CN111449986A - Compound anti-wrinkle-smoothing agent and preparation method thereof - Google Patents

Compound anti-wrinkle-smoothing agent and preparation method thereof Download PDF

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Publication number
CN111449986A
CN111449986A CN202010275641.3A CN202010275641A CN111449986A CN 111449986 A CN111449986 A CN 111449986A CN 202010275641 A CN202010275641 A CN 202010275641A CN 111449986 A CN111449986 A CN 111449986A
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sodium hyaluronate
wrinkle
compound anti
humectant
smoothing agent
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Pending
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CN202010275641.3A
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Chinese (zh)
Inventor
陈舒敏
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Guangzhou Disheng Biotechnology Co ltd
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Guangzhou Disheng Biotechnology Co ltd
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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
    • A61K8/73—Polysaccharides
    • A61K8/735—Mucopolysaccharides, e.g. hyaluronic acid; Derivatives thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/11—Encapsulated compositions
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/37—Esters of carboxylic acids
    • 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
    • A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
    • A61K8/89—Polysiloxanes
    • A61K8/891—Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • A61Q19/08—Anti-ageing preparations
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/56—Compounds, absorbed onto or entrapped into a solid carrier, e.g. encapsulated perfumes, inclusion compounds, sustained release forms

Abstract

The invention discloses a compound anti-wrinkle-smoothing agent and a preparation method thereof. The compound anti-wrinkle-smoothing agent comprises the following raw materials: 1-5% of dimethyl silyl silica, 0.05-2% of humectant, 0.05-0.5% of sodium hyaluronate, 0.1-1% of antiseptic synergistic humectant, 0.1-1% of preservative and the balance of ethylhexyl palmitate. The invention utilizes the micro-encapsulation technology to disperse sodium hyaluronate in a high polymer material matrix to form a micro spherical entity to realize encapsulation, and the sodium hyaluronate is uniformly dispersed in oil in a microsphere form, so that the sodium hyaluronate can be added into other oily products such as skin moistening cream emulsion, BB cream, lipstick and the like which mainly comprise oil phase to play a role in resisting wrinkles and smoothing wrinkles, the microspheres can burst when contacting the surface of skin, and the released small-molecule hyaluronic acid can quickly permeate into the skin to play an active role.

Description

Compound anti-wrinkle-smoothing agent and preparation method thereof
Technical Field
The invention relates to the technical field of cosmetics, in particular to a compound anti-wrinkle-smoothing agent and a preparation method thereof.
Background
Sodium hyaluronate is a kind of dextran aldehyde acid, has special water retention function, is the substance found to have the best moisture retention in nature at present, is called as an ideal natural moisture retention factor, and 2% of pure sodium hyaluronate aqueous solution can firmly retain 98% of water. However, sodium hyaluronate which is generally distributed on the market at present is insoluble in oil and fat, almost completely hydrophilic, and is not easily dispersed in an oil phase of a cosmetic, so that the sodium hyaluronate cannot be directly used in a product mainly comprising the oil phase.
Disclosure of Invention
The invention aims to provide a compound anti-wrinkle-smoothing agent and a preparation method thereof, so as to solve the technical problems.
In order to achieve the purpose, the technical scheme of the invention is as follows:
in a first aspect, the compound anti-wrinkle-smoothing agent provided by the invention comprises the following raw materials in percentage by weight: 1-5% of dimethyl silyl silica, 0.05-2% of humectant, 0.05-0.5% of sodium hyaluronate, 0.1-1% of antiseptic synergistic humectant, 0.1-1% of preservative and the balance of ethylhexyl palmitate.
Preferably, the humectant is selected from one or more of butanediol, propylene glycol and glycerol.
Further preferably, the humectant is butylene glycol.
Preferably, the preservative synergistic humectant is selected from one or more of caprylyl glycol and hexylene glycol.
Preferably, the antiseptic synergistic humectant comprises caprylyl glycol and hexylene glycol, wherein the addition amount of the caprylyl glycol in the compound type anti-wrinkle smoothing agent is 0.3-0.8%, and the addition amount of the hexylene glycol in the compound type anti-wrinkle smoothing agent is 0.05-0.2%.
Preferably, the weight ratio of the dimethylsilylated silica to the sodium hyaluronate is 10-15: 1.
Preferably, the compound anti-wrinkle-smoothing agent comprises the following raw materials in percentage by weight: 2 to 3.2% of dimethylsilylated silica, 0.8 to 1.2% of butanediol, 0.16 to 0.24% of sodium hyaluronate, 0.4 to 0.6% of caprylyl glycol, 0.08 to 0.12% of hexylene glycol, 0.3 to 0.5% of phenoxyethanol, and the balance being ethylhexyl palmitate.
Further preferably, the compound anti-wrinkle smoothing agent comprises the following raw materials in percentage by weight: 2.5% of dimethyl silyl silica, 1% of humectant, 0.2% of sodium hyaluronate, 0.6% of antiseptic synergistic humectant, 0.4% of preservative and the balance of ethylhexyl palmitate.
Preferably, the preservative is phenoxyethanol.
In a second aspect, the present invention provides a method for preparing a compound anti-wrinkle soothing agent according to the first aspect, including the following steps:
(1) dispersing and stirring sodium hyaluronate and humectant uniformly in advance for later use;
(2) heating ethylhexyl palmitate and silica dimethyl silylate to 80-90 ℃, and mixing and stirring uniformly;
(3) mixing the mixture obtained in the step (2) and the mixture obtained in the step (1), and homogenizing for 60-120 min;
(4) and (3) cooling the homogenized mixture to a temperature not higher than 45 ℃, adding the anticorrosion synergistic humectant and the preservative, uniformly stirring, and cooling.
Compared with the prior art, the invention has the beneficial effects that:
the invention utilizes the micro-encapsulation technology to disperse sodium hyaluronate in a high polymer material matrix to form a micro spherical entity to realize encapsulation, and the sodium hyaluronate is uniformly dispersed in oil in a microsphere form, so that the sodium hyaluronate can be added into other oily products such as skin moistening cream emulsion, BB cream, lipstick and the like which mainly comprise oil phase to play a role in resisting wrinkles and smoothing wrinkles, the microspheres can burst when contacting the surface of skin, and the released small-molecule hyaluronic acid can quickly permeate into the skin to play an active role.
Aiming at the problem of water-soluble sodium hyaluronate, the invention utilizes the hydrophilicity and lipophilicity of dimethyl silyl silica to form micro-capsule spheres of sodium hyaluronate and disperse the micro-capsule spheres in an oil phase through cross-linking polymerization reaction so as to be dispersed in the oil phase and fully play the roles of resisting wrinkles and smoothing wrinkles.
Drawings
Fig. 1 is a perspective electron microscope image of a sodium hyaluronate sphere before water absorption according to an embodiment of the present invention;
fig. 2 is a perspective electron microscope image of the sodium hyaluronate spheres after water absorption provided by the embodiment of the invention;
fig. 3 is a perspective electron microscope image of sodium hyaluronate spheres penetrating into skin according to the embodiment of the present invention;
fig. 4 is a perspective electron microscope image of the sodium hyaluronate spheres after swelling by water absorbed in skin provided by the embodiment of the present invention.
Detailed Description
The following further describes embodiments of the present invention with reference to the drawings. It should be noted that the description of the embodiments is provided to help understanding of the present invention, but the present invention is not limited thereto. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The sodium hyaluronate in the following examples is low molecular weight sodium hyaluronate with a molecular weight of 10-500 KDa.
Example 1
Weighing the following raw materials in percentage by weight: 2.5% of dimethyl silyl silica, 1% of butanediol, 0.2% of sodium hyaluronate, 0.5% of octyl glycol, 0.1% of hexanediol, 0.4% of phenoxyethanol and the balance of ethylhexyl palmitate.
The preparation method of the compound anti-wrinkle smoothing agent provided by the embodiment comprises the following steps:
(1) dispersing and stirring sodium hyaluronate and butanediol uniformly in advance for later use;
(2) heating ethylhexyl palmitate and silica dimethyl silylate to 85 ℃, and mixing and stirring uniformly;
(3) mixing the mixture obtained in the step (2) and the mixture obtained in the step (1), and homogenizing for 90 min;
(4) and cooling the homogenized mixture to 40 ℃, adding the caprylyl glycol, the hexanediol and the phenoxyethanol, stirring uniformly, and cooling.
The product obtained in this example was mixed with water, and the state of sodium hyaluronate spheres before and after water absorption was observed, and the results are shown in fig. 1 and 2.
It is apparent from figures 1 and 2 that the sodium hyaluronate spheres in the product obtained in this example swell by about 30 times after imbibing water.
The product obtained in this example was tested for transdermal absorption performance by the in vitro transdermal absorption test method, and the test results are shown in fig. 3 and 4.
From fig. 3 and 4, it is obvious that the sodium hyaluronate spheres permeate into the skin, absorb water to swell, swell the skin from inside to outside, and further achieve the effect of quickly removing wrinkles.
Example 2
Weighing the following raw materials in percentage by weight: 2.4% of dimethyl silyl silica, 1.2% of butanediol, 0.16% of sodium hyaluronate, 0.4% of octyl glycol, 0.08% of hexanediol, 0.3% of phenoxyethanol and the balance of ethylhexyl palmitate. The preparation of example 1 was followed to obtain the final product.
Example 3
Weighing the following raw materials in percentage by weight: 3.2% of dimethylsilylated silica, 0.8% of butanediol, 0.24% of sodium hyaluronate, 0.6% of octaethylene glycol, 0.12% of hexanediol, 0.5% of phenoxyethanol and the balance ethylhexyl palmitate. The preparation of example 1 was followed to obtain the final product.
Example 4
Weighing the following raw materials in percentage by weight: 2% of dimethyl silyl silica, 1% of butanediol, 0.2% of sodium hyaluronate, 0.5% of octyl glycol, 0.1% of hexanediol, 0.4% of phenoxyethanol and the balance of ethylhexyl palmitate. The preparation of example 1 was followed to obtain the final product. The preparation of example 1 was followed to obtain the final product.
Example 5
Weighing the following raw materials in percentage by weight: 1% of dimethyl silyl silica, 1% of butanediol, 0.2% of sodium hyaluronate, 0.5% of octyl glycol, 0.1% of hexanediol, 0.4% of phenoxyethanol and the balance of ethylhexyl palmitate. The preparation of example 1 was followed to obtain the final product.
Example 6
Weighing the following raw materials in percentage by weight: 4% of dimethyl silyl silica, 1% of butanediol, 0.2% of sodium hyaluronate, 0.5% of octyl glycol, 0.1% of hexanediol, 0.4% of phenoxyethanol and the balance of ethylhexyl palmitate. The preparation of example 1 was followed to obtain the final product. The preparation of example 1 was followed to obtain the final product.
Example 7
Weighing the following raw materials in percentage by weight: 5% of dimethyl silyl silica, 2% of butanediol, 0.5% of sodium hyaluronate, 0.8% of octyl glycol, 0.2% of hexanediol, 1% of phenoxyethanol and the balance of ethylhexyl palmitate.
The preparation method of the compound anti-wrinkle smoothing agent provided by the embodiment comprises the following steps:
(1) dispersing and stirring sodium hyaluronate and butanediol uniformly in advance for later use;
(2) heating ethylhexyl palmitate and silica dimethyl silylate to 90 ℃, and mixing and stirring uniformly;
(3) mixing the mixture obtained in the step (2) and the mixture obtained in the step (1), and homogenizing for 120 min;
(4) and cooling the homogenized mixture to 40 ℃, adding the caprylyl glycol, the hexanediol and the phenoxyethanol, stirring uniformly, and cooling.
Example 8
Weighing the following raw materials in percentage by weight: 1% of dimethyl silyl silica, 0.05% of butanediol, 0.05% of sodium hyaluronate, 0.3% of octyl glycol, 0.05% of hexanediol, 0.1% of phenoxyethanol and the balance of ethylhexyl palmitate.
The preparation method of the compound anti-wrinkle smoothing agent provided by the embodiment comprises the following steps:
(1) dispersing and stirring sodium hyaluronate and butanediol uniformly in advance for later use;
(2) heating ethylhexyl palmitate and silica dimethyl silylate to 80 ℃, and mixing and stirring uniformly;
(3) mixing the mixture obtained in the step (2) and the mixture obtained in the step (1), and homogenizing for 60 min;
(4) cooling the homogenized mixture to 45 ℃, adding the caprylyl glycol, the hexanediol and the phenoxyethanol, stirring uniformly, and cooling.
And (3) stability testing:
the product of the above example in sealed package was stored at 40 ℃ for 24h, at room temperature for 24h, at-5 ℃ for 24h, and the above procedure was repeated 3 times to see if there was delamination and color change. The test result shows that the products of the above embodiments have no layering phenomenon, and the color and luster are unchanged, and the product quality is stable.
Transdermal absorption test:
the skin penetration of the products obtained in the above examples 1 to 8 was tested by using rat skin as a test skin sample and using an in vitro skin penetration test method which is conventional in the art, and the skin penetration rate of sodium hyaluronate within 1 hour was tested, and the results are shown in table 1.
TABLE 1 results of the percutaneous absorbability test
Figure BDA0002444677490000051
Clinical testing
In order to further illustrate the beneficial effects of the invention, the anti-wrinkle smoothing effect of the product obtained in the embodiment is tested, 160 female volunteers aged 35-55 years are selected, the female volunteers are randomly divided into eight groups, the product obtained in the embodiment is applied after face cleaning every day, after trial for 1 month, the number of effective persons, the number of significant persons and the number of ineffective persons are counted, and the effective rate are calculated, wherein the statistical criteria are that ① is effective, the skin elasticity is obviously enhanced, the facial wrinkles are obviously lightened, the fine lines disappear, ② is effective, the skin elasticity is slightly improved, the fine lines are slightly reduced, the depth of the facial wrinkles is slightly lightened, ③ is ineffective, the skin elasticity and the facial wrinkles are not obviously changed, and the test results are shown in Table 1.
TABLE 1 results of clinical tests
Product source Number of effective people Number of effective persons Number of invalid persons Effective rate (%) Significant efficiency (%)
Example 1 12 8 0 100 60
Example 2 11 9 0 100 55
Example 3 9 11 0 100 45
Example 4 7 12 1 95 35
Example 5 3 12 5 75 15
Example 6 2 10 8 60 10
Example 7 3 12 5 75 15
Example 8 2 10 8 60 10
As can be seen from tables 1 and 2 and the observation results of a transmission electron microscope, the sodium hyaluronate of the products obtained in examples 1 to 4 has a significantly higher permeation rate than the products obtained in examples, and when the weight ratio of the dimethylsilylated silica to the sodium hyaluronate is 10-15: 1, the sodium hyaluronate spheres of the products of examples 1 to 3 can permeate the surface layer of the skin more rapidly, absorb water in the dermis and expand to 20-30 times of the original volume, so that the skin bulges from inside to outside, and the effect of rapidly removing wrinkles is achieved, and the sodium hyaluronate can be gradually absorbed by muscle base cells, so that the muscle base is more elastic. When the weight ratio of silica dimethyl silylate to sodium hyaluronate is 5:1, sodium hyaluronate spheres are small and can be rapidly absorbed by the skin surface layer, but the increase of the absorption swelling volume is small, the effect of removing wrinkles and smoothing wrinkles is not obvious, and the capability of preventing water evaporation is poor. When the weight ratio of silica dimethyl silylate to sodium hyaluronate is 20:1, the sodium hyaluronate spheres themselves are large in volume and are not easy to rapidly penetrate the surface layer of the skin.
The embodiments of the present invention have been described in detail with reference to the accompanying drawings, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, and the scope of protection is still within the scope of the invention.

Claims (10)

1. The compound anti-wrinkle-smoothing agent is characterized by comprising the following raw materials in percentage by weight: 1-5% of dimethyl silyl silica, 0.05-2% of humectant, 0.05-0.5% of sodium hyaluronate, 0.1-1% of antiseptic synergistic humectant, 0.1-1% of preservative and the balance of ethylhexyl palmitate.
2. The compound anti-wrinkle soothing agent according to claim 1, wherein the moisturizer is selected from one or more of butylene glycol, propylene glycol and glycerol.
3. The compound anti-wrinkle soothing agent according to claim 2, wherein the humectant is butylene glycol.
4. The compound anti-wrinkle soothing agent according to claim 1, wherein the preservative synergist humectant is selected from one or more of caprylyl glycol and hexylene glycol.
5. The compound anti-wrinkle smoothing agent according to claim 4, wherein the antiseptic synergist humectant comprises caprylyl glycol and hexylene glycol, the added amount of the caprylyl glycol in the compound anti-wrinkle smoothing agent is 0.3-0.8%, and the added amount of the hexylene glycol in the compound anti-wrinkle smoothing agent is 0.05-0.2%.
6. The compound anti-wrinkle smoothing agent according to claim 1, wherein the weight ratio of the silica dimethyl silylate to the sodium hyaluronate is 10-15: 1.
7. The compound anti-wrinkle smoothing agent according to claim 1, which comprises the following raw materials in percentage by weight: 2 to 3.2% of dimethylsilylated silica, 0.8 to 1.2% of butanediol, 0.16 to 0.24% of sodium hyaluronate, 0.4 to 0.6% of caprylyl glycol, 0.08 to 0.12% of hexylene glycol, 0.3 to 0.5% of phenoxyethanol, and the balance being ethylhexyl palmitate.
8. The compound anti-wrinkle smoothing agent according to claim 7, which comprises the following raw materials in percentage by weight: 2.5% of dimethyl silyl silica, 1% of humectant, 0.2% of sodium hyaluronate, 0.6% of antiseptic synergistic humectant, 0.4% of preservative and the balance of ethylhexyl palmitate.
9. The compound anti-wrinkle smoothing agent according to claim 1, wherein the preservative is phenoxyethanol.
10. A method for preparing the compound anti-wrinkle smoothing agent as claimed in any one of claims 1 to 9, comprising the following steps:
(1) dispersing and stirring sodium hyaluronate and humectant uniformly in advance for later use;
(2) heating ethylhexyl palmitate and silica dimethyl silylate to 80-90 ℃, and mixing and stirring uniformly;
(3) mixing the mixture obtained in the step (2) and the mixture obtained in the step (1), and homogenizing for 60-120 min;
(4) and (3) cooling the homogenized mixture to a temperature not higher than 45 ℃, adding the anticorrosion synergistic humectant and the preservative, uniformly stirring, and cooling.
CN202010275641.3A 2020-04-09 2020-04-09 Compound anti-wrinkle-smoothing agent and preparation method thereof Pending CN111449986A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1837008A2 (en) * 2006-03-21 2007-09-26 Coty Prestige Lancaster Group GmbH Cosmetic agent for lasting treatment of deeper wrinkles in the skin
CN104510631A (en) * 2013-09-27 2015-04-15 华熙福瑞达生物医药有限公司 Oil-dispersed sodium hyaluronate and preparation method and application of same
CN106074304A (en) * 2016-07-29 2016-11-09 广州市创美时美容化妆品有限公司 A kind of containing hyaluronate sodium microsphere and the anti-aging cosmetics compositions with smooth out wrinkles, even skin effect of peptide
CN107115240A (en) * 2017-05-27 2017-09-01 广州市千邦化妆品有限公司 A kind of anti-ageing face cream and preparation method thereof that compacts

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1837008A2 (en) * 2006-03-21 2007-09-26 Coty Prestige Lancaster Group GmbH Cosmetic agent for lasting treatment of deeper wrinkles in the skin
CN104510631A (en) * 2013-09-27 2015-04-15 华熙福瑞达生物医药有限公司 Oil-dispersed sodium hyaluronate and preparation method and application of same
CN106074304A (en) * 2016-07-29 2016-11-09 广州市创美时美容化妆品有限公司 A kind of containing hyaluronate sodium microsphere and the anti-aging cosmetics compositions with smooth out wrinkles, even skin effect of peptide
CN107115240A (en) * 2017-05-27 2017-09-01 广州市千邦化妆品有限公司 A kind of anti-ageing face cream and preparation method thereof that compacts

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
蒙亮亮等: "透明质酸在化妆品中的应用研究进展", 《山东化工》 *

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Application publication date: 20200728