CN111603411A - Essence containing hyaluronic acid and preparation method thereof - Google Patents
Essence containing hyaluronic acid and preparation method thereof Download PDFInfo
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- 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
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- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
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- A61K8/00—Cosmetics or similar toiletry preparations
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- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/40—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
- A61K8/44—Aminocarboxylic acids or derivatives thereof, e.g. aminocarboxylic acids containing sulfur; Salts; Esters or N-acylated derivatives thereof
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- 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
- A61K8/49—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
- A61K8/4906—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with one nitrogen as the only hetero atom
- A61K8/4913—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with one nitrogen as the only hetero atom having five membered rings, e.g. pyrrolidone carboxylic acid
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- A61K8/00—Cosmetics or similar toiletry preparations
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- A61K8/67—Vitamins
- A61K8/673—Vitamin B group
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- 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
- A61K8/67—Vitamins
- A61K8/676—Ascorbic acid, i.e. vitamin C
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- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/81—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
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- 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
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- A61K8/89—Polysiloxanes
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- 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
- A61K8/895—Polysiloxanes containing silicon bound to unsaturated aliphatic groups, e.g. vinyl dimethicone
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- A61Q19/00—Preparations for care of the skin
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- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
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Abstract
The invention discloses an essence containing hyaluronic acid and a preparation method thereof, wherein the essence comprises the following effective components: the hyaluronic acid skin-feel modifier comprises a hyaluronic acid processed product, a gel, a skin-feel modifier and an effective component, wherein the hyaluronic acid processed product is granular and is added into a mixed phase consisting of the gel, the skin-feel modifier and the effective component step by step, a formed system taking the gel as a main body and provided with hyaluronic acid particles is stable and does not delaminate, the hyaluronic acid particles can be uniformly dispersed in the system, the phenomena of particle aggregation and precipitation cannot occur, and the effectiveness of the product is ensured.
Description
Technical Field
The invention relates to the technical field of hyaluronic acid, and particularly relates to an essence containing hyaluronic acid and a preparation method thereof.
Background
Hyaluronic acid, also known as hyaluronic acid, is an acidic macromolecular mucopolysaccharide composed of N D-glucuronic acid and N-acetylglucosamine disaccharide units. The hyaluronic acid molecule can carry more than 500 times of water, so the hyaluronic acid molecule is the best natural moisturizing ingredient recognized at present and is widely applied to skin care products and cosmetics.
However, when the hyaluronic acid with large molecular weight is used in cosmetics, the hyaluronic acid is easy to be drawn and smeared during application, and the skin is easy to be sticky and poor in skin feel when sweating or in a relatively humid environment. Meanwhile, hyaluronic acid has poor stability and is easily degraded by acid, alkali, heat, free radicals, hyaluronidase and the like, so that the application of hyaluronic acid is limited. The cross-linked or modified hyaluronic acid has better stability on the basis of keeping the original skin feeling, moisturizing and other effects of the natural hyaluronic acid, and the application of the cross-linked or modified hyaluronic acid in the field of cosmetics can be possibly perfected.
In the prior art, hyaluronic acid is prepared into a hyaluronic acid particle form to increase the addition amount of hyaluronic acid, but hyaluronic acid particles are used as additives, and are unevenly distributed in a suspension system to cause the phenomena of particle aggregation and precipitation, and the suspension system is usually poor in stability and easy to delaminate, so that the stability and the efficacy of a product are greatly influenced.
Therefore, the essence containing hyaluronic acid and the preparation method thereof are provided for solving the disadvantages.
Disclosure of Invention
The invention aims to provide an essence containing hyaluronic acid and a preparation method thereof, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a hyaluronic acid-containing essence comprises the following effective components: hyaluronic acid processed product, gel, skin feeling regulator, and effective component.
As a further optimization of the scheme, the essence consists of 2-5% of hyaluronic acid processed product, 25-45% of gel, 0.5-5% of skin feel conditioning agent, 20-40% of effective components and the balance of purified water.
As a further optimization of the above scheme, the hyaluronic acid processed product is in a granular shape.
As a further optimization of the scheme, the hyaluronic acid processed product is prepared by sieving a hyaluronic acid cross-linked polymer with a 50-mesh sieve, collecting, pressing into a sheet shape by using a pressing roller, and crushing into granules with the particle size of less than 0.15 mm.
As a further optimization of the scheme, the pressure of the compression roller is 3-5Mpa, and the compression speed of the compression roller is 10-20 r/min.
As a further optimization of the above scheme, the gel is composed of polyacrylic acid, poloxamer, purified water, polyacrylic acid: poloxamer: the weight ratio of the purified water is 1: 1: 20-5: 3: 20.
as a further optimization of the scheme, the skin feeling regulator is at least one of hyaluronic acid elastomer, silicone elastomer and polyglycerol-10
As a further optimization of the scheme, the effective components consist of water-soluble amino acids, water-soluble vitamins, hyaluronate and purified water, wherein the water-soluble amino acids: water-soluble vitamins: hyaluronic acid salt: the weight ratio of the purified water is 0.05: 0.05: 0.05: 100-0.5: 0.5: 0.125: 100.
as a further optimization of the above scheme, the water-soluble amino acid may be water-soluble amino acid reported in the prior art and capable of being applied in skin care products, such as at least one of glycine, proline, hydroxyproline, lysine hydrochloride, isoleucine, leucine, serine, alanine, aspartic acid, tyrosine, glutamic acid, phenylalanine, arginine hydrochloride, valine, threonine, histidine hydrochloride, tryptophan, methionine, cystine, cysteine, and the like. The water-soluble vitamin can be water-soluble vitamins which are reported in the prior art and can be applied to skin care products, such as at least one of vitamin B1, vitamin B2, nicotinamide, vitamin B6, vitamin B12, folic acid, vitamin C and the like. The hyaluronic acid salt can be at least one of sodium salt, potassium salt, calcium salt, magnesium salt and zinc salt of hyaluronic acid.
As a further optimization of the above solution, the hyaluronic acid elastomer is an elastomer of hyaluronic acid or a hyaluronate cross-linked polymer.
As a further optimization of the above solution, the silicone elastomer is an elastomer of a dimethicone crosspolymer or a dimethicone/phenyl vinyl dimethicone crosspolymer.
A method for preparing an essence containing hyaluronic acid, the method comprising the steps of:
s1, pressing and crushing a hyaluronic acid processed object to form hyaluronic acid particles;
s2, adding purified water into an emulsification tank, heating to 75-90 ℃, keeping for 15-30min, adding polyacrylic acid and poloxamer, stirring (20-60rpm/min) for 1-2h, adjusting the pH to 3.0-3.5 by using a pH value regulator to obtain gel, and cooling to 40-50 ℃ for keeping to obtain a to-be-mixed phase A;
s3, mixing the skin feel modifier with a proper amount of purified water, heating to 40-50 ℃, and stirring (20-60rpm/min) for 2-4 hours to obtain a phase B to be mixed;
s4, mixing water-soluble amino acid, water-soluble vitamin, hyaluronate with purified water, heating to 40-50 ℃, and stirring (20-60rpm/min) for 2-4 hours to obtain a phase C to be mixed;
s5, mixing the phase A to be mixed, the phase B to be mixed and the phase C to be mixed, heating to 40-50 ℃, and stirring (20-60rpm/min) for 2-4h to obtain a phase D to be mixed;
s6, adding the hyaluronic acid particles into the mixed phase D step by step according to the following steps, and adjusting the pH value by using a pH value regulator to obtain the essence.
| Step (ii) of | Time of day | Temperature of | Procedure for the preparation of the | Hyaluronic acid particle addition | pH value |
| 1 | 0-15min | 50℃ | Stirring (20-40rpm/min) | 60～80％ | 3.5-4.5 |
| 2 | 15-30min | 35℃ | Stirring (10-20rpm/min) | Balance of | 4.5-5.5 |
| 3 | 31-60min | 35℃ | Stirring (10-20rpm/min) | —— | 6.5-7.0 |
The above-mentioned pH regulators are well known in the art and can be selected by the person skilled in the art from the prior art.
Compared with the prior art, the invention has the following advantages:
according to the invention, the hyaluronic acid processed product is granular and is added into the mixed phase consisting of the gel, the skin feel regulator and the functional components step by step, and the formed system taking the gel as a main body and provided with hyaluronic acid particles is stable and not layered, and can uniformly disperse the hyaluronic acid particles, so that the phenomena of aggregation and precipitation of the hyaluronic acid particles due to uneven distribution are avoided, the maximum effect of the effective components is exerted, and the efficacy of the product is ensured; in addition, the skin feel regulator can promote essence smearing and leveling, improve the adhesiveness of the essence, is not easy to run off and waste, and helps the skin to better absorb the essence.
Detailed Description
The following description of the exemplary embodiments of the present application, including various details of the embodiments of the present application to assist in understanding, should be taken as exemplary only. Accordingly, those of ordinary skill in the art will recognize that various changes and modifications of the embodiments described herein can be made without departing from the scope and spirit of the present application. Also, descriptions of well-known functions and constructions are omitted in the following description for clarity and conciseness.
Example 1 preparation of a serum containing hyaluronic acid
The components: 2g of hyaluronic acid processed product, 25g of gel, 0.5g of skin feel conditioning agent, 20g of functional component and 52.5g of purified water, wherein the gel comprises 1.14g of polyacrylic acid, 1.14g of poloxamer and 22.7g of purified water; the functional components comprise 0.002g of glycine, 0.002g of tyrosine, 0.002g of threonine, 0.002g of proline, 0.002g of leucine, 10.002g of vitamin B, 20.002g of vitamin B, 0.006g of vitamin C, 0.01g of sodium hyaluronate and 19.97g of purified water.
The hyaluronic acid processing product is granular, the hyaluronic acid processing product is hyaluronic acid cross-linked polymer, the hyaluronic acid cross-linked polymer is sieved by a 50-mesh sieve and collected, the hyaluronic acid cross-linked polymer is pressed into a sheet shape by a pressing roller after being collected, the sheet shape is formed by crushing, the granular particle size is less than 0.15mm, the pressure of the pressing roller is 3Mpa, and the pressing speed of the pressing roller is 10 r/min.
A preparation method of essence containing hyaluronic acid comprises the following steps:
s1, pressing and crushing a hyaluronic acid processed object to form hyaluronic acid particles;
s2, adding purified water into an emulsification tank, heating to 75 ℃, keeping for 15min, adding polyacrylic acid and poloxamer, stirring (20rpm/min) for 1h, adjusting the pH to 3.0 by using a pH value regulator to obtain gel, and cooling to 40 ℃ for keeping to obtain a to-be-mixed phase A;
s3, mixing the hyaluronic acid elastomer with a proper amount of purified water, heating to 40 ℃, and stirring (20rpm/min) for 2 hours to obtain a phase B to be mixed;
s4, heating the water-soluble amino acid, the water-soluble vitamin, the sodium hyaluronate and the purified water to 40 ℃, and stirring (20rpm/min) for 2h to obtain a to-be-mixed phase C;
s5, mixing the phase A to be mixed, the phase B to be mixed and the phase C to be mixed, heating to 40-50 ℃, and stirring (20rpm/min) for 2h to obtain a phase D to be mixed;
s6, adding the hyaluronic acid particles into the mixed phase D step by step according to the following steps to obtain the essence.
| Step (ii) of | Time of day | Temperature of | Procedure for the preparation of the | Hyaluronic acid particle addition | pH value |
| 1 | 0-15min | 50℃ | Stirring (20rpm/min) | 60％ | 3.5 |
| 2 | 15-30min | 35℃ | Stirring (10rpm/min) | 40％ | 4.5 |
| 3 | 31-60min | 35℃ | Stirring (10rpm/min) | —— | 6.0 |
Example 2 preparation of a serum containing hyaluronic acid
The components: 5g of hyaluronic acid processed product, 45g of gel, 5g of skin feel regulator, 40g of effective component and 5g of purified water, wherein the gel comprises 8.0g of polyacrylic acid, 4.8g of poloxamer and 32.2g of purified water; the functional components comprise 0.04g of glycine, 0.04g of tyrosine, 0.04g of threonine, 0.04g of proline, 0.04g of leucine, 10.04g of vitamin B, 20.04g of vitamin B, 0.12g of vitamin C, 0.05g of sodium hyaluronate and 39.55g of purified water.
The hyaluronic acid processed product is granular, the hyaluronic acid processed product is sieved by a 50-mesh sieve and collected, the hyaluronic acid processed product is pressed into a sheet shape by a pressing roller after being collected, the sheet shape is crushed to form granules, the particle size of the granules is less than 0.15mm, the pressure of the pressing roller is 5Mpa, and the pressing speed of the pressing roller is 20 r/min.
A preparation method of essence containing hyaluronic acid comprises the following steps:
s1, pressing and crushing a hyaluronic acid processed object to form hyaluronic acid particles;
s2, adding purified water into an emulsification tank, heating to 90 ℃, keeping for 30min, adding polyacrylic acid and poloxamer, stirring (60rpm/min) for 2h, adjusting the pH to 3.5 by using a pH value regulator to obtain gel, and cooling to 50 ℃ for keeping to obtain a to-be-mixed phase A;
s3, mixing the organic silicon elastomer with a proper amount of purified water, heating to 50 ℃, and stirring (60rpm/min) for 4 hours to obtain a phase B to be mixed;
s4, heating the water-soluble amino acid, the water-soluble vitamin, the sodium hyaluronate and the purified water to 50 ℃, and stirring (60rpm/min) for 4 hours to obtain a to-be-mixed phase C;
s5, mixing the phase A to be mixed, the phase B to be mixed and the phase C to be mixed, heating to 40-50 ℃, and stirring (60rpm/min) for 4 hours to obtain a phase D to be mixed;
s6, adding the hyaluronic acid particles into the mixed phase D step by step according to the following steps to obtain the essence.
| Step (ii) of | Time of day | Temperature of | Procedure for the preparation of the | Hyaluronic acid particle addition | pH value |
| 1 | 0-15min | 50℃ | Stirring (40rpm/min) | 80％ | 4.5 |
| 2 | 15-30min | 35℃ | Stirring (20rpm/min) | 20％ | 5.5 |
| 3 | 31-60min | 35℃ | Stirring (20rpm/min) | —— | 7.0 |
Example 3 preparation of a serum containing hyaluronic acid
The components: 3g of hyaluronic acid processed product, 38g of gel, 1.5g of skin feel regulator, 29g of functional component and 28.5g of purified water, wherein the gel comprises 4.85g of polyacrylic acid, 3.9g of poloxamer and 29.25g of purified water; the effective components comprise 0.014g of glycine, 0.014g of tyrosine, 0.014g of threonine, 0.014g of proline, 0.014g of leucine, 0.014g of vitamin B10.014g, vitamin B20.014g, 0.042g of vitamin C, 0.029g of sodium hyaluronate and 28.83g of purified water.
The hyaluronic acid processed product is granular, the hyaluronic acid processed product is sieved by a 50-mesh sieve and collected, the hyaluronic acid processed product is pressed into a sheet shape by a pressing roller after being collected, the sheet shape is crushed to form granules, the particle size of the granules is less than 0.15mm, the pressure of the pressing roller is 5Mpa, and the pressing speed of the pressing roller is 10 r/min.
A preparation method of essence containing hyaluronic acid comprises the following steps:
s1, pressing and crushing a hyaluronic acid processed object to form hyaluronic acid particles;
s2, adding purified water into an emulsification tank, heating to 80 ℃, keeping for 20min, adding polyacrylic acid and poloxamer, stirring (40rpm/min) for 1.5h, adjusting the pH to 3.2 by using a pH value regulator to obtain gel, and cooling to 45 ℃ for keeping to obtain a to-be-mixed phase A;
s3, mixing the hyaluronic acid elastomer with a proper amount of purified water, heating to 45 ℃, and stirring (40rpm/min) for 3 hours to obtain a phase B to be mixed;
s4, heating the water-soluble amino acid, the water-soluble vitamin, the sodium hyaluronate and the purified water to 45 ℃, and stirring (40rpm/min) for 3 hours to obtain a to-be-mixed phase C;
s5, mixing the phase A to be mixed, the phase B to be mixed and the phase C to be mixed, heating to 40-50 ℃, and stirring (40rpm/min) for 3 hours to obtain a phase D to be mixed;
s6, adding the hyaluronic acid particles into the mixed phase D step by step according to the following steps to obtain the essence.
Example 4 preparation of a serum containing hyaluronic acid
The components: 2.5g of hyaluronic acid processed product, 35g of gel, 2g of skin feel conditioning agent, 35g of effective component and 25.5g of purified water, wherein the gel comprises 4.48 g of polyacrylic acid, 3.59g of poloxamer and 26.93g of purified water; the functional components comprise 0.017g of glycine, 0.017g of tyrosine, 0.017g of threonine, 0.017g of proline, 0.017g of leucine, 0.017g of vitamin B10.017g, 0.052g of vitamin C, 0.035g of sodium hyaluronate and 34.79g of purified water.
The hyaluronic acid processed product is granular, the hyaluronic acid processed product is sieved by a 50-mesh sieve and collected, the hyaluronic acid processed product is pressed into a sheet shape by a pressing roller after being collected, the sheet shape is crushed to form granules, the particle size of the granules is less than 0.15mm, the pressure of the pressing roller is 5Mpa, and the pressing speed of the pressing roller is 20 r/min.
A preparation method of essence containing hyaluronic acid comprises the following steps:
s1, pressing and crushing a hyaluronic acid processed object to form hyaluronic acid particles;
s2, adding purified water into an emulsification tank, heating to 85 ℃, keeping for 20min, adding polyacrylic acid and poloxamer, stirring (40rpm/min) for 1.5h, adjusting the pH to 3.5 by using a pH value regulator to obtain gel, and cooling to 45 ℃ for keeping to obtain a to-be-mixed phase A;
s3, mixing the hyaluronic acid elastomer with a proper amount of purified water, heating to 45 ℃, and stirring (40rpm/min) for 2.5 hours to obtain a phase B to be mixed;
s4, heating the water-soluble amino acid, the water-soluble vitamin, the sodium hyaluronate and the purified water to 45 ℃, and stirring (40rpm/min) for 2.5 hours to obtain a to-be-mixed phase C;
s5, mixing the phase A to be mixed, the phase B to be mixed and the phase C to be mixed, heating to 40-50 ℃, and stirring (40rpm/min) for 2.5 hours to obtain a phase D to be mixed;
s6, adding the hyaluronic acid particles into the mixed phase D step by step according to the following steps to obtain the essence.
| Step (ii) of | Time of day | Temperature of | Procedure for the preparation of the | Hyaluronic acid particle addition | pH value |
| 1 | 0-15min | 50℃ | Stirring (20rpm/min) | 65％ | 4.5 |
| 2 | 15-30min | 35℃ | Stirring (20rpm/min) | 35％ | 5.0 |
| 3 | 31-60min | 35℃ | Stirring (10rpm/min) | —— | 6.8 |
Example 5 preparation of a serum containing hyaluronic acid
The components: 4g of hyaluronic acid processed product, 40g of gel, 2.5g of skin feel regulator, 30g of effective component and 23.5g of purified water, wherein the gel comprises 4.8g of polyacrylic acid, 3.2g of poloxamer and 32g of purified water, and the pH value is adjusted to 3.5; the functional components comprise 0.015g of glycine, 0.015g of tyrosine, 0.015g of threonine, 0.015g of proline, 0.015g of leucine, 10.015g of vitamin B, 20.015g of vitamin B, 0.045g of vitamin C, 0.03g of sodium hyaluronate and 29.8g of purified water.
The hyaluronic acid processed product is granular, the hyaluronic acid processed product is sieved by a 50-mesh sieve and collected, the hyaluronic acid processed product is pressed into a sheet shape by a pressing roller after being collected, and the sheet shape is crushed into granules, the particle size of the granules is less than 0.15mm, the pressure of the pressing roller is 3Mpa, and the pressing speed of the pressing roller is 20 r/min.
A preparation method of essence containing hyaluronic acid comprises the following steps:
s1, pressing and crushing a hyaluronic acid processed object to form hyaluronic acid particles;
s2, adding purified water into an emulsification tank, heating to 90 ℃, keeping for 20min, adding polyacrylic acid and poloxamer, stirring (50rpm/min) for 2h, adjusting the pH to 3.5 by using a pH value regulator to obtain gel, and cooling to 40 ℃ for keeping to obtain a to-be-mixed phase A;
s3, mixing the hyaluronic acid elastomer with a proper amount of purified water, heating to 40 ℃, and stirring (50rpm/min) for 2 hours to obtain a phase B to be mixed;
s4, heating the water-soluble amino acid, the water-soluble vitamin, the sodium hyaluronate and the purified water to 40 ℃, and stirring (50rpm/min) for 2h to obtain a to-be-mixed phase C;
s5, mixing the phase A to be mixed, the phase B to be mixed and the phase C to be mixed, heating to 40-50 ℃, and stirring (50rpm/min) for 2h to obtain a phase D to be mixed;
s6, adding the hyaluronic acid particles into the mixed phase D step by step according to the following steps to obtain the essence.
| Step (ii) of | Time of day | Temperature of | Procedure for the preparation of the | Hyaluronic acid particle addition | pH value |
| 1 | 0-15min | 50℃ | Stirring (30rpm/min) | 75％ | 4.0 |
| 2 | 15-30min | 35℃ | Stirring (30rpm/min) | 25％ | 5.0 |
| 3 | 31-60min | 35℃ | Stirring (10rpm/min) | —— | 6.8 |
Comparative examples 1 to 3 are different from example 5 in the addition step of hyaluronic acid particles:
comparative example 1 addition procedure of hyaluronic acid particles:
| step (ii) of | Time of day | Temperature of | Procedure for the preparation of the | Hyaluronic acid particle addition | pH value |
| 1 | 0-30min | 50℃ | Stirring (30rpm/min) | 100％ | 6.8 |
| 2 | 31-60min | 35℃ | Stirring (10rpm/min) | —— | 6.8 |
Comparative example 2 addition procedure of hyaluronic acid particles:
| step (ii) of | Time of day | Temperature of | Procedure for the preparation of the | Hyaluronic acid particle addition | pH value |
| 1 | 0-15min | 50℃ | Stirring (30rpm/min) | 55％ | 6.8 |
| 2 | 15-30min | 35℃ | Stirring (30rpm/min) | 45％ | 6.8 |
| 3 | 31-60min | 35℃ | Stirring (10rpm/min) | —— | 6.8 |
Comparative example 3 addition procedure of hyaluronic acid particles:
| step (ii) of | Time of day | Temperature of | Procedure for the preparation of the | Hyaluronic acid particle addition | pH value |
| 1 | 0-15min | 25℃ | Stirring (30rpm/min) | 80％ | 3.5 |
| 2 | 15-30min | 25℃ | Stirring (30rpm/min) | 20％ | 6.8 |
| 3 | 31-60min | 35℃ | Stirring (10rpm/min) | —— | 6.8 |
Comparative example 4 differs from example 5 in that the gel was added in an amount of 15g, comprising 1.8g of polyacrylic acid, 1.2g of poloxamer, and 12g of purified water.
Comparative example 5 differs from example 5 in that the gel was added in an amount of 60g, comprising 7.2g of polyacrylic acid, 4.8g of poloxamer, and 48g of purified water.
Comparative example 6 differs from example 5 in that no gel is present.
Comparative example 7 is different from example 5 in that the amount of hyaluronic acid processed product added is 10 g.
Test example 1 suspension stability
50ml of each of examples 1 to 5 and comparative examples 1 to 7 was taken in a reagent bottle, stored in a constant temperature and humidity test chamber at 60 ℃ for 2 weeks, and the initial turbidity and the turbidity of the upper layer solution after storage for 2 weeks were measured by a turbidity meter, and the measurement results are shown in the following table:
and (3) knotting: the turbidity of the upper solution of the example is not changed greatly after the upper solution is placed for 2 weeks, and the turbidity of the comparative example is obviously reduced after the upper solution is placed for two weeks, so that the phenomena of precipitation and aggregation of gel particles of the upper solution of the example are not obvious, and the phenomena of precipitation and aggregation of gel particles of the upper solution of the comparative example are shown.
Test example 2 sedimentation volume ratio
20mL of each of examples 1-5 and comparative examples 1-7 was placed in a measuring cylinder, the initial height H of the liquid was measured, after standing for 30min, the final height H 'of the sediment was observed when the sedimentation surface was not changed, and the sedimentation volume ratio F, F ═ H'/HF, was calculated as follows, and if it was 0.90 or more, it was confirmed that the product was in accordance with the specification for suspension in "Chinese pharmacopoeia 2015 edition" and the larger the value of F, the more stable the suspension. The results of the experiment are shown in the following table:
| sample (I) | F value |
| Example 1 | 0.932 |
| Example 2 | 0.927 |
| Example 3 | 0.948 |
| Example 4 | 0.917 |
| Example 5 | 0.938 |
| Comparative example 1 | 0.519 |
| Comparative example 2 | 0.644 |
| Comparative example 3 | 0.709 |
| Comparative example 4 | 0.812 |
| Comparative example 5 | 0.911 |
| Comparative example 6 | 0.344 |
| Comparative example 7 | 0.682 |
And (3) knotting: the ratio of the sedimentation solvent in example 5 is significantly higher than the ratio 1-3, which shows that the more stable the system is when hyaluronic acid particles are added in certain steps; the ratio of the sedimentation solvent in example 5 is obviously higher than the ratio of 4-7, which shows that the stability of the system can be enhanced by mixing the effective components according to a certain ratio.
Test example 3 layered test
The samples of examples 1 to 5 and comparative examples 1 to 7 were stored in a glass container in a sealed manner, and after storing at-5 ℃, 25 ℃ and 45 ℃ for 1 month, they were allowed to stand at room temperature to observe the delamination. The results of the experiment are shown in the following table:
and (3) knotting: in the examples, no delamination occurred, and in comparative examples 1-2 and 6, delamination occurred after storage at-5 ℃, 25 ℃ and 45 ℃ for 1 month, indicating that the suspension was unstable without adding gel or adding hyaluronic acid particles according to a certain procedure.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (11)
1. The essence containing hyaluronic acid is characterized in that: comprises the following effective components: hyaluronic acid processed product, gel, skin feeling regulator, and effective component.
2. The essence according to claim 1, characterized by comprising the following active ingredients: 2-5% of hyaluronic acid processed product, 25-45% of gel, 0.5-5% of skin feel regulator, 20-40% of effective component and the balance of purified water.
3. The essence according to claim 1 or 2, characterized in that: the hyaluronic acid processed product is granular.
4. The essence according to claim 1, 2 or 3, characterized in that: the hyaluronic acid processed product is prepared by sieving a sodium hyaluronate cross-linked polymer with a 50-mesh sieve, collecting, pressing into a sheet shape by using a pressing roller, and crushing into granules, wherein the particle size of the granules is less than 0.15 mm.
5. The essence of claim 4, wherein: the pressure of the compression roller is 3-5Mpa, and the compression speed of the compression roller is 10-20 r/min.
6. The essence according to claim 1 or 2, characterized in that: the gel is composed of polyacrylic acid, poloxamer and purified water, wherein the polyacrylic acid: poloxamer: the weight ratio of the purified water is 1: 1: 20-5: 3: 20.
7. the essence of claim 1, wherein: the skin feeling regulator is at least one of hyaluronic acid elastomer, silicone elastomer and polyglycerol-10.
8. The essence of claim 1, wherein: the functional components consist of water-soluble amino acid, water-soluble vitamin, hyaluronate and purified water, wherein the water-soluble amino acid: water-soluble vitamins: hyaluronic acid salt: the weight ratio of the purified water is 0.05: 0.05: 0.05: 100-0.5: 0.5: 0.125: 100.
9. the essence of claim 7, wherein: the hyaluronic acid elastomer is an elastomer of hyaluronic acid or a hyaluronate cross-linked polymer.
10. The essence of claim 7, wherein: the organic silicon elastomer is an elastomer of a polydimethylsiloxane cross-linked polymer or a polydimethylsiloxane/phenyl vinyl polydimethylsiloxane cross-linked polymer.
11. A preparation method of essence containing hyaluronic acid is characterized by comprising the following steps: the method comprises the following steps: the serum containing hyaluronic acid according to any of claims 1-10, comprising the steps of:
s1, pressing and crushing a hyaluronic acid processed object to form hyaluronic acid particles;
s2, adding purified water into an emulsification tank, heating to 75-90 ℃, keeping for 15-30min, adding polyacrylic acid and poloxamer, stirring (20-60rpm/min) for 1-2h, adjusting the pH to 3.0-3.5 by using a pH value regulator to obtain gel, and cooling to 40-50 ℃ for keeping to obtain a to-be-mixed phase A;
s3, mixing the skin feel modifier with a proper amount of purified water, heating to 40-50 ℃, and stirring (20-60rpm/min) for 2-4 hours to obtain a phase B to be mixed;
s4, mixing water-soluble amino acid, water-soluble vitamin, hyaluronate with purified water, heating to 40-50 ℃, and stirring (20-60rpm/min) for 2-4 hours to obtain a phase C to be mixed;
s5, mixing the phase A to be mixed, the phase B to be mixed and the phase C to be mixed, heating to 40-50 ℃, and stirring (20-60rpm/min) for 2-4h to obtain a phase D to be mixed;
s6, adding hyaluronic acid particles into the mixed phase D step by step according to the following steps, and adjusting the pH value by using a pH value regulator to obtain the essence:
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