CN112972337A

CN112972337A - Essence for improving skin moisture and delaying aging

Info

Publication number: CN112972337A
Application number: CN202110294538.8A
Authority: CN
Inventors: 曾启林
Original assignee: Individual
Current assignee: Individual
Priority date: 2021-03-19
Filing date: 2021-03-19
Publication date: 2021-06-18

Abstract

The invention discloses an essence for improving skin moisture and delaying senility, belonging to the technical field of skin care product preparation, and the essence for improving skin moisture and delaying senility comprises the following raw materials in parts by weight: 50-70 parts of deionized water, 5-8 parts of glycerol, 6-10 parts of propylene glycol, 3-5 parts of carbomer, 3-5 parts of triethanolamine, 1-3 parts of nicotinamide, 1-2 parts of vitamin E, 5-7 parts of a nutrient extract, 3-5 parts of an antioxidant component and 3-5 parts of an anti-aging and moisturizing component, wherein the nutrient extract is prepared by extracting various plants, the antioxidant component is prepared by using chitosan as a matrix and adding phenolic hydroxyl and carboxymethyl sulfate to further improve the antioxidant activity of the chitosan, the anti-aging performance of the essence is enhanced, the added anti-aging and moisturizing component can improve the moisturizing performance of skin and slow down the aging speed of skin cells, and the essence disclosed by the invention has the advantages of no toxicity, biodegradability, safety and reliability.

Description

Essence for improving skin moisture and delaying aging

Technical Field

The invention relates to the technical field of skin care product preparation, and particularly relates to essence for improving skin moisture and delaying aging.

Background

The essence is one of skin care products, has exquisite components, strong efficacy and obvious effect, contains active substances such as trace elements, collagen, serum and the like, and has the effects of preventing aging, resisting wrinkles, moisturizing, whitening, removing freckles and the like. The essence is divided into a water aqua and an oil aqua, the extracted essence is high in nutrient substance and concentrated, the skin-improving effect is achieved, the symptoms such as wrinkles and spots appear on the face in the process of continuous aging of cells along with the aging, meanwhile, the water loss and dry and oily skin are caused due to insufficient water storage capacity, and the antioxidation is an important aspect in the aging prevention process.

Disclosure of Invention

Technical problem to be solved

Aiming at the defects of the prior art, the invention provides essence for improving skin moisture and relieving aging, which is used for solving the problems that the skin moisture and the aging can cause wrinkles, spots and other symptoms on the face in the process of continuous aging along with the aging of cells, meanwhile, the water loss and the skin dryness and oil are caused due to insufficient water storage capacity, and the antioxidation is an important aspect in the aging prevention process.

(II) technical scheme

In order to achieve the purpose, the invention is realized by the following technical scheme: the essence for improving skin moisture and relieving aging comprises the following raw materials in parts by weight: 50-70 parts of deionized water, 5-8 parts of glycerol, 6-10 parts of propylene glycol, 3-5 parts of carbomer, 3-5 parts of triethanolamine, 1-3 parts of nicotinamide, 1-2 parts of vitamin E, 5-7 parts of a nutrient extracting solution, 3-5 parts of an antioxidant component and 3-5 parts of an anti-aging and moisturizing component;

the essence for improving skin moisture and relieving aging is prepared by the following steps:

step S1: adding the nutrient extracting solution, the antioxidant component and the anti-aging moisture-preserving component into a clean and dry stirring tank, stirring and mixing for 10-20min at the temperature of 30-40 ℃ and the rotating speed of 120-320r/min, placing the mixture into a high-temperature instantaneous sterilizer for sterilization treatment at the temperature of 150-165 ℃ after the mixing is finished, and filling and aseptically storing to obtain a component A;

step S2: adding deionized water, glycerol, propylene glycol and carbomer into a clean and dry stirring tank, stirring for 1-2h at the temperature of 75-80 ℃ and the rotation speed of 900-;

step S3: and (4) adding the component A obtained in the step S1 and the component B obtained in the step S2 into a clean and dry stirring tank, stirring for 2-3h at the temperature of 15-20 ℃ and the rotating speed of 150-250r/min, filtering, sterilizing and bottling after stirring, thus obtaining the essence for improving skin moisture and relieving aging.

Further, the nutrient extracting solution is prepared by the following steps:

step S11: weighing the following raw materials in parts by weight: 1-3 parts of white chrysanthemum, 1-3 parts of mirabilis jalapa, 1-2 parts of aloe leaves, 1-2 parts of rose hips, 0.5-1 part of tomatoes, 1-2 parts of pomegranate seeds, 1-2 parts of grape seeds and 20-30 parts of 75% ethanol solution by mass;

step S12: cleaning and draining the weighed raw materials, adding the raw materials into a pulverizer for pulverizing, adding the pulverized raw materials and 75% ethanol solution into a clean and dry stirring tank, heating and leaching for 4-5h at the temperature of 30-40 ℃ and the rotating speed of 100-200r/min, filtering after leaching, and then removing ethanol by rotary evaporation to obtain the nutrient extracting solution.

Further, the antioxidant ingredient is prepared by the following steps:

step S21: sequentially adding phthalic anhydride and 90 mass percent N, N-dimethylformamide solution into a clean and dried flask, stirring at the rotation speed of 200-;

step S22: sequentially adding deionized water and an ethanol solution with the mass fraction of 95% into a clean and dried flask, then adding the intermediate 1 obtained in the step S21, magnetically stirring for 100-:

step S23: adding dimethyl sulfide and acetone into a beaker, dropwise adding methyl iodide to react for 36-40h at the temperature of 20-30 ℃, and removing the acetone by rotary evaporation to obtain an intermediate 3; adding ionized water and the intermediate 2 obtained in the step S22 into a clean and dry flask, stirring for 10-14min at the temperature of 20-30 ℃ and the rotation speed of 400-600r/min, dropwise adding a mixture of the intermediate 3 and deionized water into the flask after stirring, reacting for 12-24h at the temperature of 25-35 ℃, adding acetone after the reaction is finished, standing for 30min, performing suction filtration, washing a filter cake for four times by using absolute ethyl alcohol, and freeze-drying for 18h at the temperature of 40 ℃ below zero to 30 ℃ below zero in a freeze-drying machine after washing to obtain an intermediate 4;

step S24: adding the intermediate 4 obtained in the step S23 into an ethanol solution of hydrazine hydrate, performing reflux reaction for 4-6h at the temperature of 90-100 ℃, cooling to room temperature, performing ice bath to 0 ℃, performing suction filtration, adding absolute ethanol into the filtrate, performing rotary evaporation, centrifuging, performing suction filtration, and freeze-drying in a freeze-dryer for 10-12h to obtain an intermediate 5;

step S25: adding 3, 4-dihydroxybenzoic acid and chloroform into a clean and dried flask, then dropwise adding phosphorus oxychloride into the flask at the temperature of 40-45 ℃, keeping the temperature at 45-55 ℃ after dropwise adding, reacting for 3-4h at constant temperature, and removing chloroform and unreacted phosphorus oxychloride by rotary evaporation after the reaction is finished to obtain an intermediate 6;

step S26: adding the intermediate 5 obtained in the step S25 and deionized water into a clean and dry flask, stirring for 20-25min at the temperature of 30-40 ℃ and the rotation speed of 200-300r/min, reducing the temperature to 0-5 ℃ after stirring, then dropwise adding the intermediate 6 mixed with toluene into the flask by using a dropping funnel, adjusting the temperature to 15-25 ℃ after dropwise adding, reacting for 24h, adding acetone into the flask after the reaction is finished, standing for 6-8h, then carrying out suction filtration on the reaction liquid, washing a filter cake for three times by using absolute ethyl alcohol, and freeze-drying the filter cake for 24h at the temperature of-40 ℃ to-30 ℃ in a freeze dryer to obtain the antioxidant component.

Further, in step S21, the phthalic anhydride, the 90% by mass N, N-dimethylformamide solution, and the chitosan are used in an amount ratio of 1 g: 10mL of: 0.2-0.4 g.

Further, in step S22, the deionized water, the 95% ethanol solution, the intermediate 1, the 40% sodium hydroxide solution, and the chloroacetic acid ethanol solution are used in a ratio of 4 mL: 1mL of: 1 g: 0.03 mol: 2mL, wherein the chloroacetic acid ethanol solution is prepared from chloroacetic acid and absolute ethyl alcohol according to the dosage ratio of 1 g: 1.2mL of the mixture.

Further, in step S23, the volume ratio of the dimethyl sulfide, acetone, and methyl iodide is 0.8: 30: 1, the dosage ratio of the deionized water, the intermediate 2 and the mixed solution of the intermediate 3 and the deionized water is 1 mL: 0.11 g:1mL, wherein the mixed solution of the intermediate 3 and the deionized water is prepared by mixing the intermediate 3 and the deionized water according to the dosage ratio of 0.2g to 1 mL.

Further, the ratio of the intermediate 4 and the ethanol solution of hydrazine hydrate used in step S24 is 1 g: 50mL, wherein the ethanol solution of hydrazine hydrate is a hydrazine hydrate solution with the mass fraction of 50% and absolute ethanol according to the volume ratio of 1: 1 are mixed to obtain the product.

Further, in step S25, the usage ratio of the 3, 4-dihydroxybenzoic acid, chloroform and phosphorus oxychloride is 1 g: 10mL of: 0.35 g; step S26 the amount ratio of intermediate 5, deionized water, and intermediate 6 mixed with toluene was 10 mg: 1mL of: 0.02mL, intermediate 6 mixed with toluene in a toluene to intermediate 6 ratio of 1 g: 10mL of the mixture was mixed.

Further, the anti-aging moisturizing component is prepared from collagen, hyaluronic acid, dipeptide and acetylated hexapeptide in a mass ratio of 1: 1: 2: 1 are mixed.

(III) advantageous effects

The invention provides essence for improving skin moisture and delaying aging. Compared with the prior art, the method has the following beneficial effects: the adopted plants contain various antibacterial, antioxidant and anti-aging active ingredients, and the addition of the nutrient extract into the essence not only can improve the fragrance of the essence, but also can enrich the active ingredients with various natural sources;

preparing an antioxidant component, using chitosan as a matrix, firstly utilizing phthalic anhydride to react with amino in chitosan molecules to protect the amino, then activating hydroxyl of which the molecular has the value of C6 to react with chloroacetic acid to produce modified chitosan with carboxymethyl, on the basis, using dimethyl sulfide to carry out alkylation reaction with methyl iodide to prepare sulfate, combining sulfate cations with carboxymethyl anions on the modified chitosan under the action of ion exchange to obtain the modified chitosan with carboxymethyl sulfate, then using a mixed solution of hydrazine hydrate and ethanol to carry out deamination protection on the obtained intermediate to obtain the modified chitosan with carboxymethyl sulfate and amino activity, then modifying the amino part of the modified chitosan, using 3, 4-dihydroxy benzoic acid to react with phosphorus oxychloride in chloroform to generate acyl chloride, reacting with amino of the modified chitosan with the amino exposed again, and combining 3, 4-dihydroxy benzoic acid with two phenolic hydroxyl groups into a chitosan molecule to finally obtain the modified chitosan with the phenolic hydroxyl groups and the carboxymethyl sulfate activity; wherein the chitosan is a polymer formed by connecting N-acetyl-2-amino-2-deoxy-D-glucose through a beta-1, 4-glycosidic bond, is natural in source, has a large amount of active groups such as amino, hydroxyl and the like in a molecular skeleton, has positive charges and higher molecular weight, can be used as a selective permeation barrier to form a protective layer which stays for a long time around the skin to form a moisturizing film, and has good activities of antioxidation, antibiosis and the like, wherein the methyl sulfide is an endogenous antioxidant substance contained in animal tissues, has the same thiomethyl structure as methionine, can inhibit the oxidation of protein amino acid residues in vivo, and simultaneously has the effects of improving the accumulation of ROS and superoxide and the generation of free radicals, the antioxidant has the functions of reducing the generation of lipid peroxides, reducing oxidative stress injury, improving the cell survival rate, prolonging the cell life and the like, and is an excellent antioxidant substance; the 3, 4-dihydroxy benzoic acid is also called protocatechuic acid, which enables a natural substance existing in plants such as leaves of Stenoloma chusanum (Chin) Chin of Lepidiaceae and leaves of ilex chinensis of Aquifoliaceae to have two phenolic hydroxyl groups, and in the antioxidation effect, the O-H bond of the phenolic hydroxyl group can be directly broken to give a hydrogen atom which is combined with a free radical molecule to achieve the effect of removing free radicals, and simultaneously, the phenolic hydroxyl group can also be reacted with ethanol to cause the regeneration effect of the phenolic hydroxyl group after the effect is exerted; the anti-oxidation component modifies chitosan with good anti-oxidation activity, and the added group with good anti-oxidation activity enables the chitosan to have better anti-oxidation capability, enhances the anti-aging performance of essence, further relieves the aging of skin cells, and simultaneously is also added with an anti-aging and moisturizing component which has functional active substances of collagen, hyaluronic acid, dipeptide and acetylated hexapeptide, wherein the hyaluronic acid has good moisturizing effect, the collagen and the acetylated hexapeptide have anti-aging activity, the dipeptide can promote the generation of the hyaluronic acid and the collagen, further improves the moisturizing performance of skin and slows down the aging speed of skin cells; most of the additives are natural materials, have non-toxicity and biodegradable performance, and have no adverse side effect while effectively improving the skin.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Example 1

The essence for improving skin moisture and relieving aging comprises the following raw materials in parts by weight: 50 parts of deionized water, 5 parts of glycerol, 6 parts of propylene glycol, 3 parts of carbomer, 3 parts of triethanolamine, 1 part of nicotinamide, 1 parts of vitamin E, 5 parts of a nutrient extracting solution, 3 parts of an antioxidant component and 3 parts of an anti-aging moisture-preserving component;

step S1: adding the nutritional extract, antioxidant component and antiaging moisture keeping component into a clean and dry stirring tank, stirring and mixing at 30 deg.C and 120r/min for 10min, sterilizing in a high temperature instant sterilizer at 150 deg.C, bottling, and storing under sterile condition to obtain component A;

step S2: adding deionized water, glycerol, propylene glycol and carbomer into a clean and dry stirring tank, stirring for 1h at 75 ℃ and at the rotating speed of 900r/min, adding a vacuum emulsifying machine after stirring is finished, emulsifying for 1h to obtain an emulsion, adding the emulsion, triethanolamine, nicotinamide and biotin E into the clean and dry stirring tank, stirring for 20min at the temperature of 40 ℃ and the rotating speed of 500r/min, and filling and storing aseptically after high-temperature instantaneous sterilization to obtain a component B;

step S3: and (4) adding the component A obtained in the step S1 and the component B obtained in the step S2 into a clean and dry stirring tank, stirring for 2 hours at the temperature of 15 ℃ and the rotating speed of 150r/min, filtering, sterilizing and bottling after stirring, thus obtaining the essence for improving skin moisture and relieving aging.

The nutrient extracting solution is prepared by the following steps:

step S11: weighing the following raw materials in parts by weight: 1 part of white chrysanthemum, 1 part of mirabilis jalapa flower, 1 part of aloe leaf, 1 part of rose hip, 0.5 part of tomato, 1 part of pomegranate seed, 1 part of grape seed and 20 parts of ethanol solution with the mass fraction of 75%;

step S12: cleaning and draining the weighed raw materials, adding the raw materials into a pulverizer for pulverizing, adding the pulverized raw materials and 75% ethanol solution into a clean and dry stirring tank, heating and leaching for 4 hours at the temperature of 30 ℃ and the rotating speed of 100r/min, filtering after leaching, and then removing ethanol by rotary evaporation to obtain the nutrient extracting solution.

The antioxidant component is prepared by the following steps:

step S21: sequentially adding phthalic anhydride and 90% by mass of N, N-dimethylformamide solution into a clean and dry flask, stirring at the rotation speed of 200r/min until the phthalic anhydride is completely dissolved, introducing nitrogen for protection, then adding chitosan into the flask, reacting for 9 hours at the temperature of 130 ℃ in an oil bath, cooling to room temperature after the reaction is finished, pouring into deionized water at the temperature of 0 ℃, then placing the deionized water in a high-speed refrigerated centrifuge, centrifuging for 8 minutes at the rotation speed of 3000r/min, collecting precipitates, washing with the deionized water and absolute ethyl alcohol for three times respectively, performing suction filtration, placing filter cakes in a freeze dryer at the temperature of minus 40-10 hours, and obtaining an intermediate 1;

step S22: sequentially adding deionized water and an ethanol solution with the mass fraction of 95% into a clean and dry flask, then adding the intermediate 1 obtained in the step S21, magnetically stirring for 100r/min, stirring and dispersing for 10min, then dropwise adding a sodium hydroxide solution with the mass fraction of 40% into the flask by using a dropping funnel, preserving heat for 1h at the temperature of 50 ℃ after the dropwise adding is finished, then adding a chloroacetic acid ethanol solution into the flask by using the dropping funnel, continuously reacting at the constant temperature of 50 ℃ for 5h after the dropwise adding is finished, washing three times by using absolute ethyl alcohol after the reaction is finished and cooled to room temperature, and freeze-drying for 12h at the temperature of 40 ℃ below zero by using a freeze-drying machine to obtain an intermediate 2:

step S23: adding dimethyl sulfide and acetone into a beaker, dropwise adding methyl iodide to react for 36 hours at the temperature of 20 ℃, and removing the acetone by rotary evaporation to obtain an intermediate 3; adding ionized water and the intermediate 2 obtained in the step S22 into a clean and dry flask, stirring for 10min at the temperature of 20 ℃ and the rotating speed of 400r/min, dropwise adding a mixture of the intermediate 3 and the deionized water into the flask after stirring, reacting for 12h at the temperature of 25 ℃, adding acetone after the reaction is finished, standing for 30min, performing suction filtration, washing a filter cake for four times by using absolute ethyl alcohol, and freeze-drying the filter cake for 18h at the temperature of 40 ℃ below zero in a freeze-drying machine after washing to obtain an intermediate 4;

step S24: adding the intermediate 4 obtained in the step S23 into an ethanol solution of hydrazine hydrate, performing reflux reaction for 4 hours at the temperature of 90 ℃, cooling to room temperature, performing ice bath to 0 ℃, performing suction filtration, adding absolute ethyl alcohol into the filtrate, performing rotary evaporation, centrifuging, performing suction filtration, and freeze-drying in a freeze dryer for 10 hours to obtain an intermediate 5;

step S25: adding 3, 4-dihydroxybenzoic acid and chloroform into a clean and dried flask, then dropwise adding phosphorus oxychloride into the flask at the temperature of 40 ℃, keeping the temperature at 45 ℃ after dropwise adding, reacting for 3 hours at constant temperature, and removing the chloroform and unreacted phosphorus oxychloride by rotary evaporation after the reaction is finished to obtain an intermediate 6;

step S26: adding the intermediate 5 obtained in the step S25 and deionized water into a clean and dry flask, stirring for 20min at the temperature of 30 ℃ and the rotation speed of 200r/min, cooling to 0 ℃ after stirring, then dropwise adding the intermediate 6 mixed with toluene into the flask by using a dropping funnel, adjusting the temperature to 15 ℃ after dropwise adding, reacting for 24h, adding acetone into the flask after the reaction is finished, standing for 6h, then carrying out suction filtration on the reaction solution, washing a filter cake for three times by using absolute ethyl alcohol, and freeze-drying the filter cake for 24h at the temperature of-40 ℃ in a freeze dryer to obtain the antioxidant component.

Wherein the dosage ratio of the phthalic anhydride, the N, N-dimethylformamide solution with the mass fraction of 90% and the chitosan in the step S21 is 1 g: 10mL of: 0.2 g; step S22, the use ratio of the deionized water, the ethanol solution with the mass fraction of 95%, the intermediate 1, the sodium hydroxide solution with the mass fraction of 40% and the chloroacetic acid ethanol solution is 4 mL: 1mL of: 1 g: 0.03 mol: 2mL, wherein the chloroacetic acid ethanol solution is prepared from chloroacetic acid and absolute ethyl alcohol according to the dosage ratio of 1 g: 1.2mL of the mixture; the volume ratio of the dosage of the dimethyl sulfide, the acetone and the methyl iodide in the step S23 is 0.8: 30: 1, the dosage ratio of the deionized water, the intermediate 2 and the mixed solution of the intermediate 3 and the deionized water is 1 mL: 0.11 g:1mL, wherein the mixed solution of the intermediate 3 and the deionized water is formed by mixing the intermediate 3 and the deionized water according to the dosage ratio of 0.2g to 1 mL; the dosage ratio of the intermediate 4 and the hydrazine hydrate ethanol solution in the step S24 is 1 g: 50mL, wherein the ethanol solution of hydrazine hydrate is a hydrazine hydrate solution with the mass fraction of 50% and absolute ethanol according to the volume ratio of 1: 1, mixing the raw materials; the dosage ratio of the 3, 4-dihydroxybenzoic acid, the chloroform and the phosphorus oxychloride in the step S25 is 1 g: 10mL of: 0.35 g; step S26 the amount ratio of intermediate 5, deionized water, and intermediate 6 mixed with toluene was 10 mg: 1mL of: 0.02mL, intermediate 6 mixed with toluene in a toluene to intermediate 6 ratio of 1 g: 10mL of the mixture was mixed.

The anti-aging moisturizing component is prepared from collagen, hyaluronic acid, dipeptide and acetylated hexapeptide in a mass ratio of 1: 1: 2: 1 are mixed to form

Example 2

The essence for improving skin moisture and relieving aging comprises the following raw materials in parts by weight: 60 parts of deionized water, 6.5 parts of glycerol, 8 parts of propylene glycol, 4 parts of carbomer, 4 parts of triethanolamine, 2 parts of nicotinamide, 1.5 parts of vitamin E, 6 parts of a nutrient extracting solution, 4 parts of an antioxidant component and 4 parts of an anti-aging moisture-preserving component;

step S1: adding the nutritional extract, antioxidant component and antiaging moisture keeping component into a clean and dry stirring tank, stirring and mixing at 35 deg.C and 220r/min for 15min, sterilizing in a high temperature instant sterilizer at 160 deg.C, bottling, and storing under sterile condition to obtain component A;

step S2: adding deionized water, glycerol, propylene glycol and carbomer into a clean and dry stirring tank, stirring for 1.5h at the temperature of 77.5 ℃ and the rotation speed of 950r/min, adding a vacuum emulsifying machine after stirring is finished, emulsifying for 1.5h to obtain an emulsion, adding the emulsion, triethanolamine, nicotinamide and biotin E into the clean and dry stirring tank, stirring for 25min at the temperature of 45 ℃ and the rotation speed of 600r/min, and performing high-temperature instantaneous sterilization, filling and aseptic storage to obtain a component B;

step S3: and (4) adding the component A obtained in the step S1 and the component B obtained in the step S2 into a clean and dry stirring tank, stirring for 2.5 hours at the temperature of 17.5 ℃ and the rotating speed of 200r/min, filtering, sterilizing and bottling after stirring, thus obtaining the essence for improving skin moisture and relieving aging.

The nutrient extracting solution is prepared by the following steps:

step S11: weighing the following raw materials in parts by weight: 2 parts of white chrysanthemum, 2 parts of mirabilis jalapa, 1.5 parts of aloe leaves, 1.5 parts of rose hips, 0.75 part of tomatoes, 1.5 parts of pomegranate seeds, 1.5 parts of grape seeds and 25 parts of ethanol solution with the mass fraction of 75%;

step S12: cleaning and draining the weighed raw materials, adding the raw materials into a pulverizer for pulverizing, adding the pulverized raw materials and 75% by mass of ethanol solution into a clean and dry stirring tank, heating and leaching for 4.5 hours at the temperature of 35 ℃ and the rotating speed of 150r/min, filtering after leaching, and performing rotary evaporation to remove ethanol to obtain the nutrient extracting solution.

The antioxidant component is prepared by the following steps:

step S21: sequentially adding phthalic anhydride and 90% by mass of N, N-dimethylformamide solution into a clean and dried flask, stirring at the rotation speed of 250r/min until the phthalic anhydride is completely dissolved, introducing nitrogen for protection, then adding chitosan into the flask, reacting for 9.5 hours at the temperature of 132.5 ℃ in an oil bath, cooling to room temperature after the reaction is finished, pouring into deionized water with the temperature of 0 ℃, then placing the deionized water into a high-speed freezing centrifuge, centrifuging for 9 minutes at the rotation speed of 3500r/min, collecting precipitates, washing with the deionized water and absolute ethyl alcohol for three times respectively, performing suction filtration, placing a filter cake into a freeze dryer, and freeze-drying for 11 hours at the temperature of 35 ℃ below zero to obtain an intermediate 1;

step S22: sequentially adding deionized water and an ethanol solution with the mass fraction of 95% into a clean and dry flask, then adding the intermediate 1 obtained in the step S21, magnetically stirring for 140r/min, stirring and dispersing for 12.5min, then dropwise adding a sodium hydroxide solution with the mass fraction of 40% into the flask by using a dropping funnel, preserving the temperature at 55 ℃ for 1.5h after the dropwise addition is finished, then adding a chloroacetic acid ethanol solution into the flask by using the dropping funnel, continuing to react at the constant temperature of 55 ℃ for 5.5h after the dropwise addition is finished, washing the mixture for three times by using absolute ethanol after the reaction is finished and cooled to room temperature, and freeze-drying the mixture for 14h at the temperature of 35 ℃ below zero by using a freeze dryer to obtain an intermediate 2:

step S23: adding dimethyl sulfide and acetone into a beaker, dropwise adding methyl iodide to react for 38 hours at the temperature of 25 ℃, and removing the acetone by rotary evaporation to obtain an intermediate 3; adding ionized water and the intermediate 2 obtained in the step S22 into a clean and dry flask, stirring for 12min at the temperature of 25 ℃ and the rotation speed of 500r/min, dropwise adding a mixture of the intermediate 3 and the deionized water into the flask after stirring, reacting for 18h at the temperature of 30 ℃, adding acetone after the reaction is finished, standing for 30min, performing suction filtration, washing a filter cake for four times by using absolute ethyl alcohol, and freeze-drying the filter cake for 18h at the temperature of 35 ℃ below zero in a freeze-drying machine after washing to obtain an intermediate 4;

step S24: adding the intermediate 4 obtained in the step S23 into an ethanol solution of hydrazine hydrate, performing reflux reaction for 5 hours at the temperature of 95 ℃, cooling to room temperature, performing ice bath to 0 ℃, performing suction filtration, adding absolute ethanol into the filtrate, performing rotary evaporation, centrifuging, performing suction filtration, and freeze-drying for 11 hours in a freeze-dryer to obtain an intermediate 5;

step S25: adding 3, 4-dihydroxybenzoic acid and chloroform into a clean and dried flask, then dropwise adding phosphorus oxychloride into the flask at the temperature of 42.5 ℃, keeping the temperature at 50 ℃ after dropwise adding, reacting for 3.5 hours at constant temperature, and performing rotary evaporation to remove chloroform and unreacted phosphorus oxychloride after the reaction is finished to obtain an intermediate 6;

step S26: adding the intermediate 5 obtained in the step S25 and deionized water into a clean and dry flask, stirring for 22.5min at the temperature of 35 ℃ and the rotation speed of 250r/min, reducing the temperature to 2.5 ℃ after stirring, then dropwise adding the intermediate 6 mixed with toluene into the flask by using a dropping funnel, adjusting the temperature to 20 ℃ after dropwise adding, reacting for 24h, adding acetone into the flask after the reaction is finished, standing for 7h, then carrying out suction filtration on the reaction solution, washing a filter cake for three times by using absolute ethyl alcohol, and freeze-drying the filter cake for 24h at the temperature of 35 ℃ below zero by using a freeze dryer to obtain the antioxidant component.

Wherein the dosage ratio of the phthalic anhydride, the N, N-dimethylformamide solution with the mass fraction of 90% and the chitosan in the step S21 is 1 g: 10mL of: 0.3 g; step S22, the use ratio of the deionized water, the ethanol solution with the mass fraction of 95%, the intermediate 1, the sodium hydroxide solution with the mass fraction of 40% and the chloroacetic acid ethanol solution is 4 mL: 1mL of: 1 g: 0.03 mol: 2mL, wherein the chloroacetic acid ethanol solution is prepared from chloroacetic acid and absolute ethyl alcohol according to the dosage ratio of 1 g: 1.2mL of the mixture; the volume ratio of the dosage of the dimethyl sulfide, the acetone and the methyl iodide in the step S23 is 0.8: 30: 1, the dosage ratio of the deionized water, the intermediate 2 and the mixed solution of the intermediate 3 and the deionized water is 1 mL: 0.11 g:1mL, wherein the mixed solution of the intermediate 3 and the deionized water is formed by mixing the intermediate 3 and the deionized water according to the dosage ratio of 0.2g to 1 mL; the dosage ratio of the intermediate 4 and the hydrazine hydrate ethanol solution in the step S24 is 1 g: 50mL, wherein the ethanol solution of hydrazine hydrate is a hydrazine hydrate solution with the mass fraction of 50% and absolute ethanol according to the volume ratio of 1: 1, mixing the raw materials; the dosage ratio of the 3, 4-dihydroxybenzoic acid, the chloroform and the phosphorus oxychloride in the step S25 is 1 g: 10mL of: 0.35 g; step S26 the amount ratio of intermediate 5, deionized water, and intermediate 6 mixed with toluene was 10 mg: 1mL of: 0.02mL, intermediate 6 mixed with toluene in a toluene to intermediate 6 ratio of 1 g: 10mL of the mixture was mixed.

Example 3

The essence for improving skin moisture and relieving aging comprises the following raw materials in parts by weight: 70 parts of deionized water, 8 parts of glycerol, 10 parts of propylene glycol, 5 parts of carbomer, 5 parts of triethanolamine, 3 parts of nicotinamide, 2 parts of vitamin E, 7 parts of a nutrient extracting solution, 5 parts of an antioxidant component and 5 parts of an anti-aging and moisturizing component;

step S1: adding the nutritional extract, antioxidant component and antiaging moisture keeping component into a clean and dry stirring tank, stirring and mixing at 40 deg.C and 320r/min for 20min, sterilizing in a high temperature instant sterilizer at 165 deg.C, bottling, and storing under sterile condition to obtain component A;

step S2: adding deionized water, glycerol, propylene glycol and carbomer into a clean and dry stirring tank, stirring for 2h at the temperature of 80 ℃ and the rotating speed of 1000r/min, adding into a vacuum emulsifying machine after stirring is finished, emulsifying for 2h to obtain an emulsion, then adding the emulsion, triethanolamine, nicotinamide and biotin E into the clean and dry stirring tank, stirring for 30min at the temperature of 50 ℃ and the rotating speed of 700r/min, and carrying out high-temperature instantaneous sterilization, filling and aseptic storage to obtain a component B;

step S3: and (4) adding the component A obtained in the step S1 and the component B obtained in the step S2 into a clean and dry stirring tank, stirring for 3 hours at the temperature of 20 ℃ and the rotating speed of 250r/min, filtering, sterilizing and bottling after stirring, thus obtaining the essence for improving skin moisture and relieving aging.

The nutrient extracting solution is prepared by the following steps:

step S11: weighing the following raw materials in parts by weight: 3 parts of white chrysanthemum, 3 parts of mirabilis jalapa flower, 2 parts of aloe leaf, 2 parts of rose hip, 1 part of tomato, 2 parts of pomegranate seed, 2 parts of grape seed and 30 parts of ethanol solution with the mass fraction of 75%;

step S12: cleaning and draining the weighed raw materials, adding the raw materials into a pulverizer for pulverizing, adding the pulverized raw materials and 75% ethanol solution into a clean and dry stirring tank, heating and leaching for 5 hours at the temperature of 40 ℃ and the rotating speed of 200r/min, filtering after leaching, and then removing ethanol by rotary evaporation to obtain the nutrient extracting solution.

The antioxidant component is prepared by the following steps:

step S21: sequentially adding phthalic anhydride and 90% by mass of N, N-dimethylformamide solution into a clean and dried flask, stirring at the rotation speed of 300r/min until the phthalic anhydride is completely dissolved, introducing nitrogen for protection, then adding chitosan into the flask, reacting for 10 hours at the temperature of 135 ℃ in an oil bath, cooling to room temperature after the reaction is finished, pouring into deionized water at the temperature of 0 ℃, then placing the deionized water in a high-speed freezing centrifuge, centrifuging for 10 minutes at the rotation speed of 4000r/min, collecting precipitates, washing the precipitates for three times respectively by using the deionized water and absolute ethyl alcohol, carrying out suction filtration, placing filter cakes in a freeze dryer, and freeze-drying for 12 hours at the temperature of-30 ℃ to obtain an intermediate 1;

step S22: sequentially adding deionized water and an ethanol solution with the mass fraction of 95% into a clean and dry flask, then adding the intermediate 1 obtained in the step S21, magnetically stirring for 180r/min, stirring and dispersing for 15min, then dropwise adding a sodium hydroxide solution with the mass fraction of 40% into the flask by using a dropping funnel, preserving heat for 2h at the temperature of 60 ℃ after the dropwise adding is finished, then adding a chloroacetic acid ethanol solution into the flask by using the dropping funnel, continuously reacting at the constant temperature of 60 ℃ for 6h after the dropwise adding is finished, washing three times by using absolute ethyl alcohol after the reaction is finished and cooled to room temperature, and freeze-drying for 16h at the temperature of-30 ℃ by using a freeze-drying machine to obtain an intermediate 2:

step S23: adding dimethyl sulfide and acetone into a beaker, dropwise adding methyl iodide to react for 40h at the temperature of 30 ℃, and removing the acetone by rotary evaporation to obtain an intermediate 3; adding ionized water and the intermediate 2 obtained in the step S22 into a clean and dry flask, stirring for 14min at the temperature of 30 ℃ and the rotation speed of 600r/min, dropwise adding a mixture of the intermediate 3 and the deionized water into the flask after stirring, reacting for 24h at the temperature of 35 ℃, adding acetone after the reaction is finished, standing for 30min, performing suction filtration, washing a filter cake for four times by using absolute ethyl alcohol, and freeze-drying the filter cake for 18h at the temperature of-30 ℃ in a freeze-drying machine after washing to obtain an intermediate 4;

step S24: adding the intermediate 4 obtained in the step S23 into an ethanol solution of hydrazine hydrate, performing reflux reaction for 6 hours at the temperature of 100 ℃, cooling to room temperature, performing ice bath to 0 ℃, performing suction filtration, adding absolute ethanol into the filtrate, performing rotary evaporation, centrifuging, performing suction filtration, and freeze-drying in a freeze-dryer for 12 hours to obtain an intermediate 5;

step S25: adding 3, 4-dihydroxybenzoic acid and chloroform into a clean and dried flask, then dropwise adding phosphorus oxychloride into the flask at the temperature of 45 ℃, keeping the temperature at 55 ℃ after dropwise adding, reacting for 4 hours at constant temperature, and removing the chloroform and the unreacted phosphorus oxychloride by rotary evaporation after the reaction is finished to obtain an intermediate 6;

step S26: adding the intermediate 5 obtained in the step S25 and deionized water into a clean and dry flask, stirring for 25min at the temperature of 40 ℃ and the rotation speed of 300r/min, cooling to 5 ℃ after stirring, then dropwise adding the intermediate 6 mixed with toluene into the flask by using a dropping funnel, adjusting the temperature to 25 ℃ after dropwise adding, reacting for 24h, adding acetone after the reaction is finished, standing for 8h, then carrying out suction filtration on the reaction liquid, washing a filter cake for three times by using absolute ethyl alcohol, and freeze-drying the filter cake for 24h at the temperature of-30 ℃ in a freeze dryer to obtain the antioxidant component.

Wherein the dosage ratio of the phthalic anhydride, the N, N-dimethylformamide solution with the mass fraction of 90% and the chitosan in the step S21 is 1 g: 10mL of: 0.4 g; step S22, the use ratio of the deionized water, the ethanol solution with the mass fraction of 95%, the intermediate 1, the sodium hydroxide solution with the mass fraction of 40% and the chloroacetic acid ethanol solution is 4 mL: 1mL of: 1 g: 0.03 mol: 2mL, wherein the chloroacetic acid ethanol solution is prepared from chloroacetic acid and absolute ethyl alcohol according to the dosage ratio of 1 g: 1.2mL of the mixture; the volume ratio of the dosage of the dimethyl sulfide, the acetone and the methyl iodide in the step S23 is 0.8: 30: 1, the dosage ratio of the deionized water, the intermediate 2 and the mixed solution of the intermediate 3 and the deionized water is 1 mL: 0.11 g:1mL, wherein the mixed solution of the intermediate 3 and the deionized water is formed by mixing the intermediate 3 and the deionized water according to the dosage ratio of 0.2g to 1 mL; the dosage ratio of the intermediate 4 and the hydrazine hydrate ethanol solution in the step S24 is 1 g: 50mL, wherein the ethanol solution of hydrazine hydrate is a hydrazine hydrate solution with the mass fraction of 50% and absolute ethanol according to the volume ratio of 1: 1, mixing the raw materials; the dosage ratio of the 3, 4-dihydroxybenzoic acid, the chloroform and the phosphorus oxychloride in the step S25 is 1 g: 10mL of: 0.35 g; step S26 the amount ratio of intermediate 5, deionized water, and intermediate 6 mixed with toluene was 10 mg: 1mL of: 0.02mL, intermediate 6 mixed with toluene in a toluene to intermediate 6 ratio of 1 g: 10mL of the mixture was mixed.

The anti-aging moisturizing component is prepared from collagen, hyaluronic acid, dipeptide and acetylated hexapeptide in a mass ratio of 1: 1: 2: 1 are mixed.

Comparative example: an anti-aging moisturizing essence sold on the market.

The essence liquids of examples 1 to 3 and comparative example were tested, 80 volunteers were randomly selected, and the essence liquids of examples 1 to 3 and comparative example were used in 4 groups, and skin improvement was observed for 7 days, 14 days, and 30 days, and the results of use effect evaluation were shown in the following table

It can be seen from the above table that the use of the essences of examples 1 to 3 has a significant improvement effect on the skin compared to the essence of comparative example.

It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.

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

1. The essence for improving skin moisture and delaying aging is characterized in that: the feed comprises the following raw materials in parts by weight: 50-70 parts of deionized water, 5-8 parts of glycerol, 6-10 parts of propylene glycol, 3-5 parts of carbomer, 3-5 parts of triethanolamine, 1-3 parts of nicotinamide, 1-2 parts of vitamin E, 5-7 parts of a nutrient extracting solution, 3-5 parts of an antioxidant component and 3-5 parts of an anti-aging and moisturizing component;

the antioxidant component is prepared by the following steps:

step S21: adding phthalic anhydride and N, N-dimethylformamide solution into a flask, stirring until the phthalic anhydride is completely dissolved, introducing nitrogen for protection, then adding chitosan for reaction, cooling to room temperature after the reaction is finished, pouring into deionized water with the temperature of 0 ℃, centrifuging, collecting precipitate, washing with deionized water and absolute ethyl alcohol, performing suction filtration, and freeze-drying a filter cake to obtain an intermediate 1;

step S22: adding deionized water and an ethanol solution into a flask, then adding the intermediate 1, dropwise adding a sodium hydroxide solution into the flask after stirring, keeping the temperature for 1-2h, adding a chloroacetic acid ethanol solution for carrying out a constant-temperature reaction, cooling to room temperature after the reaction is finished, washing with absolute ethanol, and freeze-drying to obtain an intermediate 2:

step S23: adding dimethyl sulfide and acetone into a beaker, dropwise adding methyl iodide for reaction, and removing acetone by rotary evaporation to obtain an intermediate 3; adding ionized water and an intermediate 2 into a flask, dropwise adding a mixture of the intermediate 3 and the deionized water into the flask after stirring for reaction, adding the mixture into acetone after the reaction is finished, standing, performing suction filtration, washing a filter cake, and freeze-drying after the washing is finished to obtain an intermediate 4;

step S24: adding the intermediate 4 into an ethanol solution of hydrazine hydrate for reflux reaction, cooling to room temperature after the reaction is finished, carrying out ice bath, adding absolute ethanol into filtrate after suction filtration, centrifuging after rotary evaporation, carrying out suction filtration, and freeze-drying to obtain an intermediate 5;

step S25: adding 3, 4-dihydroxybenzoic acid and chloroform into a flask, then dropwise adding phosphorus oxychloride, reacting at constant temperature after dropwise adding, and performing rotary evaporation after the reaction is finished to obtain an intermediate 6;

step S26: adding the intermediate 5 and deionized water into a flask, stirring, cooling, adding the intermediate 6 mixed with toluene dropwise, adding acetone after the reaction is finished, standing, performing suction filtration, washing a filter cake, and freeze-drying to obtain the antioxidant component.

2. The essence for improving skin moisture and relieving aging as claimed in claim 1, wherein: the dosage ratio of the phthalic anhydride, the N, N-dimethylformamide solution and the chitosan in the step S21 is 1 g: 10mL of: 0.2-0.4 g.

3. The essence for improving skin moisture and relieving aging as claimed in claim 1, wherein: step S22, the use ratio of the deionized water, the ethanol solution with the mass fraction of 95%, the intermediate 1, the sodium hydroxide solution with the mass fraction of 40% and the chloroacetic acid ethanol solution is 4 mL: 1mL of: 1 g: 0.03 mol: 2mL, wherein the chloroacetic acid ethanol solution is prepared from chloroacetic acid and absolute ethyl alcohol according to the dosage ratio of 1 g: 1.2mL of the mixture.

4. The essence for improving skin moisture and relieving aging as claimed in claim 1, wherein: the volume ratio of the dosage of the dimethyl sulfide, the acetone and the methyl iodide in the step S23 is 0.8: 30: 1, the dosage ratio of the deionized water, the intermediate 2 and the mixed solution of the intermediate 3 and the deionized water is 1 mL: 0.11 g:1mL, wherein the mixed solution of the intermediate 3 and the deionized water is prepared by mixing the intermediate 3 and the deionized water according to the dosage ratio of 0.2g to 1 mL.

5. The essence for improving skin moisture and relieving aging as claimed in claim 1, wherein: the dosage ratio of the intermediate 4 and the hydrazine hydrate ethanol solution in the step S24 is 1 g: 50mL, wherein the ethanol solution of hydrazine hydrate is a hydrazine hydrate solution with the mass fraction of 50% and absolute ethanol according to the volume ratio of 1: 1 are mixed to obtain the product.

6. The essence for improving skin moisture and relieving aging as claimed in claim 1, wherein: the dosage ratio of the 3, 4-dihydroxybenzoic acid, the chloroform and the phosphorus oxychloride in the step S25 is 1 g: 10mL of: 0.35 g; step S26 the amount ratio of intermediate 5, deionized water, and intermediate 6 mixed with toluene was 10 mg: 1mL of: 0.02mL, intermediate 6 mixed with toluene in a toluene to intermediate 6 ratio of 1 g: 10mL of the mixture was mixed.