CN112773734A - Hyaluronic acid skin-changing essence and preparation method thereof - Google Patents
Hyaluronic acid skin-changing essence and preparation method thereof Download PDFInfo
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- CN112773734A CN112773734A CN202011593784.5A CN202011593784A CN112773734A CN 112773734 A CN112773734 A CN 112773734A CN 202011593784 A CN202011593784 A CN 202011593784A CN 112773734 A CN112773734 A CN 112773734A
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- hyaluronic acid
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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
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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
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/31—Hydrocarbons
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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
- A61K8/30—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
- A61K8/41—Amines
- A61K8/416—Quaternary ammonium compounds
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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
- A61K8/84—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
- A61K8/894—Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone modified by a polyoxyalkylene group, e.g. cetyl dimethicone copolyol
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- 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
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- 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
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Abstract
The invention belongs to the technical field of cosmetics, and particularly relates to an identification method of hyaluronic acid skin-changing essence, which comprises the steps of firstly soaking hyaluronic acid essence in an amphoteric solvent, dissolving and separating a dodecyl dimethyl allyl ammonium chloride coating and a hexadecyl dimethyl allyl ammonium chloride coating, and then washing with deionized water to remove the hyaluronic acid essence with the dodecyl dimethyl allyl ammonium chloride coating and the hexadecyl dimethyl allyl ammonium chloride coating; then centrifugally separating to obtain an amphoteric solvent solution, and then destroying and removing a gasoline film outside the hyaluronic acid essence in a stirring and heating mode; and finally, identifying the structure of the hyaluronic acid essence after treatment through a reagent combination test reaction test and analyzing and calculating a result. The identification method is simple and easy to implement, is easy to popularize, and can have wide significance for the development of the field of cosmetics, particularly natural cosmetics, towards the green environmental protection direction.
Description
Technical Field
The invention belongs to the technical field of cosmetics, and particularly relates to hyaluronic acid and a preparation method thereof.
Background
Hyaluronic acid (Hyaluronan, Hyaluronicacid) is a transparent and viscous colloidal substance, is essentially a macromolecular glycosaminoglycan, is composed of glucuronyl-N-acetylglucosamine as disaccharide molecular units connected by branched chains, is filled in the space between cells and collagen fibers of a human body, and is the biggest difference from other glycosaminoglycans: it contains no sulfur. Hyaluronic acid is firstly separated from bovine vitreous humor by Meyer of university of Columbia in 1934, however, most of the existing hyaluronic acid is artificially synthesized products, most of the artificial products have strong chemical substances, and are harmful to human bodies when used, and an identification method which is easy to detect natural hyaluronic acid is currently lacked, so that any one of the problems needs to be solved urgently.
Disclosure of Invention
In order to solve one of the problems, the invention provides an identification method of hyaluronic acid skin-changing essence, which comprises the steps of firstly soaking the hyaluronic acid essence in an amphoteric solvent, dissolving and separating a dodecyl and hexadecyl dimethyl allyl ammonium chloride coating, and then washing with deionized water to remove the hyaluronic acid essence coated with the dodecyl and hexadecyl dimethyl allyl ammonium chloride; then centrifugally separating to obtain an amphoteric solvent solution, and then destroying and removing a gasoline film outside the hyaluronic acid essence in a stirring and heating mode; and finally, identifying the structure of the hyaluronic acid essence after treatment through a reagent combination test reaction test and analyzing and calculating a result.
Further, the amphoteric solvent is a mixture of methanol, ethanol, water and No. 3 white oil, the soaking mode is that the hyaluronic acid essence is soaked in the mixture of the methanol, the ethanol and the No. 3 white oil for a plurality of minutes at the temperature of 30-45 ℃, then the hyaluronic acid essence is filtered and separated, the mixture of the methanol and the ethanol is used for intermittent leaching for a plurality of times until no foam is generated on the surface of the hyaluronic acid essence when the hyaluronic acid essence is washed by a mixed solution of the methanol and the water, and the residual alcohols on the surface of the hyaluronic acid essence are dried by hot air; the deionized water washing comprises washing with deionized water at a temperature below 30 ℃ until liquid drops are hung on the surface of the hyaluronic acid essence; the centrifugal process adopts a centrifuge tube with a filter screen, the stirring and heating process comprises the steps of firstly placing the hyaluronic acid essence into a container for stirring, then blowing hot air with the temperature of more than 30 ℃ from bottom to top from the bottom of the container, and stirring under the heating of the air flow of the hot air until no obvious smell is generated, so as to obtain the treated hyaluronic acid essence; the medicament combination test comprises the steps of preparing the treated hyaluronic acid essence into 0.5-2% aqueous solution, adjusting the pH value of the aqueous solution, testing the viscosity A of the aqueous solution, dividing the aqueous solution into a plurality of parts, adding a cross-linking agent into each part to test the viscosity An of the aqueous solution, and analyzing and calculating the data result of the viscosity A and the viscosity An to obtain the result.
Further, after adjusting the pH of the aqueous solution to 7 to 9, the viscosity A thereof is measured, and then the solution is divided into at least 2 parts, one part is added with 0.5 to 3% of a boron-based crosslinking agent to measure the viscosity A1 thereof, and the other part is added with 0.5 to 2% of a zirconium-based crosslinking agent to measure the viscosity A2 thereof, when the viscosity value satisfies any one of the following formulas,the hyaluronic acid is judged to be non-natural hyaluronic acid. Further, when the solution was divided into at least 3 parts after the viscosity of the test solution was a, the viscosity of A3 was tested after adding 3 to 20% of the aldehyde-based acidic crosslinking agent to the third part of the solution, and when the viscosity of A3 was aIf so, judging the hyaluronic acid to be natural hyaluronic acid; when three solutions are available, 0.5 to 3 percent of boron crosslinking agent is added into one solution to measure the viscosity A1, 0.5 to 2 percent of zirconium crosslinking agent is added into the other solution to measure the viscosity A2, after 3 to 20 percent of aldehyde acid crosslinking agent is added into the third solution, the viscosity A3 is tested, when the values of the viscosities A1, A2 and A3 meet any one of the following formulas,the hyaluronic acid is judged to be natural hyaluronic acid.
Has the advantages that: the identification method is simple and easy to implement, is easy to popularize, and can have wide significance for the development of the field of cosmetics, particularly natural cosmetics, towards the green environmental protection direction.
Detailed Description
Firstly, soaking the hyaluronic acid essence in an amphoteric solvent, dissolving and separating a dodecyl and hexadecyl dimethyl allyl ammonium chloride coating, and washing with deionized water to remove the hyaluronic acid essence coated with the dodecyl and hexadecyl dimethyl allyl ammonium chloride; separating the amphoteric solvent solution by a centrifugal machine, and then destroying and removing a gasoline film outside the hyaluronic acid essence by stirring and heating; and finally, identifying the structure of the hyaluronic acid essence after treatment through a reagent combination test reaction test and analyzing and calculating a result.
Further, the amphoteric solvent is a mixture of methanol, ethanol, water and No. 3 white oil, and the soaking manner is that the hyaluronic acid essence is firstly mixed according to a mass ratio of 1:1, soaking in a mixture of methanol, ethanol and No. 3 white oil at the temperature of 30-45 ℃ for several minutes, diluting oil substances on the surface by the No. 3 white oil, filtering and separating, intermittently leaching for several times by using the mixture of the methanol and the ethanol with the mass ratio of 3:1 until no foam is generated on the surface of the hyaluronic acid essence when the hyaluronic acid essence is washed by using a mixed solution of methanol and water, and then, hot-drying alcohol substances remained on the surface of the hyaluronic acid essence by using hot air; the deionized water washing comprises washing with deionized water at a temperature below 30 ℃ until liquid drops are hung on the surface of the hyaluronic acid essence; the centrifugal process comprises the steps of centrifuging for 5-10 minutes at 1000 rotating speed by using a centrifugal tube with a filter screen, wherein the hyaluronic acid essence is placed in a container to be stirred for 10-30 minutes, then hot air with the temperature of more than 30 ℃ is blown from the bottom of the container from bottom to top, and the hyaluronic acid essence is stirred under the heating of the air flow of the hot air until no obvious odor is generated, so that the treated hyaluronic acid essence is obtained; the medicament combination test comprises the steps of preparing the treated hyaluronic acid essence into 0.5-2% aqueous solution, adjusting the pH value of the aqueous solution, testing the viscosity A of the aqueous solution, dividing the aqueous solution into a plurality of parts, adding a cross-linking agent into each part to test the viscosity An of the aqueous solution, and analyzing and calculating the data result of the viscosity A and the viscosity An to obtain a result.
The identification method of the hyaluronic acid skin-changing essence comprises the steps of preparing hyaluronic acid essence into 1% aqueous solution, adjusting the pH value of the aqueous solution to 7-9, preferably 8, testing the viscosity A of the aqueous solution to be 15mpa.s, dividing the aqueous solution into at least 2 parts, adding 0.5-3% of boron cross-linking agent, preferably 2%, into one part, uniformly stirring for 1 minute, testing the viscosity A1 of the solution to be 14, and adding 0.5-2% of zirconium into the other partThe cross-linking agent, preferably 2% after being stirred for 1 minute uniformly, has a viscosity a2 of 13, when the viscosity value satisfies any one of the following formulas,14≤16.5;13 is less than or equal to 21, and natural hyaluronic acid is judged because the data of the two parts do not satisfy any formula.
Further, when the solution is divided into at least 3 parts after the viscosity of the test solution is a, the test viscosity A3 is 14 after adding 3 to 20% of the aldehyde acid crosslinking agent to the third part solution, preferably after 4% of the aldehyde acid crosslinking agent is uniformly stirred, and the viscosity of the test solution is A3When the data is obtained, the natural hyaluronic acid is judged if 14 is less than or equal to 18.75;
further, when three solutions are used, one solution is added with 0.5 to 3% of boron crosslinking agent to measure A1, the other solution is added with 0.5 to 2% of zirconium crosslinking agent to measure A2, and after 3 to 20% of aldehyde acid crosslinking agent is added to the third solution, the viscosity A3 is measured, when the values of the viscosities A1, A2 and A3 satisfy any one of the following formulas,the hyaluronic acid is judged to be natural hyaluronic acid. The coefficients of the formula are obtained by comparison tests according to different experimental test process modes according to the crosslinking effect of the crosslinking group, and the operation modes of the data are as above.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (3)
1. The identification method of the hyaluronic acid skin-changing essence is characterized by comprising the steps of firstly, soaking the hyaluronic acid essence in an amphoteric solvent, dissolving and separating a dodecyl dimethyl allyl ammonium chloride coating and a hexadecyl dimethyl allyl ammonium chloride coating, and then washing with deionized water to remove the hyaluronic acid essence coated with the dodecyl dimethyl allyl ammonium chloride coating and the hexadecyl dimethyl allyl ammonium chloride coating; then centrifugally separating to obtain an amphoteric solvent solution, and then destroying and removing a gasoline film outside the hyaluronic acid essence in a stirring and heating mode; and finally, identifying the structure of the hyaluronic acid essence after treatment through a reagent combination test reaction test and analyzing and calculating a result.
2. The method according to claim 1, wherein the amphoteric solvent is a mixture of methanol, ethanol, water and 3 # white oil, the soaking method comprises the steps of firstly soaking the hyaluronic acid essence in the mixture of methanol, ethanol and 3 # white oil for several minutes at the temperature of 30-45 ℃, then filtering and separating, intermittently leaching for several times by using the mixture of methanol and ethanol until no foam is generated on the surface of the hyaluronic acid essence when the hyaluronic acid essence is washed by using a mixed solution of methanol and water, and then hot drying alcohol substances remained on the surface of the hyaluronic acid essence by using hot air; the deionized water washing comprises washing with deionized water at a temperature below 30 ℃ until liquid drops are hung on the surface of the hyaluronic acid essence; the centrifugal process adopts a centrifuge tube with a filter screen, the stirring and heating process comprises the steps of firstly placing the hyaluronic acid essence into a container for stirring, then blowing hot air with the temperature of more than 30 ℃ from bottom to top from the bottom of the container, and stirring under the heating of the air flow of the hot air until no obvious smell is generated, so as to obtain the treated hyaluronic acid essence; the medicament combination test comprises the steps of preparing the treated hyaluronic acid essence into 0.5-2% aqueous solution, adjusting the pH value of the aqueous solution, testing the viscosity A of the aqueous solution, dividing the aqueous solution into a plurality of parts, adding a cross-linking agent into each part to test the viscosity An of the aqueous solution, and analyzing and calculating the data result of the viscosity A and the viscosity An to obtain the result.
3. The method of claim 2, wherein the viscosity A of the aqueous solution is measured after the pH of the aqueous solution is adjusted to 7 to 9, and then the solution is divided into at least 2 parts, one part is added with 0.5 to 3% of the boron-based crosslinking agent and then the viscosity A1 is measured, and the other part is added with 0.5 to 2% of the zirconium-based crosslinking agent and then the viscosity A2 is measured, and when the viscosity value satisfies any one of the following formulas,the hyaluronic acid is judged to be non-natural hyaluronic acid. Further, when the solution was divided into at least 3 parts after the viscosity of the test solution was a, the viscosity of A3 was tested after adding 3 to 20% of the aldehyde-based acidic crosslinking agent to the third part of the solution, and when the viscosity of A3 was aIf so, judging the hyaluronic acid to be natural hyaluronic acid; when three solutions are available, 0.5 to 3 percent of boron crosslinking agent is added into one solution to measure the viscosity A1, 0.5 to 2 percent of zirconium crosslinking agent is added into the other solution to measure the viscosity A2, after 3 to 20 percent of aldehyde acid crosslinking agent is added into the third solution, the viscosity A3 is tested, when the values of the viscosities A1, A2 and A3 meet any one of the following formulas,the hyaluronic acid is judged to be natural hyaluronic acid.
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