effect.
Experimental example 3
Testing the change of the L-value and the ITA-degree value of the skin before and after using different products, and evaluating the lightening effect of the test sample:
1. test sample:
Example 2 product, example 4 product, example 5 product, example 6 product, comparative example 1 product, comparative example 2 product, comparative example 3 product, before use
2. And (3) test design:
Volunteers who were screened for compliance were enrolled in the test, with the test area being the face. The skin color L value and ITA value data of 7 days, 14 days, 21 days and 28 days after application are collected after the sample is used, and the lightening effect of the sample of the example is evaluated by comparing the sample with the product of the comparative example and the sample before use.
3. Test requirements:
1. volunteer enrollment criteria:
1) Age 18-60 years, healthy men or women;
2) No allergic diseases, no allergic history of cosmetics or other external preparations;
3) The test process can be understood, and the person voluntarily participates in the test and signs written informed consent;
2. volunteer exclusion criteria:
1) Antihistamines used for the last week or immunosuppressants used for the last month;
2) Any anti-inflammatory agent is administered to the subject in the last two months; insulin dependent diabetes mellitus patients;
3) A patient suffering from a respiratory disease undergoing treatment; women in lactation or gestation;
4) Allergic constitution, allergic dermatitis, etc., and has skin diseases or disease history;
5) A violin subject who is receiving dermatological treatment or one month of oral hydroxy acids, whitening and anti-aging drugs;
6) The test area has skin symptoms affecting the test, such as large-area birthmarks, scratches, white spots, pigmented nevi, keloids and the like;
7) In addition to the above, other test persons were judged to be unsuitable for the population as the test subject.
4. Sample size:
and 8 people can guarantee effective data.
5. Sample application mode:
the skin care product is taken to be applied to the facial skin, gently massaged until being absorbed, and used according to the dosage of the skin care product per se.
6. The testing process comprises the following steps:
1) Volunteer screening; registering group entering information and informed consent;
2) Washing the face with clear water and sitting still for half an hour;
3) Collecting background skin color L value and ITA degree value data;
3) Smearing a sample; collecting data of L-value and ITA DEG value of skin color after 7 days, 14 days, 21 days and 28 days of smearing samples;
4) Skin color L values, ITA ° values were collected and 3 times in parallel.
7. Test time point:
Pre-sample (T0), 7 days post-sample (Td 7), 14 days post-sample (Td 14), 21 days post-sample (Td 21), 28 days post-sample (Td 28).
8. Data analysis:
Intra-group analysis: post-use (Td 7, td14, td21, td 28) vs T0;
inter-group variance analysis: example 2 product vs. comparative example 1 product; example 2 product vs. comparative example 2 product; example 2 product vs. comparative example 3 product; example 2 product vs example 6 product.
9. The specific experimental results are as follows:
1. The skin color L values are shown in table 15 and fig. 13.
Table 15 skin color L value test results
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Note that: n=8, based on human face test; results were tested using T-test, which shows significant differences (p.ltoreq.0.05) compared to before use; # represents a significant difference (P < 0.05) compared with comparative example 1, comparative example 2, comparative example 3, example 6; the rate of change (%) = (after-use-before-use)/100% before use shown in fig. 13.
2. The skin color ita° values are shown in table 16 and fig. 14.
TABLE 16 skin color ITA value test results
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Note that: n=8, based on human face test; results were tested using T-test, which shows significant differences (p.ltoreq.0.05) compared to before use; # represents a significant difference (P < 0.05) compared with comparative example 1, comparative example 2, comparative example 3, example 6; the rate of change (%) = (after-use-before-use)/100% before use shown in fig. 14.
In summary, the skin color L x value is significantly increased after 21 days and 28 days of use of the product of the embodiment of the application, and the skin color ITA ° value is significantly increased after 28 days of use of the product, as compared with before use. The skin color L and ITA values were significantly improved after 7 days, 14 days, 21 days and 28 days of use of the inventive example product compared to the products of comparative examples 1-3. This shows that the product of the application has remarkable brightening effect.
While the application has been described in terms of preferred embodiments, it will be understood by those skilled in the art that various changes and modifications can be made without departing from the scope of the application, and it is intended that the application is not limited to the specific embodiments disclosed.
Claims (10)
1. Use of cerium oxide for the preparation of a soothing, repairing and/or lightening product.
2. The use according to claim 1, wherein the cerium oxide is spherical;
the particle size of the cerium oxide is 0.1-20 mu m;
the cerium oxide is prepared by a water/solvent thermal method;
preferably, the particle size of the cerium oxide is 0.2-0.5 μm;
Preferably, the particle size of the cerium oxide is 0.3 μm;
Preferably, the preparation process of the cerium oxide comprises the following steps: mixing cerium nitrate with water to obtain a precursor solution; adding acetic acid into the precursor solution to obtain a first solution; adding ethylene glycol into the first solution, and uniformly mixing to obtain a second solution; heating the second solution to obtain the cerium oxide;
Preferably, the temperature of the heating reaction is 160-170 ℃;
the heating reaction time is 155-165 min;
the pressure of the heating reaction is 0.4-0.6 Mpa;
Preferably, the temperature of the heating reaction is 165 ℃;
the heating reaction time is 160min;
The pressure of the heating reaction is 0.5Mpa;
the product comprises a cosmetic;
Preferably, in the application process, the addition amount of the cerium oxide is 0.05-2%;
Preferably, in the application process, the addition amount of the cerium oxide is 0.5-1.5%;
preferably, the cerium oxide is added in an amount of 1% during the application.
3. The soothing and repairing composition is characterized by comprising the following components in parts by mass: 0.05 to 2 parts of cerium oxide, 1 to 10 parts of emulsifying agent, 1 to 10 parts of thickening agent, 5 to 50 parts of emollient, 0.1 to 20 parts of humectant, 0.01 to 2 parts of chelating agent and 1 to 95 parts of water.
4. A soothing repair composition according to claim 3, comprising the following components in parts by mass: 0.2 to 1 part of cerium oxide, 1 to 5 parts of emulsifying agent, 1 to 5 parts of thickening agent, 5 to 10 parts of emollient, 5 to 10 parts of humectant, 0.01 to 0.05 part of chelating agent and 60 to 90 parts of water.
5. A soothing composition according to claim 3, wherein the cerium oxide is spherical;
the particle size of the cerium oxide is 0.1-20 mu m;
the cerium oxide is prepared by a water/solvent thermal method;
preferably, the particle size of the cerium oxide is 0.2-0.5 μm;
Preferably, the particle size of the cerium oxide is 0.3 μm;
Preferably, the preparation process of the cerium oxide comprises the following steps: mixing cerium nitrate with water to obtain a precursor solution; adding acetic acid into the precursor solution to obtain a first solution; adding ethylene glycol into the first solution, and uniformly mixing to obtain a second solution; heating the second solution to obtain the cerium oxide;
Preferably, the temperature of the heating reaction is 160-170 ℃;
the heating reaction time is 155-165 min;
the pressure of the heating reaction is 0.4-0.6 Mpa;
Preferably, the temperature of the heating reaction is 165 ℃;
the heating reaction time is 160min;
The pressure of the heating reaction is 0.5Mpa.
6. A soothing and repairing composition according to claim 3, wherein the emulsifier comprises at least one of polyol ester type emulsifier, alkyl glycoside type emulsifier, span and tween type emulsifier, phosphate ester type emulsifier, fatty alcohol polyether type emulsifier, polyglycerol type emulsifier, and high molecular polymer type emulsifier;
Preferably, the emulsifier comprises at least one of cetyl alcohol/cetostearyl glucoside/sucrose stearate, span 20, span 40, span 60, span 80, tween 120, polyglycerol-10 stearate, sorbitan fatty acid ester, polyoxyethylene sorbitan fatty acid ester;
Preferably, the thickener comprises at least one of polyacrylic acid, fatty alcohol and fatty acid, cellulose, natural gum and its modified substance, esters, inorganic macromolecule and its modified substance;
preferably, the thickener comprises at least one of cetostearyl alcohol, pentaerythritol distearate, ammonium acryloyldimethyl taurate/VP copolymer, starch, acacia, pectin, agar, gelatin, seaweed gel, carrageenan, dextrin;
Preferably, the thickener is a combination of cetostearyl alcohol, pentaerythritol distearate, ammonium acryloyldimethyl taurate/VP copolymer;
preferably, the mass ratio of cetostearyl alcohol, pentaerythritol distearate and acrylamide dimethyl taurate/VP copolymer in the composition is 1-2:0.5-1:0.1-0.5;
Preferably, the mass ratio of cetostearyl alcohol, pentaerythritol distearate, ammonium acryloyldimethyl taurate/VP copolymer in the composition is 1.5:0.8:0.3;
Preferably, the emollient comprises at least one of high molecular polymers, vegetable oils, animal oils, mineral oils, synthetic oils;
Preferably, the emollient comprises at least one of polydimethylsiloxane, hydrogenated polyisobutene, ethylhexyl palmitate, coconut oil, olive oil, palm oil, lanolin, beeswax, jojoba oil, mineral oil, petrolatum;
Preferably, the emollient is a combination of polydimethylsiloxane, hydrogenated polyisobutene, ethylhexyl palmitate;
Preferably, the mass ratio of the polydimethylsiloxane, the hydrogenated polyisobutene and the ethylhexyl palmitate in the composition is 1-3:4:1-3;
Preferably, the mass ratio of the polydimethylsiloxane, the hydrogenated polyisobutene and the ethylhexyl palmitate in the composition is 2:4:2;
preferably, the humectant comprises at least one of natural moisturizing factor, polyalcohol humectant, polymer biochemical humectant and amino acid humectant;
preferably, the humectant comprises at least one of glycerol, butylene glycol, glycerol polyether-26, trehalose;
preferably, the humectant is a combination of glycerin and butylene glycol;
preferably, in the composition, the mass ratio of glycerin to butanediol is 3-5:3;
preferably, the mass ratio of glycerin to butylene glycol in the composition is 4:3;
Preferably, the chelating agent comprises a hydroxy acid chelating agent and/or an amino acid derivative chelating agent;
Preferably, the chelating agent comprises at least one of disodium EDTA, ethylenediamine tetraacetic acid tetrasodium salt, and disodium nitrilotriacetate;
Preferably, the composition further comprises 0.1-5 parts of preservative;
preferably, the composition further comprises 0.5-1 part of preservative;
Preferably, the preservative comprises at least one of an alcohol preservative, a paraben preservative, methyl chloroisothiazolinone and methyl isothiazolinone, a formaldehyde releaser preservative, and an acid preservative;
Preferably, the preservative comprises at least one of phenoxyethanol/ethylhexyl glycerol, methyl benzoate, ethyl benzoate, propyl benzoate, sorbic acid, benzoic acid, dehydroacetic acid.
7. A process for the preparation of a soothing composition according to any one of claims 3 to 6, comprising the steps of:
And uniformly mixing a mixture containing cerium oxide, water, a humectant, a chelating agent, an emulsifying agent, a thickening agent and an emollient to obtain the soothing and repairing composition.
8. A method of preparing a soothing repair composition according to claim 7 comprising the steps of:
(1) Mixing cerium oxide with water, heating to 80-85 ℃, homogenizing, adding a humectant and a chelating agent, and stirring under heat preservation to obtain a mixture 1;
(2) Mixing an emulsifying agent, a thickening agent and an emollient, heating to 80-85 ℃, and preserving heat to obtain a mixture 2;
(3) Homogenizing the mixture 1, adding the mixture 2 in the homogenizing process, and carrying out heat preservation and stirring after homogenizing to obtain a mixture 3;
(4) And (3) cooling the mixture 3 to 30-40 ℃, adding a preservative, and stirring uniformly to obtain the relief repair composition.
9. A method of preparing a soothing repair composition according to claim 8 wherein in step (1) the homogenising speed is from 3000 to 4000rpm;
the homogenizing time is 1-5 min;
the rotation speed of the heat preservation stirring is 50-150 rpm;
the time of heat preservation and stirring is 25-35 min;
preferably, in the step (1), the homogenizing rotation speed is 3000-3500 rpm;
the homogenizing time is 2-4 min;
The rotation speed of the heat preservation stirring is 80-120 rpm;
the time of heat preservation and stirring is 28-32 min;
Preferably, in the step (3), the homogenizing rotation speed is 3000-4000 rpm;
The homogenizing time is 5-15 min;
the rotation speed of the heat preservation stirring is 50-150 rpm;
the time of heat preservation and stirring is 25-35 min;
preferably, in the step (3), the homogenizing rotation speed is 3400-3600 rpm;
the homogenizing time is 8-12 min;
The rotation speed of the heat preservation stirring is 80-120 rpm;
The time of heat preservation and stirring is 28-32 min.
10. Use of a soothing composition according to any one of claims 3 to 6 or a soothing composition prepared by a method according to any one of claims 7 to 9 in the preparation of a cosmetic.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410299876.4A CN118178228A (en) | 2024-03-15 | 2024-03-15 | Application of cerium oxide in preparation of relieving, repairing and/or brightening products |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410299876.4A CN118178228A (en) | 2024-03-15 | 2024-03-15 | Application of cerium oxide in preparation of relieving, repairing and/or brightening products |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN118178228A true CN118178228A (en) | 2024-06-14 |
Family
ID=91409532
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202410299876.4A Pending CN118178228A (en) | 2024-03-15 | 2024-03-15 | Application of cerium oxide in preparation of relieving, repairing and/or brightening products |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN118178228A (en) |
-
2024
- 2024-03-15 CN CN202410299876.4A patent/CN118178228A/en active Pending
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