CN117017833A - Compound with multiple-effect repairing and anti-aging effects and preparation method thereof - Google Patents
Compound with multiple-effect repairing and anti-aging effects and preparation method thereof Download PDFInfo
- Publication number
- CN117017833A CN117017833A CN202311158649.1A CN202311158649A CN117017833A CN 117017833 A CN117017833 A CN 117017833A CN 202311158649 A CN202311158649 A CN 202311158649A CN 117017833 A CN117017833 A CN 117017833A
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- Prior art keywords
- freeze
- dried powder
- compound
- water
- aging effects
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- GVJHHUAWPYXKBD-UHFFFAOYSA-N (±)-α-Tocopherol Chemical compound OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-UHFFFAOYSA-N 0.000 claims abstract description 20
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- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 claims abstract description 13
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- ROTFCACGLKOUGI-JYJNAYRXSA-N (2s)-2-[[(2s)-2-[[(2s)-2-(3-acetamidopropanoylamino)-3-(1h-imidazol-5-yl)propanoyl]amino]-3-hydroxypropanoyl]amino]-3-(1h-imidazol-5-yl)propanoic acid Chemical compound C([C@H](NC(=O)CCNC(=O)C)C(=O)N[C@@H](CO)C(=O)N[C@@H](CC=1NC=NC=1)C(O)=O)C1=CN=CN1 ROTFCACGLKOUGI-JYJNAYRXSA-N 0.000 claims abstract description 11
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Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
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Abstract
The invention belongs to the technical field of skin care products, and discloses a compound with multiple-effect repairing and anti-aging effects and a preparation method thereof. The compound comprises freeze-dried powder and solvent liquid matched with the freeze-dried powder for use; the freeze-dried powder comprises astaxanthin, vitamin E, mannitol, sodium hyaluronate, acetyl tetrapeptide-5, fullerene, polyquaternary ammonium salt-10 and glyceroglycolipid; the solvent liquid comprises water, glycerol, butanediol, centella asiatica extract, passion fruit extract, tremella polysaccharide, water-soluble polysiloxane film forming agent and disodium hydrogen phosphate. The compound has synergistic whitening, anti-aging and repairing effects through the addition of functional active components in the freeze-dried powder and the solvent. And further, the anionic water-soluble polysiloxane with a specific structure is used as a film forming agent, so that the skin feel of the product can be obviously improved, and the moisturizing effect of the product can be improved.
Description
Technical Field
The invention belongs to the technical field of skin care products, and particularly relates to a compound with multiple-effect repairing and anti-aging effects and a preparation method thereof.
Background
With the improvement of living standard, consumers are paying more attention to the ingredients and efficacy of cosmetic formulations. However, highly active ingredients are often unstable in physicochemical properties, and particularly lose or lose activity very easily under normal temperature and liquid conditions. Because the vacuum freeze-drying technology is carried out in a low-temperature and low-oxygen environment, most biological reactions are stagnant, liquid water is not present in the treatment process, and moisture is directly sublimated in a solid state, so that the damage to the structure and the characteristics of tissues and cells is small, the original structure and the shape of the materials are protected to the greatest extent, meanwhile, the freeze-drying technology effectively retains the original characteristics of components, particularly improves the stability of a plurality of thermosensitive active components, protects and retains the activities of some higher biological activity or easily-oxidized components, and finally can obtain a high-quality dried product with both appearance and internal quality. The color of the freeze-dried powder product is not changed basically after drying, the morphological structure is loose, and the freeze-dried powder product can be quickly dissolved and restored to a solution form after being added with solvents such as water and the like, and the freeze-dried powder product presents the original physicochemical property and biological activity. In addition, in view of the preparation principle of the freeze-dried powder, the moisture content in the freeze-dried powder is very low, so that the stability of the product is greatly improved, the transportation is convenient, and the storage life of the product is prolonged.
CN 114259418A discloses a polypeptide lyophilized powder comprising a peptide and an excipient to which the peptide is easily attached; the peptide comprises 0.1-2 parts by weight of oligopeptide-1, 0.1-2 parts by weight of tripeptide-1 and 0.1-2 parts by weight of oligopeptide-1; the excipient comprises mannitol 4-25 weight parts, disodium hydrogen phosphate 0.5-1.0 weight parts, and sodium dihydrogen phosphate 0.6-1.2 weight parts. The polypeptide freeze-dried powder preparation can be prepared by compounding the freeze-dried powder and solvent liquid. The method effectively protects the stability of the effective components of a plurality of thermosensitive biological products. But the freeze-dried powder adopts single polypeptide component, the used oligopeptide-1 has safety risk, and the development of the freeze-dried powder and the compound preparation with safer and more comprehensive efficacy has good market prospect.
CN 113171318A discloses a freeze-dried powder preparation with multiple effects of moisturizing, whitening, relieving and repairing. The raw materials of the freeze-dried powder preparation comprise the following components: mannitol, dipotassium glycyrrhizinate, cell complex biological peptide, tripeptide-1 copper, nicotinamide, glycyrrhiza glabra root extract and grape seed extract. The lyophilized powder preparation has four-in-one effects of moisturizing, whitening, relieving and repairing.
Due to the morphological characteristics of the freeze-dried powder, the freeze-dried powder is matched with a solvent liquid for use in application, and the solvent liquid plays a key role in the performance of the functional components of the freeze-dried powder. Patent CN 115212133A discloses a freeze-dried powder solvent, which is prepared from water, glycerol, propylene glycol, 1, 2-hexanediol, p-hydroxyacetophenone, butanediol, saccharide isomers, trehalose and oat peptide. The freeze-dried powder solvent is matched with each other through various components, and has synergistic effect, excellent moisturizing and anti-wrinkle effects, the skin hydration capacity is improved, the elastin generation is promoted, and cells are rich in elasticity; the skin antioxidation capability can be improved, melanin precipitation is effectively prevented, the skin is kept bright, and the health and freshness of the skin are maintained; improving the repairing effect of skin.
The existing freeze-dried powder and solvent liquid components generally pay attention to whether the efficacy is comprehensive or not, so active ingredients with high content such as repairing and whitening are used, however, the active ingredients with the efficacy are generally components such as polypeptide, hyaluronic acid, plant extracts, fullerene and the like, the defect of poor film forming spreadability exists, and the skin is easy to feel tight when the freeze-dried powder and solvent liquid are applied to the skin. How to improve the skin feel of the freeze-dried powder and the compound preparation when in use is a technical problem which needs to be solved by the technicians in the field.
Disclosure of Invention
In view of the above drawbacks and shortcomings of the prior art, a primary object of the present invention is to provide a composite with multiple-effect repair and anti-aging effects. The compound has synergistic whitening, anti-aging and repairing effects through the addition of various functional active components, and improves the skin feel through the specific water-soluble polysiloxane film forming agent.
Another object of the present invention is to provide a method for preparing the above-mentioned complex having multiple-effect repairing and anti-aging effects.
The invention aims at realizing the following technical scheme:
a compound with multiple-effect repairing and anti-aging effects comprises lyophilized powder and solvent solution matched with the lyophilized powder; the freeze-dried powder comprises astaxanthin, vitamin E, mannitol, sodium hyaluronate, acetyl tetrapeptide-5, fullerene, polyquaternary ammonium salt-10 and glyceroglycolipid; the solvent liquid comprises water, glycerol, butanediol, centella asiatica extract, passion fruit extract, tremella polysaccharide, water-soluble polysiloxane film forming agent and disodium hydrogen phosphate.
Further, the water-soluble polysiloxane film forming agent is water-soluble polysiloxane with an anionic structure, and is prepared by the following method:
adding hydrogen-containing silicone oil and allyl polyoxyethylene ether into an alcohol solvent to be uniformly dissolved, heating to 70-85 ℃, adding a chloroplatinic acid catalyst, stirring and reacting until the alkenyl reaction is complete, adding maleic anhydride, continuously carrying out heat preservation and reacting for 0.5-2 h, and vacuum drying to remove the solvent, thereby obtaining the water-soluble polysiloxane with the anionic structure.
Further preferably, the hydrogen-containing silicone oil is a hydrogen-containing silicone oil having a (active) hydrogen content of 0.1% to 0.9% and a viscosity of 50 to 500mpa.s at 25 ℃.
Further preferably, the molecular weight of the allyl polyoxyethylene ether is 200 to 2000.
Further preferably, the addition amount of the allyl polyoxyethylene ether is 0.05 to 0.5 times of the molar amount of hydrogen contained in the hydrogen-containing silicone oil.
Further preferably, the addition amount of the maleic anhydride is 0.8 to 1 time of the molar amount of the allyl polyoxyethylene ether.
Further, the freeze-dried powder comprises the following raw material components in parts by weight:
further, the solvent liquid comprises the following raw material components in parts by weight:
further, in the compound with multiple-effect repairing and anti-aging effects, the ratio of the freeze-dried powder to the solvent is 50-200 mg:1-10 mL.
The preparation method of the compound with the multiple-effect repairing and anti-aging effects comprises the following preparation steps:
(1) Preparing freeze-dried powder: adding astaxanthin, vitamin E and glyceroglycolipid into ethanol, dissolving uniformly, adding fullerene, stirring and dispersing uniformly to obtain ethanol mixed solution; mannitol, sodium hyaluronate, acetyl tetrapeptide-5 and polyquaternium-10 are added into water to be dissolved uniformly, so as to obtain an aqueous solution; homogenizing and mixing the ethanol mixed solution and the aqueous solution, filtering to remove insoluble substances, and vacuum freeze-drying to obtain freeze-dried powder;
(2) Preparing solvent liquid: adding glycerol, butanediol and water-soluble polysiloxane film forming agent into water, stirring and dissolving uniformly, adding herba Centellae extract, herba Passiflorae Caeruleae fruit extract and tremella polysaccharide, stirring and dissolving uniformly, and finally adding disodium hydrogen phosphate and dissolving uniformly to obtain a vehicle solution;
(3) The freeze-dried powder and the solvent liquid are mixed according to a proportion, dissolved and dispersed uniformly to obtain the compound with multiple-effect repairing and anti-aging effects.
Further, in the preparation process of the freeze-dried powder, the mass ratio of the ethanol to the water is kept to be 1-3:1 when the ethanol mixed solution and the water solution are uniformly stirred and mixed.
Compared with the prior art, the invention has the beneficial effects that:
(1) The invention adopts anion water-soluble polysiloxane with a specific structure as a film forming agent, and can form a soft polysiloxane film with polyquaternium-10 through ion adsorption codeposition in the use process, thereby remarkably improving the use skin feel and improving the moisturizing effect of the product.
(2) The invention has synergistic whitening, anti-aging and repairing effects through the addition of functional active components in the freeze-dried powder and the solvent.
(3) The freeze-dried powder adopts the specific glyceroglycolipid as the carrier and the protective agent of the effective active ingredients, has obvious function of stabilizing the effective active ingredients, and can better synergistically improve the effects of moisturizing, repairing and relieving.
(4) The invention adopts the specific polyquaternium-10 as the forming auxiliary agent of the freeze-dried powder, and can reduce the particle size of the freeze-dried powder and obviously promote the dissolution and dispersion effects of the freeze-dried powder in aqueous solvent by controlling the ratio of solvent ethanol to water in the preparation process of the freeze-dried powder.
Detailed Description
The present invention will be described in further detail with reference to examples, but embodiments of the present invention are not limited thereto.
Example 1
The compound with multiple-effect repairing and anti-aging effects comprises freeze-dried powder and solvent liquid matched with the freeze-dried powder.
The freeze-dried powder is prepared by the following method:
(1) According to the mass parts, 4 parts of astaxanthin, 6 parts of vitamin E and 20 parts of glyceroglycolipid are added into 100 parts of ethanol for uniform dissolution, and then 3 parts of fullerene is added for uniform stirring and dispersion, thus obtaining ethanol mixed solution.
(2) 8 parts of mannitol, 2 parts of sodium hyaluronate, 5 parts of acetyl tetrapeptide-5 and 3 parts of polyquaternary ammonium salt-10 are added into 50 parts of water to be uniformly dissolved, so as to obtain an aqueous solution.
(3) And (3) homogenizing and mixing the ethanol mixed solution in the step (1) and the aqueous solution in the step (2), filtering to remove insoluble substances, and performing vacuum freeze drying to obtain the whitening compact repairing freeze-dried powder.
The solvent liquid is prepared by the following method:
according to the mass parts, adding 4 parts of glycerin, 3 parts of butanediol and 2 parts of water-soluble polysiloxane film forming agent into 86.8 parts of water, stirring and dissolving uniformly, adding 1.5 parts of centella asiatica extract, 1.5 parts of passion fruit extract and 1 part of tremella polysaccharide, stirring and dissolving uniformly, and finally adding 0.2 part of disodium hydrogen phosphate, dissolving uniformly, thus obtaining the solvent.
The water-soluble polysiloxane film forming agent is water-soluble polysiloxane with an anionic structure, and is prepared by the following method:
adding hydrogen-containing silicone oil with hydrogen content of 0.45% and viscosity of 150mPa.s at 25 ℃ and allyl polyoxyethylene ether with average molecular weight of 800 into ethanol solvent, and dissolving uniformly, wherein the addition amount of the allyl polyoxyethylene ether is 0.3 times of the molar weight of hydrogen contained in the hydrogen-containing silicone oil. Then heating to 75-80 ℃, adding chloroplatinic acid catalyst, stirring and reacting until the alkenyl reaction is complete, adding maleic anhydride, continuously preserving heat and reacting for 2 hours, wherein the adding amount of the maleic anhydride is 1 time of the molar amount of the allyl polyoxyethylene ether, and vacuum drying to remove the solvent, thus obtaining the water-soluble polysiloxane with the anionic structure.
When in use, the freeze-dried powder and the solvent liquid are mixed, dissolved and uniformly dispersed according to the proportion of 100mg to 5mL, so as to obtain the compound with multiple-effect repairing and anti-aging effects.
In the embodiment, the mass ratio of the mixed solution solvent ethanol to water before vacuum freeze drying in the preparation process of the freeze-dried powder is respectively regulated to be 0.5:1, 1:1, 2:1, 3:1 and 4:1, and the total addition amount of the ethanol and the water is 150 parts by weight and is kept unchanged. The average particle diameter and the dissolution time (the time from shaking table mixing to complete dissolution and dispersion uniformity) of the obtained lyophilized powder were respectively measured, and the results are shown in table 1 below.
TABLE 1
Test sample | Average particle diameter | Dissolution time |
0.5:1 | 465.4nm | 1min43s |
1:1 | 245.3nm | 56s |
2:1 | 158.6nm | 45s |
3:1 | 212.7nm | 51s |
4:1 | 328.2nm | 1min15s |
As shown in table 1, the particle size of the obtained lyophilized powder tended to decrease and increase with increasing mass ratio of ethanol to water in the mixed solution solvent before lyophilization, and the smaller the particle size was, the shorter the dissolution time was. Under the condition that the mass ratio of the ethanol to the water is 1-3:1, the dissolution and dispersion time of the obtained freeze-dried powder in the solvent liquid can be controlled within 1 min.
Example 2
The compound with multiple-effect repairing and anti-aging effects comprises freeze-dried powder and solvent liquid matched with the freeze-dried powder.
The freeze-dried powder is prepared by the following method:
(1) According to the mass parts, 2 parts of astaxanthin, 8 parts of vitamin E and 15 parts of glyceroglycolipid are added into 80 parts of ethanol for uniform dissolution, and then 2 parts of fullerene is added for uniform stirring and dispersion, thus obtaining ethanol mixed solution.
(2) 5 parts of mannitol, 1 part of sodium hyaluronate, 6 parts of acetyl tetrapeptide-5 and 2 parts of polyquaternary ammonium salt-10 are added into 40 parts of water to be uniformly dissolved, so as to obtain an aqueous solution.
(3) And (3) homogenizing and mixing the ethanol mixed solution in the step (1) and the aqueous solution in the step (2), filtering to remove insoluble substances, and performing vacuum freeze drying to obtain the whitening compact repairing freeze-dried powder.
The solvent liquid is prepared by the following method:
according to the mass parts, adding 6 parts of glycerin, 1 part of butanediol and 0.5 part of water-soluble polysiloxane film forming agent into 82.1 parts of water, stirring and dissolving uniformly, adding 4 parts of centella asiatica extract, 4 parts of passion fruit extract and 2 parts of tremella polysaccharide, stirring and dissolving uniformly, and finally adding 0.4 part of disodium hydrogen phosphate, dissolving uniformly, thus obtaining the solvent.
The water-soluble polysiloxane film forming agent is water-soluble polysiloxane with an anionic structure, and is prepared by the following method:
adding hydrogen-containing silicone oil with hydrogen content of 0.55% and viscosity of 250mPa.s at 25 ℃ and allyl polyoxyethylene ether with average molecular weight of 1200 into ethanol solvent, and dissolving uniformly, wherein the addition amount of the allyl polyoxyethylene ether is 0.2 times of the molar weight of hydrogen contained in the hydrogen-containing silicone oil. Then heating to 75-80 ℃, adding chloroplatinic acid catalyst, stirring and reacting until the alkenyl reaction is complete, adding maleic anhydride, continuously preserving heat and reacting for 2 hours, wherein the adding amount of the maleic anhydride is 1 time of the molar amount of the allyl polyoxyethylene ether, and vacuum drying to remove the solvent, thus obtaining the water-soluble polysiloxane with the anionic structure.
When in use, the freeze-dried powder and the solvent liquid are mixed, dissolved and uniformly dispersed according to the proportion of 100mg to 3mL, so as to obtain the compound with multiple-effect repairing and anti-aging effects.
Example 3
The compound with multiple-effect repairing and anti-aging effects comprises freeze-dried powder and solvent liquid matched with the freeze-dried powder.
The freeze-dried powder is prepared by the following method:
(1) According to the mass parts, adding 6 parts of astaxanthin, 4 parts of vitamin E and 30 parts of glyceroglycolipid into 120 parts of ethanol for uniform dissolution, and then adding 4 parts of fullerene for uniform stirring and dispersion to obtain an ethanol mixed solution.
(2) 10 parts of mannitol, 3 parts of sodium hyaluronate, 3 parts of acetyl tetrapeptide-5 and 5 parts of polyquaternary ammonium salt-10 are added into 60 parts of water to be uniformly dissolved, so as to obtain an aqueous solution.
(3) And (3) homogenizing and mixing the ethanol mixed solution in the step (1) and the aqueous solution in the step (2), filtering to remove insoluble substances, and performing vacuum freeze drying to obtain the whitening compact repairing freeze-dried powder.
The solvent liquid is prepared by the following method:
according to the mass parts, adding 2 parts of glycerin, 5 parts of butanediol and 4 parts of water-soluble polysiloxane film forming agent into 86.4 parts of water, stirring and dissolving uniformly, adding 1 part of centella asiatica extract, 1 part of passion fruit extract and 0.5 part of tremella polysaccharide, stirring and dissolving uniformly, and finally adding 0.1 part of disodium hydrogen phosphate, dissolving uniformly, thus obtaining the solvent.
The water-soluble polysiloxane film forming agent is water-soluble polysiloxane with an anionic structure, and is prepared by the following method:
adding hydrogen-containing silicone oil with the hydrogen content of 0.36% and the viscosity of 200mPa.s at 25 ℃ and allyl polyoxyethylene ether with the average molecular weight of 1000 into an ethanol solvent, and uniformly dissolving, wherein the adding amount of the allyl polyoxyethylene ether is 0.4 times of the molar weight of hydrogen contained in the hydrogen-containing silicone oil. Then heating to 75-80 ℃, adding chloroplatinic acid catalyst, stirring and reacting until the alkenyl reaction is complete, adding maleic anhydride, continuously preserving heat and reacting for 2 hours, wherein the addition amount of the maleic anhydride is 0.9 times of the molar amount of the allyl polyoxyethylene ether, and vacuum drying to remove the solvent, thus obtaining the water-soluble polysiloxane with the anionic structure.
When in use, the freeze-dried powder and the solvent liquid are mixed, dissolved and uniformly dispersed according to the proportion of 100mg to 5mL, so as to obtain the compound with multiple-effect repairing and anti-aging effects.
Comparative example 1
In this comparative example, the preparation process of the lyophilized powder was not added with polyquaternium-10, and the rest was the same.
The lyophilized powders obtained in example 1 and comparative example were each tested for the average particle size and dissolution time in a solvent liquid, and the results are shown in table 2 below.
TABLE 2
Test sample | Average particle diameter | Dissolution time |
Example 1 | 158.6nm | 45s |
Comparative example 1 | 652.7nm | 2min56s |
As can be seen from the results in table 2, the invention adopts the specific polyquaternium-10 as the forming auxiliary agent of the freeze-dried powder, which can reduce the particle size of the freeze-dried powder and obviously promote the dissolution and dispersion of the freeze-dried powder in the aqueous solvent.
Comparative example 2
In this comparative example, compared with example 1, no glyceroglycolipid was added during the preparation of the lyophilized powder, and the remaining components were the same.
Comparative example 3
Compared with the example 1, the freeze-dried powder adopts the same amount of trehalose to replace glyceroglycolipid in the preparation process, and the rest components are the same.
Comparative example 4
Compared with the example 1, the freeze-dried powder is prepared without adding astaxanthin and vitamin E, and the rest components are the same.
Comparative example 5
In this comparative example, sodium hyaluronate and acetyl tetrapeptide-5 were not added during the preparation of the lyophilized powder as in example 1, and the remaining components were the same.
Comparative example 6
Compared with the example 1, the comparative example has the advantages that fullerene is not added in the preparation process of the freeze-dried powder, and the rest components are the same.
Comparative example 7
In this comparative example, as compared with example 1, no water-soluble polysiloxane film former was added during the solvent liquid preparation, and the remaining components were the same.
Comparative example 8
Compared with the example 1, the comparative example adopts equivalent nonionic structure water-soluble polysiloxane to replace anionic structure water-soluble polysiloxane in the solvent liquid preparation process, and the rest components are the same. Compared with the preparation process of the water-soluble polysiloxane with the anion structure, the water-soluble polysiloxane with the nonionic structure is not added with maleic anhydride for anion modification, and the rest is the same, and the specific preparation process is as follows:
adding hydrogen-containing silicone oil with hydrogen content of 0.45% and viscosity of 150mPa.s at 25 ℃ and allyl polyoxyethylene ether with average molecular weight of 800 into ethanol solvent, and dissolving uniformly, wherein the addition amount of the allyl polyoxyethylene ether is 0.3 times of the molar weight of hydrogen contained in the hydrogen-containing silicone oil. Then heating to 75-80 ℃, adding chloroplatinic acid catalyst, stirring and reacting until the alkenyl reaction is complete, and vacuum drying to remove the solvent to obtain the nonionic structure water-soluble polysiloxane.
The composites obtained in the above examples and comparative examples were subjected to application performance tests:
1. skin feel test
55 female volunteers aged 25-40 years were selected and randomized into 11 groups of 5 persons each of examples 1-3 and comparative examples 1-8, respectively. The face of the subject is uniformly looped and smeared with 0.5g of sample to be measured, and the soft and moist skin feeling of the skin of the face after being smeared is scored, wherein the soft skin feeling is the best 5 minutes, the skin tightening feeling is the worst 1 minute, and the average value is taken, and the result is shown in the following table 3.
TABLE 3 Table 3
Test sample | Skin feel score |
Example 1 | 4.8 |
Example 2 | 4.6 |
Example 3 | 5.0 |
Comparative example 1 | 4.2 |
Comparative example 2 | 5.0 |
Comparative example 3 | 4.6 |
Comparative example 4 | 4.6 |
Comparative example 5 | 4.6 |
Comparative example 6 | 4.8 |
Comparative example 7 | 3.2 |
Comparative example 8 | 4.0 |
As can be seen from the results of comparative example 7 in table 3, the present invention can significantly improve the skin feel of the sample using the water-soluble polysiloxane with a specific anionic structure as the film forming agent, and it can be further found from the results of comparative example 1 and comparative example 8 that the polyquaternium-10 and the water-soluble polysiloxane with an anionic structure have a significant synergistic effect in improving the skin feel of the sample using, probably because the polyquaternium-10 and the water-soluble polysiloxane with an anionic structure are co-deposited into a film by ion adsorption to contribute to the improvement of the soft skin feel.
2. Moisture effect test
The testing method comprises the following steps:
under constant environmental conditions, a negative control group and a positive control group were set, the positive control group was 5% glycerol, the negative control group was deionized water, and the operation procedure was consistent with that of the sample group.
1. Placing color-changing silica gel at the bottom of the dryer, attaching 3M air-permeable adhesive tape onto glass plate, placing into the dryer one day in advance, and weighing M 0 ;
2. Accurately weighing the sample, and then weighing the sample by 2 mg+/-0.1 mg/cm according to the size of the adhesive tape 2 Weighing corresponding sample and reference substance, uniformly coating on adhesive tape, and weighing its weight M 1 ;
3. Placing the glass plate coated with the object to be measured into a dryer, and accurately weighing the mass M after 2 hours, 4 hours and 6 hours t ;
4. The formula for calculating the moisture retention (P) refers to the following formula:
moisture retention (%) = (M t –M 0 )/(M 1 –M 0 )×100%;
5. Relative moisture retention: comparison of the moisture retention properties of the test samples with 5% glycerol under the same conditions;
6. the relative moisture retention calculation formula is referred to below
Relative moisture retention (%) = (P) t –P 0 )/(P Glycerol –P 0 )×100%;
Wherein: pt-the moisture retention rate of the sample to be measured after t hours;
p0-moisture retention after t hours for negative control;
P glycerol Positive control% moisture retention after t hours.
The relative moisture retention rate evaluation results of the above examples and comparative examples are shown in table 4 below.
TABLE 4 Table 4
The relative moisture retention rate is lower than 0-50%, 50-100% is middle, 100-150% is high, and 150% is good. Tests show that the relative moisture retention rate of the sample solution in the embodiment of the invention is above 150% in 2 hours, and the moisture retention performance is good; the relative moisture retention rates of 4h and 6h are above 100%, and the moisture retention performance is high. Wherein the comparative example 2 and comparative example 3 were free of added glyceroglycolipid or replaced with trehalose, and their moisturizing properties were significantly reduced. It is explained that the improvement effect of the glyceroglycolipid on the moisturizing performance is most remarkable in the system of the present invention. In addition, as can be seen from the results of comparative example 7, the water-soluble silicone film-forming agent also has a more remarkable effect of improving the moisturizing performance.
3. Test of soothing efficacy
The current study considers the occurrence of sensitive skin as a complex process involving skin barrier-neurovascular-immune inflammation. Hyaluronic acid is the component with the largest content and proportion in the extracellular matrix, can maintain the volume of the extracellular matrix, regulate and control the secretion of cell growth factors and cytokines, and influence the adhesion, growth, proliferation and differentiation of cells, thereby playing an important role in maintaining the skin moisture and elasticity, wound healing, angiogenesis and other processes.
Hyaluronidase is an endogenous amino hexose which causes the decomposition of macromolecular hyaluronic acid, has strong correlation with inflammation and allergy, and researches report that various medicines for releasing histamine by fat large cells can regulate the activity of the hyaluronidase, and some antiallergic medicines have strong inhibition of the activity of the hyaluronidase, so that the inhibition of the activity of the hyaluronidase is used as an index for researching the antiallergic effect.
The macromolecular hyaluronic acid is decomposed to generate the N-acetylglucosamine under the action of hyaluronidase, and the activity of the hyaluronidase can be indirectly reacted by measuring the N-acetylglucosamine content in a reaction system. The inhibition of the activity of the hyaluronidase can ensure the normal content and function of the hyaluronic acid, so that whether a test sample has the effect of relieving or not can be judged by utilizing the inhibition rate of the hyaluronidase activity, and the higher the inhibition rate of the hyaluronidase activity is, the stronger the relieving effect of the substance is reflected, and the weaker the relieving effect is on the contrary.
The testing method comprises the following steps:
and (3) taking a proper amount of sample and a solution of hyaluronidase and the like for color reaction, testing absorbance at 530nm, and calculating the inhibition rate (%) of the hyaluronidase activity.
Hyaluronidase inhibition ratio (%) = [ (C-D) - (a-B) ]/(C-D) ×100%;
wherein: OD value of a- (hyaluronidase + sample + potassium hyaluronate) sample solution;
OD value of B- (hyaluronidase + sample + acetate buffer) sample blank;
OD value of C- (hyaluronidase + deionized water + potassium hyaluronate) control solution;
d- (acetate buffer + deionized water + acetate buffer) versus OD value of blank.
The results of the soothing efficacy evaluation of the above examples and comparative examples are shown in Table 5 below.
TABLE 5
Test sample | Inhibition rate |
Example 1 | 58.7% |
Example 2 | 60.6% |
Example 3 | 52.8% |
Comparative example 1 | 58.5% |
Comparative example 2 | 43.6% |
Comparative example 3 | 44.7% |
Comparative example 4 | 50.2% |
Comparative example 5 | 44.5% |
Comparative example 6 | 48.2% |
Comparative example 7 | 56.2% |
Comparative example 8 | 55.7% |
As is apparent from the results in Table 5, the glyceroglycolipid of the present invention has a remarkable synergistic effect with sodium hyaluronate and acetyl tetrapeptide-5, and fullerene components in exerting the soothing effect of the product.
4. Whitening efficacy test
The testing method comprises the following steps: the 55 volunteers with darker complexion were screened and randomly divided into 11 groups of 5 volunteers. The skin red melanin tester and test probe (Mexameter MX18, CK, germany) were used to collect melanin MI data from the face prior to sample testing, and the data were used as skin background values. The sample was used once in the morning and evening by the test person, and data were collected after 4 weeks of continuous use. The change of the melanin content of the skin of the subject before and after the sample is tested is evaluated, so that the whitening effect is determined. The corresponding test results are shown in table 6 below.
Wherein, the melanin content change rate Δmi% = (T n -T 0 )/T 0 Averaging the final result; the higher Δmi% reduction value indicates better whitening efficacy.
Wherein T is n -the melanin content value of the tested area after 4 weeks of continuous use; t (T) 0 -initial value of melanin content of the test area.
TABLE 6
Test sample | △MI% |
Example 1 | -16.78 |
Example 2 | -16.52 |
Example 3 | -15.51 |
Comparative example 1 | -16.56 |
Comparative example 2 | -9.23 |
Comparative example 3 | -12.30 |
Comparative example 4 | -7.98 |
Comparative example 5 | -13.95 |
Comparative example 6 | -12.24 |
Comparative example 7 | -14.62 |
Comparative example 8 | -15.81 |
As apparent from the results in Table 6, the glyceroglycolipid, astaxanthin, vitamin E and fullerene components of the present invention have obvious synergistic effect in the effect of whitening the product.
5. Test of repair and anti-aging effects
The test method employs a method of promoting human skin fibroblast proliferation (MTT assay):
taking human skin fibroblast in logarithmic growth phase, digesting, preparing into 1×10 concentration with DMEM medium containing 15% fetal calf serum and 1% diabody 5 Cell suspension/mL, inoculated in 96-well plate at 150. Mu.L per well, 37℃and 5% CO 2 After culturing in an incubator for 24 hours, the culture medium is replaced by DMEM culture medium containing 50 mug/mL of sample to be tested, 15% fetal bovine serum and 1% double antibody for continuous culture, after continuous culture for 24 hours, the culture medium is sucked, PBS is used for washing, 150 mug of DMEM culture medium containing 15% fetal bovine serum and 1% double antibody and 20 mug LMTT solution (5 mg/mL) are added, 37 ℃ and 5% CO are added 2 Culturing for 4h, absorbing supernatant, adding 150 μl of DMSO into each well, shaking for 10min, and dissolving the crystals completely. Meanwhile, a control group is arranged, wherein the control group is to replace a sample to be tested with normal saline, and the rest is identical, and each group has 5 compound holes. Absorbance was measured at 490nm for each well, 5 sets of experiments were performed for each set, averaged, and proliferation rate calculated. Proliferation rate (%) = (absorbance value of sample to be measured-absorbance value of control group)/(absorbance value of control group×100%, the result is shown in table 7 below.
TABLE 7
Test sample | Proliferation promoting rate |
Example 1 | 128.6% |
Example 2 | 130.9% |
Example 3 | 127.5% |
Comparative example 1 | 128.7% |
Comparative example 2 | 93.2% |
Comparative example 3 | 99.6% |
Comparative example 4 | 110.7% |
Comparative example 5 | 84.2% |
Comparative example 6 | 87.3% |
Comparative example 7 | 126.9% |
Comparative example 8 | 125.4% |
As apparent from the results in Table 7, the glyceroglycolipid of the present invention has an obvious synergistic effect with sodium hyaluronate and acetyl tetrapeptide-5, and the fullerene component in the effect of product repair and anti-aging.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
Claims (10)
1. A compound with multiple-effect repairing and anti-aging effects is characterized by comprising freeze-dried powder and solvent liquid matched with the freeze-dried powder; the freeze-dried powder comprises astaxanthin, vitamin E, mannitol, sodium hyaluronate, acetyl tetrapeptide-5, fullerene, polyquaternary ammonium salt-10 and glyceroglycolipid; the solvent liquid comprises water, glycerol, butanediol, centella asiatica extract, passion fruit extract, tremella polysaccharide, water-soluble polysiloxane film forming agent and disodium hydrogen phosphate.
2. The compound with multiple-effect repairing and anti-aging effects according to claim 1, wherein the water-soluble polysiloxane film forming agent is an anionic structure water-soluble polysiloxane, and is prepared by the following method:
adding hydrogen-containing silicone oil and allyl polyoxyethylene ether into an alcohol solvent to be uniformly dissolved, heating to 70-85 ℃, adding a chloroplatinic acid catalyst, stirring and reacting until the alkenyl reaction is complete, adding maleic anhydride, continuously carrying out heat preservation and reacting for 0.5-2 h, and vacuum drying to remove the solvent, thereby obtaining the water-soluble polysiloxane with the anionic structure.
3. The compound with multiple-effect repairing and anti-aging effects according to claim 2, wherein the hydrogen-containing silicone oil is hydrogen-containing silicone oil with hydrogen content of 0.1-0.9% and viscosity of 50-500 mpa.s at 25 ℃; the molecular weight of the allyl polyoxyethylene ether is 200-2000.
4. The compound with multiple-effect repairing and anti-aging effects according to claim 3, wherein the addition amount of the allyl polyoxyethylene ether is 0.05-0.5 times of the hydrogen-containing molar amount of the hydrogen-containing silicone oil.
5. The compound with multiple-effect repairing and anti-aging effects according to claim 4, wherein the addition amount of the maleic anhydride is 0.8-1 times of the molar amount of the allyl polyoxyethylene ether.
6. The compound with multiple-effect repairing and anti-aging effects according to claim 1, wherein the freeze-dried powder comprises the following raw material components in parts by weight:
7. the compound with multiple-effect repairing and anti-aging effects according to claim 1, wherein the solvent liquid comprises the following raw material components in parts by weight:
8. the compound with multiple-effect repairing and anti-aging effects according to claim 1, wherein the ratio of the freeze-dried powder to the solvent is 50-200 mg:1-10 mL.
9. A method for preparing a compound having multiple-effect repairing and anti-aging effects as claimed in any one of claims 1 to 8, comprising the following steps:
(1) Preparing freeze-dried powder: adding astaxanthin, vitamin E and glyceroglycolipid into ethanol, dissolving uniformly, adding fullerene, stirring and dispersing uniformly to obtain ethanol mixed solution; mannitol, sodium hyaluronate, acetyl tetrapeptide-5 and polyquaternium-10 are added into water to be dissolved uniformly, so as to obtain an aqueous solution; homogenizing and mixing the ethanol mixed solution and the aqueous solution, filtering to remove insoluble substances, and vacuum freeze-drying to obtain freeze-dried powder;
(2) Preparing solvent liquid: adding glycerol, butanediol and water-soluble polysiloxane film forming agent into water, stirring and dissolving uniformly, adding herba Centellae extract, herba Passiflorae Caeruleae fruit extract and tremella polysaccharide, stirring and dissolving uniformly, and finally adding disodium hydrogen phosphate and dissolving uniformly to obtain a vehicle solution;
(3) The freeze-dried powder and the solvent liquid are mixed according to a proportion, dissolved and dispersed uniformly to obtain the compound with multiple-effect repairing and anti-aging effects.
10. The method for preparing the compound with multiple-effect repairing and anti-aging effects according to claim 9, wherein in the preparation process of the freeze-dried powder, the mass ratio of ethanol to water is kept within a range of 1-3:1 when the ethanol mixed solution and the aqueous solution are uniformly stirred and mixed.
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US20200405610A1 (en) * | 2016-12-29 | 2020-12-31 | Shaanxi Huikang Bio-Tech Co., Ltd. | Cosmetic composition |
CN115212133A (en) * | 2022-07-25 | 2022-10-21 | 广州丽彦妆生物科技有限公司 | Freeze-dried powder solvent and preparation method and application thereof |
CN116617145A (en) * | 2023-04-10 | 2023-08-22 | 上海优萃生物科技有限公司 | Rapid anti-aging repair composition and application thereof |
CN116898766A (en) * | 2023-06-26 | 2023-10-20 | 上海捷丽生物科技有限公司 | A lyophilized liquid, lyophilized film and repairing facial mask containing liposome active substances |
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JP2003342121A (en) * | 2002-05-28 | 2003-12-03 | Noevir Co Ltd | Skin care preparation |
CN104177620A (en) * | 2014-07-26 | 2014-12-03 | 张家港格瑞特化学有限公司 | Polyfunctional-group-modified polysiloxane emulsifier and preparation method thereof |
US20200405610A1 (en) * | 2016-12-29 | 2020-12-31 | Shaanxi Huikang Bio-Tech Co., Ltd. | Cosmetic composition |
CN115212133A (en) * | 2022-07-25 | 2022-10-21 | 广州丽彦妆生物科技有限公司 | Freeze-dried powder solvent and preparation method and application thereof |
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