阅读说明：本技术 一种含阳离子透明质酸的保湿抗衰老化妆品组合物的制备方法 (Preparation method of moisturizing and anti-aging cosmetic composition containing cationic hyaluronic acid ) 是由 张俊停 廉少杰 康传利 刘磊 李庆 张梦益 于 2021-09-28 设计创作，主要内容包括：本发明公开了一种含阳离子透明质酸的保湿抗衰老化妆品组合物,包括：透明质酸组合物,纯化水,乳化剂,增稠剂,防腐剂,香精,表面活性剂；所述透明质酸组合物,包括：超低分子透明质酸和阳离子透明质酸的混合液,聚二甲基硅氧烷,乙酰基六肽-8,聚谷氨酸钠,烟酰胺；所述超低分子透明质酸和阳离子透明质酸的混合液中超低分子透明质酸和阳离子透明质酸的质量比1:0.5-2；本发明通过使用超低分子透明质酸和阳离子透明质酸的组合物,既具有了抗氧化和抗衰老功效,又富含羟基、羧基等极性基团,可以通过分子间作用力实现对水分子的高亲和作用,实现强有力的保水效果。(The invention discloses a moisturizing and anti-aging cosmetic composition containing cationic hyaluronic acid, which comprises the following components in part by weight: hyaluronic acid composition, purified water, emulsifier, thickener, preservative, essence and surfactant; the hyaluronic acid composition comprises: mixed solution of ultra-low molecular weight hyaluronic acid and cationic hyaluronic acid, polydimethylsiloxane, acetyl hexapeptide-8, sodium polyglutamate and nicotinamide; the mass ratio of the ultralow molecular hyaluronic acid to the cationic hyaluronic acid in the mixed solution of the ultralow molecular hyaluronic acid and the cationic hyaluronic acid is 1: 0.5-2; the composition of the ultra-low molecular hyaluronic acid and the cationic hyaluronic acid has the effects of resisting oxidation and ageing, is rich in polar groups such as hydroxyl groups and carboxyl groups, can realize high affinity action on water molecules through intermolecular force, and realizes a powerful water retention effect.)

1. A moisturizing and anti-aging cosmetic composition containing cationic hyaluronic acid is characterized by comprising the following components in parts by weight: 30-51 parts of hyaluronic acid composition, 40-80 parts of purified water, 1.8-2.2 parts of emulsifier, 1.8-2.2 parts of thickener, 0.09-0.11 part of preservative, 0.01-0.02 part of essence and 8-12 parts of surfactant;

the hyaluronic acid composition comprises: 20-30 parts of mixed solution of ultra-low molecular hyaluronic acid and cationic hyaluronic acid, 3-5 parts of polydimethylsiloxane, 81-3 parts of acetyl hexapeptide, 5-10 parts of sodium polyglutamate and 1-3 parts of nicotinamide;

the mass ratio of the ultra-low molecular hyaluronic acid to the cationic hyaluronic acid in the mixed solution of the ultra-low molecular hyaluronic acid and the cationic hyaluronic acid is 1: 0.5-2.

2. The moisturizing and anti-aging cosmetic composition containing cationic hyaluronic acid according to claim 1, wherein the emulsifier is sorbitan trioleate, the thickener is lauryl alcohol, the preservative is methyl paraben, the perfume is isomethylionone, and the surfactant is disodium sulfosuccinate.

3. The moisturizing and anti-aging cosmetic composition as claimed in claim 1, wherein the molecular weight of the ultra-low molecular hyaluronic acid is 5000-10000 Da;

the molecular weight of the cationic hyaluronic acid is 20-40WDa, and the cationic degree is 0.5-0.7.

4. The moisturizing and anti-aging cosmetic composition containing cationic hyaluronic acid according to claim 3, wherein the preparation method of the hyaluronic acid composition comprises preparing an ultra-low molecular hyaluronic acid solution, preparing a cationic hyaluronic acid solution, and mixing.

5. The moisturizing and anti-aging cosmetic composition containing cationic hyaluronic acid according to claim 4, wherein the preparation of the ultra-low molecular hyaluronic acid solution comprises slowly and uniformly adding the ultra-low molecular hyaluronic acid into purified water with the mass 100 times that of the ultra-low molecular hyaluronic acid, controlling the adding time to be 1min, and then completely dissolving the ultra-low molecular hyaluronic acid solution under the stirring action of 200 r/min; and then adding sodium polyglutamate under the stirring action of 200r/min, adding nicotinamide for dissolving after the sodium polyglutamate is completely dissolved, and obtaining the ultra-low molecular hyaluronic acid solution after the sodium polyglutamate is completely dissolved.

6. The moisturizing and anti-aging cosmetic composition containing cationic hyaluronic acid according to claim 4, wherein the cationic hyaluronic acid solution is prepared by slowly and uniformly adding cationic hyaluronic acid into purified water with the mass 100 times that of the cationic hyaluronic acid, controlling the adding time to be 1min, heating to 40 ℃ under the stirring action of 200r/min, and completely dissolving the cationic hyaluronic acid; and then adding polydimethylsiloxane under the stirring action of 200r/min, adding acetyl hexapeptide-8 for dissolving after the polydimethylsiloxane is completely dissolved, and obtaining the cationic hyaluronic acid solution after complete dissolution.

7. The moisturizing and anti-aging cosmetic composition containing cationic hyaluronic acid according to claim 4, wherein the mixing is carried out by slowly adding the cationic hyaluronic acid solution into the ultra-low molecular hyaluronic acid solution under the stirring action of 200r/min, and stirring until the solution is clear and transparent, thereby obtaining the hyaluronic acid composition.

8. The moisturizing and anti-aging cosmetic composition containing cationic hyaluronic acid according to claim 3, wherein the preparation method of the cationic hyaluronic acid comprises cationization, first dissolution, second dissolution, third dissolution, dehydration of the material, and drying of the material.

9. The moisturizing anti-aging cosmetic composition comprising cationic hyaluronic acid according to claim 8, characterized in that the cationization reaction is carried out by adding alcohol solution into a dissolving tank, starting stirring, controlling the stirring speed at 310rpm of 300-, then heating to 58-60 ℃, adding 2, 3-epoxypropyltrimethylammonium chloride for dissolving, adding hyaluronic acid with molecular weight of 20-40WDa after 2, 3-epoxypropyltrimethylammonium chloride is completely dissolved, then adding saline-alkali water for reaction, sealing the opening of the dissolving tank in the reaction process to prevent alcohol from volatilizing, when materials in the tank are condensed and layered to reach the state that the upper layer is brown transparent solution and the lower layer is gel mass, stopping stirring, standing for 5-10min, and pumping out the upper brown transparent solution to obtain the primary cationized product.

10. The moisturizing and anti-aging cosmetic composition containing cationic hyaluronic acid as claimed in claim 9, wherein the alcohol solution, 2, 3-epoxypropyltrimethylammonium chloride, hyaluronic acid with molecular weight of 20-40WDa, the volume mass ratio of the saline water is 190-210L: 38-42 kg: 18-22 kg: 23-27 kg.

Technical Field

The invention belongs to the field of cosmetics, and particularly relates to a preparation method of a moisturizing and anti-aging cosmetic composition containing cationic hyaluronic acid.

Background

With age, the morphological structure and physiological function of the skin change. Skin aging is the result of multiple factors, and skin damage, infection, malnutrition, metabolic disorders, and drug abuse can affect skin condition. Healthy skin is smooth, moist and elastic, free radicals destroy collagen and active substances in normal cell membrane tissues to form fine lines and wrinkles, and the skin is evaporated, lacks water and loses elasticity to form the wrinkles.

The root cause of skin aging is that the water in the body is lost too fast, cells cannot obtain sufficient water, the metabolism of the cells is influenced, the division and the propagation of the cells are influenced, and a large number of aged tissue cells cannot be normally updated, so that the skin is rough and has wrinkles. Meanwhile, excessive oxygen radicals in the body are an important reason for accelerating skin aging, and the generation of the oxygen radicals can be originated from the metabolism of the human body and can also be caused by a plurality of factors such as ultraviolet irradiation, environmental pollution, bad living habits and the like. The free radicals are originally intermediates of human metabolism and are effective defense systems of organisms; but when the free radicals are excessive and cannot be cleared in time, the aging process of the body is accelerated.

Many cosmetics cover the skin with some whitening components, and cannot fundamentally solve the problem of skin aging acceleration. The moisturizing and anti-aging cosmetic composition invented today can effectively inhibit rapid aging of the skin.

Disclosure of Invention

In order to fundamentally solve the problem of rapid skin aging, the invention provides a preparation method of a moisturizing and anti-aging cosmetic composition containing cationic hyaluronic acid, ultralow molecular hyaluronic acid in the composition can be instantly absorbed by the skin, the hyaluronic acid is rich in polar groups such as hydroxyl, carboxyl and the like, the high affinity effect on water molecules can be realized through intermolecular force, the hyaluronic acid can be rapidly combined with water molecules in the skin, the powerful water retention effect is realized, and the loss of water in the skin is prevented. When the ultra-low molecular hyaluronic acid is absorbed by the skin instantly, the cationic hyaluronic acid can enter the skin through the channel, and the anti-oxidation property of the cationic hyaluronic acid is matched, so that the rapid aging of the skin is effectively inhibited.

In order to solve the technical problems, the technical scheme adopted by the invention is as follows:

a moisturizing and anti-aging cosmetic composition containing cationic hyaluronic acid comprises the following components in parts by weight: 30-51 parts of hyaluronic acid composition, 40-80 parts of purified water, 1.8-2.2 parts of emulsifier, 1.8-2.2 parts of thickener, 0.09-0.11 part of preservative, 0.01-0.02 part of essence and 8-12 parts of surfactant.

Preferably, the emulsifier is sorbitan trioleate, the thickener is lauryl alcohol, the preservative is methyl p-hydroxybenzoate, the essence is isomethylionone, and the surfactant is disodium sulfosuccinate.

The hyaluronic acid composition comprises: 20-30 parts of mixed solution of ultra-low molecular hyaluronic acid and cationic hyaluronic acid, 3-5 parts of polydimethylsiloxane, 81-3 parts of acetyl hexapeptide, 5-10 parts of sodium polyglutamate and 1-3 parts of nicotinamide;

the mass ratio of the ultralow molecular hyaluronic acid to the cationic hyaluronic acid in the mixed solution of the ultralow molecular hyaluronic acid and the cationic hyaluronic acid is 1: 0.5-2;

the molecular weight of the ultra-low molecular hyaluronic acid is 5000-;

the molecular weight of the cationic hyaluronic acid is 20-40WDa, and the cationic degree is 0.5-0.7.

The preparation method of the hyaluronic acid composition comprises the steps of preparing an ultra-low molecular hyaluronic acid solution, preparing a cationic hyaluronic acid solution and mixing.

The preparation of the ultra-low molecular hyaluronic acid solution comprises the steps of slowly and uniformly adding the ultra-low molecular hyaluronic acid into purified water with the mass 100 times that of the ultra-low molecular hyaluronic acid, controlling the adding time to be 1min, and then completely dissolving the ultra-low molecular hyaluronic acid under the stirring action of 200 r/min; and then adding sodium polyglutamate under the stirring action of 200r/min, adding nicotinamide for dissolving after the sodium polyglutamate is completely dissolved, and obtaining the ultra-low molecular hyaluronic acid solution after the sodium polyglutamate is completely dissolved.

The preparation method comprises the steps of slowly and uniformly adding cationic hyaluronic acid into purified water with the mass 100 times that of the cationic hyaluronic acid, controlling the adding time to be 1min, heating to 40 ℃ under the stirring action of 200r/min, and completely dissolving the cationic hyaluronic acid; and then adding polydimethylsiloxane under the stirring action of 200r/min, adding acetyl hexapeptide-8 for dissolving after the polydimethylsiloxane is completely dissolved, and obtaining the cationic hyaluronic acid solution after complete dissolution.

And mixing, namely slowly adding the cationic hyaluronic acid solution into the ultra-low molecular hyaluronic acid solution under the stirring action of 200r/min, and stirring until the solution is clear and transparent to obtain the hyaluronic acid composition.

The preparation method of the cationic hyaluronic acid comprises cationization reaction, first dissolution, second dissolution, third dissolution, material dehydration and material drying.

Adding an alcohol solution into a dissolving tank, starting stirring, controlling the stirring speed to be 300-310rpm, heating to 58-60 ℃, adding 2, 3-epoxypropyltrimethylammonium chloride for dissolving, adding hyaluronic acid with the molecular weight of 20-40WDa after the 2, 3-epoxypropyltrimethylammonium chloride is completely dissolved, adding saline-alkali water for reacting, sealing the tank opening of the dissolving tank in the reaction process to prevent the alcohol from volatilizing, stopping stirring when materials in the tank are condensed and layered to reach the state that the upper layer is a brown transparent solution and the lower layer is a gel cluster, standing for 5-10min, and pumping out the brown transparent solution on the upper layer to obtain a primary cationized product;

the alcohol solution is 80-degree alcohol containing 1.9% -2.1% of NaCl;

the saline-alkali water is prepared by taking purified water as a solvent and contains 0.9% -1.1% of NaCl and 6.2% -6.3% of NaOH;

wherein, the alcohol solution, 2, 3-epoxypropyl trimethyl ammonium chloride, hyaluronic acid with the molecular weight of 20-40WDa, and the volume mass ratio of the saline-alkali water is 190-210L: 38-42 kg: 18-22 kg: 23-27 kg.

And the first dissolution, adding purified water into the primary cationization product, starting stirring, controlling the stirring speed to be 310rpm, then heating to 48-50 ℃, adding NaCl accounting for 9-11% of the total material by mass percent after the materials are completely dissolved, adjusting the pH of the materials to 6-7 by using liquid alkali, stirring for 19-21min, then adding 95-degree alcohol for material precipitation, controlling the alcohol degree to be 60-65 ℃, stopping stirring, standing for 5-10min, and after the materials are layered, pumping out the upper brown transparent solution to obtain the first dissolution product.

The volume ratio of the purified water in the first dissolution to the alcohol solution in the cationization reaction is 1.8-2.2: 1.

And (3) adding purified water into the first dissolved product, starting stirring, heating to 48-50 ℃, adding NaCl accounting for 7-9% of the total material by mass after the materials are completely dissolved, adjusting the pH of the materials to 6-7 with alkali liquor, stirring for 19-21min, adding 95-degree alcohol to perform material precipitation, controlling the alcohol content to be 60-65 ℃, stopping stirring, standing for 5-10min, and taking out the upper brown transparent solution after the materials are layered to obtain a second dissolved product.

The volume ratio of the purified water in the second dissolution to the alcohol solution in the cationization reaction is 1.8-2.2: 1.

And (3) dissolving for the third time, adding purified water into the second dissolved product, starting stirring, heating to 48-50 ℃, adding NaCl accounting for 19-21% of the total material by mass after the materials are completely dissolved, adjusting the pH of the materials to 6-7 by using an alkali liquor, stirring for 19-21min, adding 95-degree alcohol to perform material precipitation, controlling the alcoholic strength to be 60-65 ℃, stopping stirring, standing for 5-10min, and removing the upper brown transparent solution after the materials are layered to obtain a third dissolved product.

The volume ratio of the purified water in the third dissolution to the alcohol solution in the cationization reaction is 4.8-5.2: 1.

And (3) dehydrating the material, namely dehydrating the material of the third dissolved product for 29-31min by using a centrifuge with the power of 4900-5100rps to obtain the dehydrated material.

And (3) drying the material, namely putting the dehydrated material into an oven at 63-67 ℃ for material drying until the moisture measured by a halogen moisture tester is reduced to below 7 percent, so as to obtain the cationic hyaluronic acid.

Compared with the prior art, the invention has the beneficial effects that:

(1) the moisturizing and anti-aging cosmetic composition has the effects of oxidation resistance and aging resistance by using the composition of the ultra-low molecular hyaluronic acid and the cationic hyaluronic acid, is rich in polar groups such as hydroxyl groups and carboxyl groups, can realize high affinity action on water molecules by intermolecular force, and realizes powerful water retention effect;

(2) the moisturizing and anti-aging cosmetic composition has optimal film-forming property by adjusting the ratio of the ultra-low molecular hyaluronic acid to the cationic hyaluronic acid, can form a uniform film layer on the inner surface of the skin, effectively reduces the outward dissipation of water in the horny layer of the skin, and can realize good instant and long-acting moisturizing effect and moisturizing effect in a dry environment;

(3) the moisturizing and anti-aging cosmetic composition disclosed by the invention uses the sodium polyglutamate and the nicotinamide as whitening active ingredients, wherein the sodium polyglutamate can promote the repair of skin, and the nicotinamide can inhibit the migration of melanin to stratum corneum to realize a whitening effect;

(4) the moisturizing and anti-aging cosmetic composition disclosed by the invention uses polydimethylsiloxane and acetyl hexapeptide-8 as an emollient and a nutrient to improve the skin feeling of the cosmetic composition;

(5) the moisture-preserving anti-aging cosmetic composition has the advantages that the moisture content of the skin can reach 62.58-63.51% after 8 hours of use, the moisture content of the skin can reach 62.68-64.05% after 2 weeks of use, and the moisture content of the skin can reach 61.87-63.55% after 4 weeks of use;

(6) the moisture-preserving and anti-aging cosmetic composition disclosed by the invention has the advantages that the skin elasticity value can reach 0.68-0.74 after 8 hours of use, the skin moisture content can reach 0.78-0.88 after 2 weeks of use, and the skin moisture content can reach 0.80-0.87 after 4 weeks of use.

Detailed Description

The present invention will be further described with reference to specific examples, which are not intended to limit the invention in any way, except as otherwise indicated, reagents, methods and equipment used in the invention are conventional in the art.

Unless otherwise indicated, reagents and materials used in the following examples are commercially available.

Example 1

A moisturizing and anti-aging cosmetic composition containing cationic hyaluronic acid comprises the following components in parts by weight:

24 parts of hyaluronic acid composition, 58 parts of purified water, 2 parts of sorbitan trioleate, 2 parts of lauryl alcohol, 0.1 part of methyl p-hydroxybenzoate, 0.02 part of iso-methyl ionone and 10 parts of disodium sulfosuccinate monoester.

The hyaluronic acid composition comprises: 16 parts of ultra-low molecular hyaluronic acid, 8 parts of cationic hyaluronic acid, 4 parts of polydimethylsiloxane, 8 parts of acetyl hexapeptide-82, 8 parts of sodium polyglutamate and 4 parts of nicotinamide

Wherein the molecular weight of the ultra-low molecular hyaluronic acid is 5000 Da;

the cationic hyaluronic acid has a molecular weight of 20WDa and a cationicity of 0.6.

The preparation method of the hyaluronic acid composition comprises the following specific steps:

(1) weighing the raw materials according to the parts by weight of each component in the composition, slowly and uniformly adding the ultra-low molecular hyaluronic acid into purified water with the mass 100 times that of the ultra-low molecular hyaluronic acid, controlling the adding time to be 1min, and then completely dissolving the ultra-low molecular hyaluronic acid under the stirring action of 200 r/min;

(2) slowly and uniformly adding cationic hyaluronic acid into purified water 100 times the mass of the cationic hyaluronic acid, controlling the adding time to be 1min, heating to 40 ℃ under the stirring action of 200r/min, and completely dissolving the cationic hyaluronic acid;

(3) adding sodium polyglutamate into the ultra-low molecular weight hyaluronic acid aqueous solution obtained in the step (1) under the stirring action of 200r/min, and adding nicotinamide for dissolving after the sodium polyglutamate is completely dissolved;

(4) adding polydimethylsiloxane into the cationic hyaluronic acid aqueous solution obtained in the step (2) under the stirring action of 200r/min, and adding acetyl hexapeptide-8 for dissolving after the polydimethylsiloxane is completely dissolved;

(5) and (3) slowly adding the mixed solution obtained in the step (4) into the mixed solution obtained in the step (3) under the stirring action of 200r/min, uniformly stirring, and stirring until the mixed solution is clear and transparent to form a uniformly dispersed spherical state in which the cationic hyaluronic acid is surrounded by the ultra-low molecular hyaluronic acid, so as to obtain the hyaluronic acid composition.

Example 2

A moisturizing and anti-aging cosmetic composition containing cationic hyaluronic acid comprises the following components in parts by weight:

24 parts of hyaluronic acid composition, 58 parts of purified water, 2 parts of sorbitan trioleate, 2 parts of lauryl alcohol, 0.1 part of methyl p-hydroxybenzoate, 0.02 part of iso-methyl ionone and 10 parts of disodium sulfosuccinate monoester.

The hyaluronic acid composition comprises: 12 parts of ultra-low molecular hyaluronic acid, 12 parts of cationic hyaluronic acid, 4 parts of polydimethylsiloxane, acetyl hexapeptide-82 parts, 8 parts of sodium polyglutamate and 4 parts of nicotinamide

Wherein the molecular weight of the ultra-low molecular hyaluronic acid is 5000 Da;

the cationic hyaluronic acid has a molecular weight of 20WDa and a cationicity of 0.6.

The preparation method of the hyaluronic acid composition comprises the following specific steps:

(1) weighing the raw materials according to the parts by weight of each component in the composition, slowly and uniformly adding the ultra-low molecular hyaluronic acid into purified water with the mass 100 times that of the ultra-low molecular hyaluronic acid, controlling the adding time to be 1min, and then completely dissolving the ultra-low molecular hyaluronic acid under the stirring action of 200 r/min;

(2) slowly and uniformly adding cationic hyaluronic acid into purified water 100 times the mass of the cationic hyaluronic acid, controlling the adding time to be 1min, heating to 41 ℃ under the stirring action of 200r/min, and completely dissolving the cationic hyaluronic acid;

(3) adding sodium polyglutamate into the ultra-low molecular weight hyaluronic acid aqueous solution obtained in the step (1) under the stirring action of 200r/min, and adding nicotinamide for dissolving after the sodium polyglutamate is completely dissolved;

(4) adding polydimethylsiloxane into the cationic hyaluronic acid aqueous solution obtained in the step (2) under the stirring action of 200r/min, and adding acetyl hexapeptide-8 for dissolving after the polydimethylsiloxane is completely dissolved;

(5) and (3) slowly adding the mixed solution obtained in the step (4) into the mixed solution obtained in the step (3) under the stirring action of 200r/min, uniformly stirring, and stirring until the mixed solution is clear and transparent to form a uniformly dispersed spherical state in which the cationic hyaluronic acid is surrounded by the ultra-low molecular hyaluronic acid, so as to obtain the hyaluronic acid composition.

Example 3

A moisturizing and anti-aging cosmetic composition containing cationic hyaluronic acid comprises the following components in parts by weight:

24 parts of hyaluronic acid composition, 58 parts of purified water, 2 parts of sorbitan trioleate, 2 parts of lauryl alcohol, 0.1 part of methyl p-hydroxybenzoate, 0.02 part of iso-methyl ionone and 10 parts of disodium sulfosuccinate monoester.

The hyaluronic acid composition comprises: 8 parts of ultra-low molecular hyaluronic acid, 16 parts of cationic hyaluronic acid, 4 parts of polydimethylsiloxane, 8 parts of acetyl hexapeptide-82, 8 parts of sodium polyglutamate and 4 parts of nicotinamide

Wherein the molecular weight of the ultra-low molecular weight hyaluronic acid is 1 WDa;

the cationic hyaluronic acid has a molecular weight of 40WDa and a cationicity of 0.6.

The preparation method of the hyaluronic acid composition comprises the following specific steps:

(1) weighing the raw materials according to the parts by weight of each component in the composition, slowly and uniformly adding the ultra-low molecular hyaluronic acid into purified water with the mass 100 times that of the ultra-low molecular hyaluronic acid, controlling the adding time to be 1min, and then completely dissolving the ultra-low molecular hyaluronic acid under the stirring action of 200 r/min;

(2) slowly and uniformly adding cationic hyaluronic acid into purified water 100 times the mass of the cationic hyaluronic acid, controlling the adding time to be 1min, heating to 42 ℃ under the stirring action of 200r/min, and completely dissolving the cationic hyaluronic acid;

(3) adding sodium polyglutamate into the ultra-low molecular weight hyaluronic acid aqueous solution obtained in the step (1) under the stirring action of 200r/min, and adding nicotinamide for dissolving after the sodium polyglutamate is completely dissolved;

(4) adding polydimethylsiloxane into the cationic hyaluronic acid aqueous solution obtained in the step (2) under the stirring action of 200r/min, and adding acetyl hexapeptide-8 for dissolving after the polydimethylsiloxane is completely dissolved;

(5) and (3) slowly adding the mixed solution obtained in the step (4) into the mixed solution obtained in the step (3) under the stirring action of 200r/min, uniformly stirring, and stirring until the mixed solution is clear and transparent to form a uniformly dispersed spherical state in which the cationic hyaluronic acid is surrounded by the ultra-low molecular hyaluronic acid, so as to obtain the hyaluronic acid composition.

Example 4

A moisturizing and anti-aging cosmetic composition containing cationic hyaluronic acid comprises the following components in parts by weight:

20 parts of hyaluronic acid composition, 58 parts of purified water, 2 parts of sorbitan trioleate, 2 parts of lauryl alcohol, 0.1 part of methyl p-hydroxybenzoate, 0.02 part of iso-methyl ionone and 10 parts of disodium sulfosuccinate monoester.

The hyaluronic acid composition comprises: 10 parts of ultra-low molecular hyaluronic acid, 10 parts of cationic hyaluronic acid, 8 parts of polydimethylsiloxane, 8 parts of acetyl hexapeptide-82, 8 parts of sodium polyglutamate and 4 parts of nicotinamide

Wherein the molecular weight of the ultra-low molecular hyaluronic acid is 5000 Da;

the cationic hyaluronic acid has a molecular weight of 40WDa and a cationicity of 0.6.

The preparation method of the hyaluronic acid composition comprises the following specific steps:

(1) weighing the raw materials according to the parts by weight of each component in the composition, slowly and uniformly adding the ultra-low molecular hyaluronic acid into purified water with the mass 100 times that of the ultra-low molecular hyaluronic acid, controlling the adding time to be 1min, and then completely dissolving the ultra-low molecular hyaluronic acid under the stirring action of 200 r/min;

(2) slowly and uniformly adding cationic hyaluronic acid into purified water 100 times the mass of the cationic hyaluronic acid, controlling the adding time to be 1min, heating to 44 ℃ under the stirring action of 200r/min, and completely dissolving the cationic hyaluronic acid;

(3) adding sodium polyglutamate into the ultra-low molecular weight hyaluronic acid aqueous solution obtained in the step (1) under the stirring action of 200r/min, and adding nicotinamide for dissolving after the sodium polyglutamate is completely dissolved;

(4) adding polydimethylsiloxane into the cationic hyaluronic acid aqueous solution obtained in the step (2) under the stirring action of 200r/min, and adding acetyl hexapeptide-8 for dissolving after the polydimethylsiloxane is completely dissolved;

(5) and (3) slowly adding the mixed solution obtained in the step (4) into the mixed solution obtained in the step (3) under the stirring action of 200r/min, uniformly stirring, and stirring until the mixed solution is clear and transparent to form a uniformly dispersed spherical state in which the cationic hyaluronic acid is surrounded by the ultra-low molecular hyaluronic acid, so as to obtain the hyaluronic acid composition.

Example 5

A moisturizing and anti-aging cosmetic composition containing cationic hyaluronic acid comprises the following components in parts by weight:

30 parts of hyaluronic acid composition, 58 parts of purified water, 2 parts of sorbitan trioleate, 2 parts of lauryl alcohol, 0.1 part of methyl p-hydroxybenzoate, 0.02 part of iso-methyl ionone and 10 parts of disodium sulfosuccinate monoester.

The hyaluronic acid composition comprises: 15 parts of ultra-low molecular hyaluronic acid, 15 parts of cationic hyaluronic acid, 2 parts of polydimethylsiloxane, 4 parts of sodium polyglutamate and 4 parts of nicotinamide

Wherein the molecular weight of the ultra-low molecular hyaluronic acid is 7000 Da;

the cationic hyaluronic acid has a molecular weight of 30WDa and a cationicity of 0.6.

The preparation method of the hyaluronic acid composition comprises the following specific steps:

(1) weighing the raw materials according to the parts by weight of each component in the composition, slowly and uniformly adding the ultra-low molecular hyaluronic acid into purified water with the mass 100 times that of the ultra-low molecular hyaluronic acid, controlling the adding time to be 1min, and then completely dissolving the ultra-low molecular hyaluronic acid under the stirring action of 200 r/min;

(2) slowly and uniformly adding cationic hyaluronic acid into purified water 100 times the mass of the cationic hyaluronic acid, controlling the adding time to be 1min, heating to 45 ℃ under the stirring action of 200r/min, and completely dissolving the cationic hyaluronic acid;

(3) adding sodium polyglutamate into the ultra-low molecular weight hyaluronic acid aqueous solution obtained in the step (1) under the stirring action of 200r/min, and adding nicotinamide for dissolving after the sodium polyglutamate is completely dissolved;

(4) adding polydimethylsiloxane into the cationic hyaluronic acid aqueous solution obtained in the step (2) under the stirring action of 200r/min, and adding acetyl hexapeptide-8 for dissolving after the polydimethylsiloxane is completely dissolved;

(5) and (3) slowly adding the mixed solution obtained in the step (4) into the mixed solution obtained in the step (3) under the stirring action of 200r/min, uniformly stirring, and stirring until the mixed solution is clear and transparent to form a uniformly dispersed spherical state in which the cationic hyaluronic acid is surrounded by the ultra-low molecular hyaluronic acid, so as to obtain the hyaluronic acid composition.

Example 6

The method for preparing the cationic hyaluronic acid used in example 1 specifically includes:

(1) cationization reaction: adding 200L of 80-degree alcohol containing 2% NaCl into a dissolving tank with the volume of 2T, starting stirring, controlling the stirring speed to be 300rpm, heating to 58 ℃, adding 40kg of 2, 3-epoxypropyltrimethylammonium chloride for dissolving, adding 20kg of hyaluronic acid with the molecular weight of 20WDa after the 2, 3-epoxypropyltrimethylammonium chloride is completely dissolved, adding 25kg of saline-alkali water containing 1% NaCl and 6.25% NaOH, which is prepared by taking purified water as a solvent, for reacting, sealing the tank opening of the dissolving tank by using a preservative film in the reaction process, preventing the alcohol from volatilizing, standing for 5min after materials in the tank are condensed and layered to reach the state that the upper layer is brown transparent solution and the lower layer is gel mass, and pumping off the brown transparent solution on the upper layer.

(2) First dissolution: adding 400L of purified water into a dissolving tank, starting stirring, controlling the stirring speed at 300rpm, heating to 48 ℃, adding NaCl accounting for 10% of the total material by mass after the materials are completely dissolved, adjusting the pH of the materials to 6 by using liquid alkali, stirring for 20min, adding 95-degree alcohol for material precipitation, controlling the alcoholic strength at 60 ℃, stopping stirring, standing for 5min, and after the materials are layered, pumping out the upper brown transparent solution.

(3) And (3) second dissolution: adding 400L of purified water into a dissolving tank, starting stirring, heating to 48 ℃, adding NaCl accounting for 8% of the total material by mass after the materials are completely dissolved, adjusting the pH of the materials to 6 by using an alkali solution, stirring for 20min, then adding 95-degree alcohol to perform material precipitation, controlling the alcoholic strength to be 60 ℃, stopping stirring, standing for 5min, and after the materials are layered, pumping out the brown transparent solution on the upper layer.

(4) And (3) dissolving for the third time: adding 1000L of purified water into a dissolving tank, starting stirring, heating to 48 ℃, adding NaCl accounting for 20% of the total material by mass after the materials are completely dissolved, adjusting the pH of the materials to 6 by using an alkali solution, stirring for 20min, then adding 95-degree alcohol to precipitate the materials, controlling the alcoholic strength to be 60 ℃, stopping stirring, standing for 5min, and after the materials are layered, pumping out the brown transparent solution on the upper layer.

(5) Dehydrating materials: and dehydrating the precipitated material for 30min by using a 5000rps centrifuge.

(6) Drying materials: and (3) putting the dehydrated material into a 65-DEG C oven for material drying until the moisture measured by a halogen moisture tester is reduced to 7 percent, thus obtaining the cationic hyaluronic acid.

Example 7

The method for preparing the cationic hyaluronic acid used in example 5 specifically includes:

(1) cationization reaction: adding 200L of 80-degree alcohol containing 2% NaCl into a dissolving tank with the volume of 2T, starting stirring, controlling the stirring speed to be 310rpm, then heating to 60 ℃, adding 40kg of 2, 3-epoxypropyltrimethylammonium chloride for dissolving, adding 20kg of hyaluronic acid with the molecular weight of 30WDa after the 2, 3-epoxypropyltrimethylammonium chloride is completely dissolved, then adding 25kg of saline-alkali water containing 1% NaCl and 6.25% NaOH and prepared by taking purified water as a solvent for reacting, sealing the tank opening of the dissolving tank by using a preservative film in the reaction process to prevent alcohol from volatilizing, standing for 10min after materials in the tank are condensed and layered to reach the state that the upper layer is brown transparent solution and the lower layer is gel mass, and pumping off the brown transparent solution on the upper layer.

(2) First dissolution: adding 400L of purified water into a dissolving tank, starting stirring, controlling the stirring speed to be 310rpm, then heating to 50 ℃, adding NaCl accounting for 10% of the total material by mass after the materials are completely dissolved, adjusting the pH of the materials to be 7 by using liquid alkali, stirring for 20min, then adding 95-degree alcohol to perform material precipitation, controlling the alcoholic strength to be 65 ℃, stopping stirring, standing for 10min, and after the materials are layered, pumping out the brown transparent solution on the upper layer.

(3) And (3) second dissolution: adding 400L of purified water into a dissolving tank, starting stirring, heating to 50 ℃, adding NaCl accounting for 8% of the total material by mass after the materials are completely dissolved, adjusting the pH of the materials to 7 with an alkali solution, stirring for 20min, then adding 95-degree alcohol to precipitate the materials, controlling the alcoholic strength to be 65 ℃, stopping stirring, standing for 10min, and after the materials are layered, pumping out the brown transparent solution on the upper layer.

(4) And (3) dissolving for the third time: adding 1000L of purified water into a dissolving tank, starting stirring, heating to 50 ℃, adding NaCl accounting for 20% of the total material by mass after the materials are completely dissolved, adjusting the pH of the materials to 7 by using an alkali liquor, stirring for 20min, then adding 95-degree alcohol to precipitate the materials, controlling the alcoholic strength to be 65 ℃, stopping stirring, standing for 10min, and after the materials are layered, pumping out the brown transparent solution on the upper layer.

(5) Dehydrating materials: and dehydrating the precipitated material for 30min by using a 5000rps centrifuge.

(6) Drying materials: and (3) putting the dehydrated material into a 65-DEG C oven for material drying until the moisture measured by a halogen moisture tester is reduced to 6 percent, thus obtaining the cationic hyaluronic acid.

Comparative example 1

The composition of a moisturizing and anti-aging cosmetic composition containing cationic hyaluronic acid, the composition of the hyaluronic acid composition, the preparation method of the hyaluronic acid composition and the like are the same as those in example 1, except that: the composition of the hyaluronic acid composition does not contain cationic hyaluronic acid, and the hyaluronic acid composition is prepared without adding cationic hyaluronic acid.

Comparative example 2

The composition of a moisturizing and anti-aging cosmetic composition containing cationic hyaluronic acid, the composition of the hyaluronic acid composition, the preparation method of the hyaluronic acid composition and the like are the same as those in example 1, except that: the composition of the hyaluronic acid composition does not contain the ultra-low molecular weight hyaluronic acid, and the ultra-low molecular weight hyaluronic acid is not added in the preparation of the hyaluronic acid composition.

Comparative example 3

The composition of a moisturizing and anti-aging cosmetic composition containing cationic hyaluronic acid, the composition of the hyaluronic acid composition, the preparation method of the hyaluronic acid composition and the like are the same as those in example 1, except that: resveratrol was used in the preparation of the hyaluronic acid composition instead of cationic hyaluronic acid.

Comparative example 4

The composition of a moisturizing and anti-aging cosmetic composition containing cationic hyaluronic acid, the composition of the hyaluronic acid composition, the preparation method of the hyaluronic acid composition and the like are the same as those in example 1, except that: the hyaluronic acid composition is prepared by using natural mucopolysaccharide trehalose instead of ultra-low molecular weight hyaluronic acid.

Comparative example 5

The composition of a moisturizing and anti-aging cosmetic composition containing cationic hyaluronic acid, the composition of the hyaluronic acid composition, the preparation method of the hyaluronic acid composition and the like are the same as those in example 1, except that: the hyaluronic acid composition is prepared by using natural mucopolysaccharide trehalose instead of ultra-low molecular weight hyaluronic acid, and using resveratrol instead of cationic hyaluronic acid.

Comparative example 6

The composition of a moisturizing and anti-aging cosmetic composition containing cationic hyaluronic acid and the composition of the hyaluronic acid composition are the same as in example 1;

the preparation method of the hyaluronic acid composition comprises the following specific steps:

(1) weighing the raw materials according to the parts by weight of each component in the composition, slowly and uniformly adding the ultra-low molecular hyaluronic acid into purified water with the mass 100 times that of the ultra-low molecular hyaluronic acid, controlling the adding time to be 1min, and then completely dissolving the ultra-low molecular hyaluronic acid under the stirring action of 200 r/min;

(2) slowly and uniformly adding cationic hyaluronic acid into purified water 100 times the mass of the cationic hyaluronic acid, controlling the adding time to be 1min, heating to 40 ℃ under the stirring action of 200r/min, and completely dissolving the cationic hyaluronic acid;

(3) slowly adding the solution in the step (2) into the solution in the step (1) under the stirring action of 200r/min, and stirring until the solution is clear and transparent, so as to form a uniformly dispersed spherical state in which the cationic hyaluronic acid is surrounded by the ultra-low molecular hyaluronic acid.

(4) Adding polydimethylsiloxane, acetyl hexapeptide-8, sodium polyglutamate and nicotinamide into the solution obtained in the step (3) under the stirring action of 200r/min to obtain a clear and transparent hyaluronic acid composition.

Comparative example 7

The composition of a moisturizing and anti-aging cosmetic composition containing cationic hyaluronic acid is the same as that of example 1;

the hyaluronic acid composition comprises: 6 parts of ultra-low molecular hyaluronic acid, 18 parts of cationic hyaluronic acid, 4 parts of polydimethylsiloxane, 4 parts of acetyl hexapeptide-82, 8 parts of sodium polyglutamate and 4 parts of nicotinamide

Wherein the molecular weight of the ultra-low molecular hyaluronic acid is 5000 Da;

the cationic hyaluronic acid has a molecular weight of 20WDa and a cationicity of 0.6.

The preparation method of the hyaluronic acid composition is the same as that of example 1.

Comparative example 8

The composition of a moisturizing and anti-aging cosmetic composition containing cationic hyaluronic acid is the same as that of example 1;

the hyaluronic acid composition comprises: 18 parts of ultra-low molecular hyaluronic acid, 6 parts of cationic hyaluronic acid, 4 parts of polydimethylsiloxane, 8 parts of sodium polyglutamate and 4 parts of nicotinamide

Wherein the molecular weight of the ultra-low molecular hyaluronic acid is 5000 Da;

the cationic hyaluronic acid has a molecular weight of 20WDa and a cationicity of 0.6.

The preparation method of the hyaluronic acid composition is the same as that of example 1.

The moisturizing and anti-aging effects of the moisturizing and anti-aging cosmetic compositions of examples 1 to 5 and comparative examples 1 to 8 were examined, and the experimental results were as follows:

1. and (3) moisture retention detection:

30 subjects aged 25-40 years were tested using a skin moisture content test probe Corneometer CM 825 from CK, Germany. The inner forearm of the subject should be kept free of any cosmetic product 2-3 days before applying the test sample. The test area mark should be made on the inner side of the forearm of the test subject, the area of the test area is 3cm multiplied by 3cm, a plurality of areas can be marked on the same arm at the same time, and the interval between each test area is at least 1 cm. The test areas of the products of the examples and comparative examples should be randomly distributed over the left and right arm mark areas during application to ensure that the test area locations of all test samples are statistically balanced. The test specimens were applied in a single application in an amount of 1mg, and the test specimens were applied uniformly to the test area. The test subjects used the test samples in the test area daily, morning and evening during the test period, and after use the test samples were stored in a home freezer. Before each instrument test, the testee needs to clean the inner sides of the forearms of both hands uniformly, the cleaning method is to wipe the forearms clean by using dry facial tissues, then sit still for 20min in a room meeting the standard, cannot drink water and beverages, expose the forearms, place the forearms in a test state and keep relaxed. Test times were before use, after 8 hours of use, after 2 weeks and after 4 weeks.

Table one: skin moisture content (MMV) of different samples

From the above data analysis, it can be seen that:

(1) from the data analysis of comparative examples 1 and 2, it is understood that the moisture content in the skin is slightly increased by adding only one of the ultra-low molecular hyaluronic acid and the cationic hyaluronic acid, because the ultra-low molecular hyaluronic acid is absorbed instantaneously to bind with water molecules in the skin, but the water is slowly lost without the protective barrier formed by the cationic hyaluronic acid in the skin. And the absorption channel opened by ultra-low molecules entering the skin instantly is also lacked, so that the speed of the cationic hyaluronic acid entering the skin is very slow, and the moisturizing effect of the skin is influenced.

(2) According to the data analysis of comparative example 3, even if the ultra-low molecular hyaluronic acid exists, the long-term moisturizing effect can not be achieved due to the absence of the components capable of participating in the co-construction of the protective layer of the skin tissue.

(3) According to the data analysis of the comparative examples 2 and 4, the ultra-low molecular hyaluronic acid plays an important role in opening skin absorption channels and improving the protection effect of the skin care product.

(4) From the data analysis of comparative example 5, it is found that the water retention efficacy of the hyaluronic acid composition is more prominent.

(5) As can be seen from the comparative analysis of the data of example 2 and comparative example 6, the ultra-low molecular hyaluronic acid and the cationic hyaluronic acid are directly mixed, and then the sodium polyglutamate, the nicotinamide, the polydimethylsiloxane and the acetyl hexapeptide-8 are added into the mixture, so that the sodium polyglutamate, the nicotinamide, the polydimethylsiloxane and the acetyl hexapeptide-8 are not enclosed in the spherical liquid formed by the ultra-low molecular weight hyaluronic acid, the absorption of the spherical liquid is influenced, the repairing effect of the skin is influenced, and the moisturizing and anti-aging effects of the skin are reduced.

(6) As can be seen from comparative analysis of the data of examples 1 to 5 and comparative examples 7 to 8, when the ratio of the ultra-low molecular weight hyaluronic acid to the cationic hyaluronic acid is 1:3 and 3:1, the moisturizing effect is reduced, because when the ratio of the ultra-low molecular weight hyaluronic acid to the cationic hyaluronic acid is 1:3, the amount of the ultra-low molecular weight hyaluronic acid is too small to completely surround the cations, so that a part of the cationic hyaluronic acid is difficult to enter skin tissues, the anti-aging effect of the skin is reduced, and the moisturizing effect of the skin is reduced; when the ratio of the ultra-low molecular weight hyaluronic acid to the cationic hyaluronic acid is 3:1, the cationic hyaluronic acid enters skin tissues under the protection of the ultra-low molecular weight hyaluronic acid, but the skin aging resistance is reduced due to too small amount of the ultra-low molecular weight hyaluronic acid, so that the skin water retention effect is reduced.

2. And (3) anti-aging test:

the skin elasticity test of the inner forearm test area of the subject was performed using a skin elasticity tester Cutomer Dual MPA580 from CK, Germany to reflect the anti-aging effect of the present invention, and the average of the skin elasticity values measured 3 times per test area is as good as being closer to 1. Finally, the average value of the skin elasticity values of the 30 subjects of examples 1 to 5 and comparative examples 1 to 8 was counted.

Table two: skin elasticity values of different samples

From the above data analysis, it can be seen that:

(1) from the data analysis of comparative examples 1 and 2, it can be seen that the change of the elastic value in the skin is small by adding only one of the ultra-low molecular hyaluronic acid and the cationic hyaluronic acid, because the moisture content in the skin is reduced, the normal division and proliferation of cells are hindered, the normal metabolism of the cells is affected, and the skin lacks the protection of the antioxidant protective component, which accelerates the aging of skin tissue cells.

(2) As can be seen from the data analysis of comparative example 3, the skin elasticity value of comparative example 3 was significantly decreased from that of example 2 after replacing the cationic hyaluronic acid with resveratrol having antioxidant effect, because resveratrol has only the antioxidant function of the cationic hyaluronic acid and lacks the water retention property of the cationic hyaluronic acid film-forming, so that the anti-aging effect was poor.

(3) As can be seen from the data analysis of comparative example 4, the instant absorption channel opened by the ultra-low molecular hyaluronic acid is lacked, the antioxidant moisturizing component is difficult to enter, and the moisturizing and anti-aging effects are still not achieved.

(4) As can be seen from the data analysis of comparative examples 3-5, the ultra-low molecular hyaluronic acid and the cationic hyaluronic acid supplement each other, and in the absence of one of them, it is difficult for skin tissue cells to undergo normal metabolism and replacement of normal tissue cells, resulting in accelerated skin aging.

(5) As can be seen from the comparative analysis of the data of example 2 and comparative example 6, the ultra-low molecular hyaluronic acid and the cationic hyaluronic acid are directly mixed, and then the sodium polyglutamate, the nicotinamide, the polydimethylsiloxane and the acetyl hexapeptide-8 are added into the mixture, so that the sodium polyglutamate, the nicotinamide, the polydimethylsiloxane and the acetyl hexapeptide-8 are not enclosed in the spherical liquid formed by the ultra-low molecular weight hyaluronic acid, the absorption of the spherical liquid is influenced, the repairing effect of the skin is influenced, and the moisturizing and anti-aging effects of the skin are reduced.

(6) As can be seen from comparative analysis of the data of examples 1-5 and comparative examples 7-8, when the ratio of the ultra-low molecular weight hyaluronic acid to the cationic hyaluronic acid is 1:3 and 3:1, the moisturizing effect is reduced, because when the ratio of the ultra-low molecular weight hyaluronic acid to the cationic hyaluronic acid is 1:3, the amount of the ultra-low molecular weight hyaluronic acid is too small to completely surround the cations, so that a part of the cationic hyaluronic acid is difficult to enter skin tissues, and the skin aging resistance is reduced; when the ratio of the ultra-low molecular weight hyaluronic acid to the cationic hyaluronic acid is 3:1, the cationic hyaluronic acid enters skin tissues under the protection of the ultra-low molecular weight hyaluronic acid, but the anti-aging capability of the skin is reduced due to too small amount of the ultra-low molecular weight hyaluronic acid.

All percentages used in the present invention are mass percentages unless otherwise indicated.

Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.