Wrinkle-fading eye cream containing ascorbyl glucoside and preparation method of wrinkle-fading eye cream

Abstract

The invention belongs to the technical field of cosmetics, and particularly discloses a wrinkle-fading eye cream containing ascorbyl glucoside and a preparation method of the wrinkle-fading eye cream. The wrinkle fading eye cream is prepared from the following raw material components: a component A, a component B, a component C, a component D and water, wherein the component A comprises a first emulsifier, an emollient, a first thickener and a first antioxidant; the component B comprises a first humectant, a second thickener, a chelating agent and a second emulsifier; the component C comprises a second antioxidant and a second humectant; the component D is prepared from ascorbyl glucoside and acetylated sodium hyaluronate. The wrinkle-fading eye cream provided by the invention not only can improve the stability of ascorbic acid glucoside, but also can obtain a good eye skin care effect through effective compounding of the raw materials.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of cosmetics, in particular to an ascorbyl glucoside-containing fine line eye cream and a preparation method thereof. BACKGROUND

[0002] The skin around the eyes is the thinnest part of the human body and is the most frequently moving part. The skin around the eyes has no sebaceous glands and sweat glands and cannot secrete sebum that can moisturize the skin and prevent water evaporation. In addition, with age, excessive exposure to ultraviolet rays and some bad eye habits, the epidermal tissue of the skin around the eyes will become dry and thin, collagen and elastin will gradually be lost, and metabolism will slow down, which will cause the skin to easily form fine lines, crow's feet, dark circles and bags, and once the related lines appear, they are difficult to eliminate. In order to delay the aging of the skin around the eyes and improve the skin tightness and fine lines, in addition to ensuring adequate sleep, paying attention to sun protection, developing good habits and eye habits, it is more important to do a good job of facial moisturizing and the selection and use of external skin care products.

[0003] Ascorbyl glucoside (AA-2G) is one of the derivatives of vitamin C, which can be converted into vitamin C into skin cells to promote collagen synthesis in fibroblasts, and has obvious effect on reducing wrinkles and rough skin. However, the preparation process of many cosmetics containing AA-2G is too simple, which is only to directly and simply mix AA-2G with other ingredients, which can easily lead to inactivation or degradation of AA-2G, poor stability, and cannot effectively protect the activity of AA-2G in cosmetics, thereby resulting in poor use effect. Therefore, it is of great significance to provide a processing technology for improving the activity of AA-2G to ensure the activity of AA-2G in cosmetics, to achieve efficient moisturizing of the skin, improve skin elasticity and tightness, and reduce related lines. SUMMARY

[0004] In view of the above, it is necessary to provide an ascorbyl glucoside-containing fine line eye cream and a preparation method thereof. The fine line eye cream provided by the present application can not only improve the stability of ascorbyl glucoside and reduce the loss by optimizing the auxiliary materials and preparation process, but also can obtain good eye care effect by effective compounding of each raw material.

[0005] To achieve the above purpose, the technical scheme adopted by the present application is:

[0006] An ascorbyl glucoside-containing fine line eye cream, the fine line eye cream comprises A component, B component, C component, D component and water; wherein:

[0007] The A component comprises a first emulsifier, an emollient, a first thickening agent and a first antioxidant;

[0008] The B component comprises a first moisturizer, a second thickening agent, a chelating agent and a second emulsifier;

[0009] The C component comprises a second antioxidant and a second moisturizer;

[0010] The D component comprises active substances, which comprise ascorbyl glucoside and sodium acetylated hyaluronate.

[0011] Preferably, the first emulsifier comprises a mixture of glyceryl stearate, cetearyl alcohol and sodium stearoyl lactylate and / or tri (ceteareth-4) phosphate; the emollient comprises dimethicone and / or isononyl isononanoate; the first thickening agent comprises calcium octenyl succinate starch and / or cetearyl alcohol; the first antioxidant comprises tocopheryl acetate;

[0012] The first moisturizer comprises glycerin and / or erythritol; the second thickening agent comprises hydroxypropyl guar and / or polyacryloyldimethyltaurate sodium; the chelating agent comprises disodium EDTA; the second emulsifier comprises a mixture of polyacryloyldimethyltaurate sodium, hydrogenated polydecene and trideceth-10;

[0013] The second antioxidant comprises para-hydroxyacetophenone; the second moisturizer comprises 1,2-hexanediol and / or butylene glycol.

[0014] Preferably, the mass percentage of each component of the fine line cream is as follows: the first emulsifier 1.5-2.0%, the emollient 5.5-6.5%, the first thickening agent 4.5-5.5%, and the first antioxidant 0.4-0.6%, the first moisturizer 6.5-7.5%, the second thickening agent 0.4-0.6%, the chelating agent 0.04-0.06%, the second emulsifier 0.4-0.6%, the second antioxidant 0.5-0.7%, the second moisturizer 6.5-7.0%, ascorbyl glucoside 0.9-1.2%, and sodium acetylated hyaluronate 0.1-0.2%, and the rest is water.

[0015] Preferably, the active substances further comprise radix astragali extract and motherwort extract.

[0016] Preferably, the mass percentage of the radix astragali extract and the motherwort extract is 0.1-0.2% and 0.05-0.10% respectively.

[0017] The application further provides a preparation method of the fine line cream containing ascorbyl glucoside, comprising the following steps:

[0018] (1) mixing all raw materials of the A component, dissolving at 75-80°C, and stirring uniformly to obtain the A phase;

[0019] (2) Mix all raw materials of the B component, dissolve at 75-80℃, and stir to be uniform to obtain the B phase;

[0020] (3) Mix all raw materials of the C component to be uniform to obtain the C phase;

[0021] (4) Dissolve the D component in the buffer solution first, then add vitamin E and EDTA-2Na, and stir to be uniform to obtain the D phase;

[0022] (5) Maintain the B phase at 75℃, add the A phase into the B phase under homogenization, continue to homogenize for 3-5 min after the addition is completed, then gradiently reduce the temperature to 55-60℃, add the C phase, homogenize for 3-5 min, then add the pH regulator to adjust the pH to 6.0-6.5, continue to gradiently reduce the temperature to 45-50℃, then add the D phase and stir to be uniform, and naturally cool to obtain the fine line eye cream.

[0023] Preferably, in the step (4), the mass percentage of the vitamin E is 0.02-0.05% and the mass percentage of the EDTA-2Na is 0.05-0.07% based on the total mass of the fine line eye cream raw materials; and the buffer solution is a citric acid / citrate sodium tri buffer solution.

[0024] Preferably, in the step (5), the gradient temperature reduction process is as follows: from 75℃ to 55-60℃, reduce the temperature by 2-3℃ per minute, and keep for 10-15 min after the temperature reduction; and then from 55-60℃ to 45-50℃, reduce the temperature by 1-2℃ per minute, and keep for 10-15 min after the temperature reduction.

[0025] Preferably, in the step (5), the pH regulator is triethanolamine.

[0026] The present application has the following beneficial effects:

[0027] 1. In the fine line eye cream provided by the present application, the auxiliary materials matched with ascorbic acid glucoside and the overall preparation process are screened and optimized, so that the product obtained can not only ensure the stability of ascorbic acid glucoside, but also obtain good eye skin care effect.

[0028] 2. Compared with the preparation process of directly mixing ascorbic acid glucoside with other excipients in the prior art, firstly, the ascorbic acid glucoside is first dissolved in a buffer solution, so that the ascorbic acid glucoside is in a low temperature state, thereby ensuring the activity thereof, secondly, VE and ETDA-2Na are added to the ascorbic acid glucoside solution, and the two cooperate to quench free radicals and prevent metal ion catalytic oxidation, thereby reducing the risk of oxidative degradation and inactivation of the ascorbic acid glucoside, thirdly, the pH of the emulsion system is adjusted to 6.0-6.5 before the active substances are mixed, at the pH value, the stability of the ascorbic acid glucoside is optimal, and the risk of hydrolysis or discoloration by oxidation is avoided, and the residual activity rate is as high as 90% or more, thereby reducing the loss rate of the ascorbic acid glucoside in the preparation process, and finally, the emulsion system is cooled to 45-50 DEG C before the ascorbic acid glucoside is added, which can effectively avoid the decomposition and inactivation of the ascorbic acid glucoside due to high temperature, and the emulsion system adopts gradient cooling, which can improve the stability of the whole system compared with natural cooling, so that the ascorbic acid glucoside and the emulsion system maintain good compatibility, thereby further improving the stability thereof. Therefore, by optimizing the preparation process and organically combining various steps and process parameters, the stability of the ascorbic acid glucoside can be effectively improved, the loss rate of the ascorbic acid glucoside in the preparation process can be reduced, the residual activity rate is high, the loss rate of the ascorbic acid glucoside in the storage process can be reduced, and thus the use effect of the fine line eye cream is effectively improved.

[0029] 3. By compounding acetylated sodium hyaluronate or acetylated sodium hyaluronate, astragalus extract and motherwort extract with ascorbic acid glucoside as active substances, compared with using only ascorbic acid glucoside as active substances, the nutrition of the eye cream can be effectively improved, and the absorption and utilization of the eye cream are more beneficial, thereby further improving the use effect of the eye cream. DETAILED DESCRIPTION

[0030] In order to make the technical problems, technical solutions and advantages to be solved by the present application more clear, specific embodiments will be described in detail below.

[0031] In the present application, the reagents and consumables used are purchased from conventional reagent manufacturers in the field, and the experimental methods and technical means used are conventional methods and means in the field, unless otherwise specified.

[0032] A fine line eye cream containing ascorbic acid glucoside, the fine line eye cream comprising A component, B component, C component, D component and water, wherein:

[0033] The A component comprises a first emulsifier, an emollient, a first thickening agent and a first antioxidant;

[0034] The B component includes a first humectant, a second thickening agent, a chelating agent, and a second emulsifier;

[0035] The C component includes a second antioxidant and a second humectant.

[0036] The D component includes ascorbyl glucoside and sodium acetylated hyaluronate.

[0037] Preferably, the first emulsifier includes a mixture of glyceryl stearate, cetearyl alcohol, and sodium stearoyl lactylate and / or tri(ceteareth-4) phosphate. Illustratively, the first emulsifier is a mixture of glyceryl stearate, cetearyl alcohol, and sodium stearoyl lactylate and tri(ceteareth-4) phosphate.

[0038] Preferably, the emollient includes dimethicone and / or isononyl isononanoate. Illustratively, the emollient is dimethicone and isononyl isononanoate.

[0039] Preferably, the first thickening agent includes calcium starch octenyl succinate and / or cetearyl alcohol. Illustratively, the first thickening agent is calcium starch octenyl succinate and cetearyl alcohol.

[0040] Preferably, the first antioxidant includes tocopheryl acetate.

[0041] Preferably, the first humectant includes glycerin and / or erythritol. Illustratively, the first humectant includes glycerin and erythritol.

[0042] Preferably, the second thickening agent includes hydroxypropyl guar and / or polyacryloyldimethyltaurate. Illustratively, the second thickening agent includes hydroxypropyl guar and polyacryloyldimethyltaurate.

[0043] Preferably, the chelating agent includes disodium EDTA.

[0044] Preferably, the second emulsifier includes a mixture of polyacryloyldimethyltaurate, hydrogenated polydecene, and trideceth-10.

[0045] Preferably, the second antioxidant includes para-hydroxyacetophenone.

[0046] Preferably, the second humectant includes 1,2-hexanediol and / or butylene glycol.

[0047] Preferably, the mass percentage of each component in the fine line eye cream is: 1.5-2.0% of the first emulsifier, 5.5-6.5% of the emollient, 4.5-5.5% of the first thickening agent, and 0.4-0.6% of the first antioxidant, 6.5-7.5% of the first humectant, 0.4-0.6% of the second thickening agent, 0.04-0.06% of the chelating agent, 0.4-0.6% of the second emulsifier, 0.5-0.7% of the second antioxidant, 6.5-7.0% of the second humectant, 0.9-1.2% of ascorbyl glucoside, and 0.1-0.2% of sodium acetylated hyaluronic acid, and the rest is water.

[0048] For example, the mass percentage of each component in the fine line eye cream is: 1.7% of the first emulsifier, 6.0% of the emollient, 5.0% of the first thickening agent, and 0.5% of the first antioxidant, 7.0% of the first humectant, 0.5% of the second thickening agent, 0.05% of the chelating agent, 0.5% of the second emulsifier, 0.6% of the second antioxidant, 6.6% of the second humectant, 1.0% of ascorbyl glucoside, and 0.1% of sodium acetylated hyaluronic acid, and the rest is water.

[0049] For example, in the fine line eye cream:

[0050] The mass percentage of the first emulsifier can also be: 1.5%, 1.8%, 2.0%, etc.

[0051] The mass percentage of the emollient can also be: 5.5%, 5.8%, 6.2%, 6.5%, etc.

[0052] The mass percentage of the first thickening agent can also be: 4.5%, 4.8%, 5.3%, 5.5%, etc.

[0053] The mass percentage of the first antioxidant can also be: 0.4%, 0.6%, etc.

[0054] The mass percentage of the first humectant can also be: 6.5%, 6.8%, 7.2%, 7.5%, etc.

[0055] The mass percentage of the second thickening agent can also be: 0.4%, 0.6%, etc.

[0056] The mass percentage of the chelating agent can also be: 0.04%, 0.06%, etc.

[0057] The mass percentage of the second emulsifier can also be: 0.4%, 0.6%, etc.

[0058] The mass percentage of the second antioxidant can also be: 0.5%, 0.7%, etc.

[0059] The mass percentage of the second moisturizing agent can also be 6.5%, 6.7%, 7.0%, etc.

[0060] The mass percentage of the ascorbic acid glucoside can also be 0.9%, 1.1%, 1.2%, etc.

[0061] The mass percentage of the sodium acetylated hyaluronic acid can also be 0.15%, 0.2%, etc.

[0062] Preferably, the D component further comprises Astragalus extract and Motherwort extract.

[0063] Preferably, the mass percentages of the Astragalus extract and the Motherwort extract are 0.1-0.2% and 0.05-0.10%, respectively.

[0064] Illustratively, the mass percentage of the Astragalus extract can be 0.1%, 0.15%, 0.2%, etc.

[0065] Illustratively, the mass percentage of the Motherwort extract can be 0.05%, 0.08%, 0.10%, etc.

[0066] Illustratively, the Astragalus extract is prepared by the following method: Astragalus is pulverized to obtain Astragalus powder, the Astragalus powder and 95% ethanol are mixed at a solid-liquid ratio of 1:5, extraction is performed at 90°C for 3 hours, the extract is separated and filtered, the extract is concentrated and dried, and the Astragalus extract is obtained.

[0067] Illustratively, the Motherwort extract is prepared by the following method: Motherwort is pulverized to obtain Motherwort powder, the Motherwort powder and 95% ethanol are mixed at a solid-liquid ratio of 1:20, extraction is performed at 80°C for 2 hours, the extract is separated and filtered, the extract is concentrated and dried, and the Motherwort extract is obtained.

[0068] The present application also provides a preparation method of the light wrinkle cream containing ascorbic acid glucoside, comprising the following steps:

[0069] (1) all raw materials of the A component are mixed, dissolved at 75-80°C, and stirred uniformly to obtain A phase;

[0070] (2) all raw materials of the B component are mixed, dissolved at 75-80°C, and stirred uniformly to obtain B phase;

[0071] (3) all raw materials of the C component are mixed uniformly to obtain C phase;

[0072] (4) the D component is first dissolved in buffer, then vitamin E and EDTA-2Na are added and stirred uniformly to obtain D phase;

[0073] (5) maintaining B phase at 75℃, adding A phase into B phase under homogenization, after adding, continuing homogenization for 3-5 min, gradiently reducing temperature to 55-60℃, adding C phase, homogenizing for 3-5 min, then adding pH regulator to adjust pH to 6.0-6.5, continuing gradiently reducing temperature to 45-50℃, adding D phase to stir until mixed evenly, naturally cooling, thus the fine line eye cream is obtained.

[0074] Preferably, in step (4), the mass percentage of vitamin E is 0.02-0.05% and the mass percentage of EDTA-2Na is 0.05-0.07% based on the total mass of the fine line eye cream raw materials; and the buffer is citric acid / citrate buffer.

[0075] Illustratively, the mass percentage of vitamin E can be 0.02%, 0.03%, 0.04%, 0.05%, etc.

[0076] Illustratively, the mass percentage of EDTA-2Na can be 0.05%, 0.06%, 0.07%, etc.

[0077] Preferably, in step (5), the gradiently reducing temperature process is: reducing from 75℃ to 55-60℃, reducing temperature by 2-3℃ per minute, and maintaining for 10-15 min after reducing temperature; then reducing from 55-60℃ to 45-50℃, reducing temperature by 1-2℃ per minute, and maintaining for 10-15 min after reducing temperature.

[0078] Illustratively, in step (5), the maintaining time after reducing temperature can be 10 min, 12 min, 14 min or 15 min, etc.

[0079] Preferably, in step (5), the pH regulator is triethanolamine.

[0080] The present application will be further described below in conjunction with specific examples. It should be understood that these examples are only used to illustrate the present application and not to limit the scope of the present application.

[0081] First, the following example raw material components correspond to the following trade names:

[0082] Table 1 Fine line eye cream raw material component corresponding trade name and manufacturer

[0083]

[0084] Secondly, the ascorbic acid glucoside used in the following examples is prepared by the following method:

[0085] (1) constructing a recombinant plasmid pET-28a / SPase: selecting pET-28a as a plasmid vector, cloning a coding gene of sucrose phosphorylase into the pET-28a vector, so as to obtain the recombinant plasmid pET-28a / SPase containing the sucrose phosphorylase gene;

[0086] (2) constructing a recombinant E. coli BL21(DE3) / pET28a-SPase: taking E. coli BL21(DE3) as a host cell, transferring the recombinant plasmid pET-28a / SPase into the E. coli BL21(DE3) competent cell, and coating on the LB solid culture medium containing 50 μg / mL kanamycin for cultivation, so as to obtain a single colony; transferring the single colony into the LB liquid culture medium containing 50 μg / mL kanamycin for cultivation, so as to obtain the recombinant E. coli BL21(DE3) / pET28a-SPase;

[0087] (3) cultivation and induced expression of the recombinant E. coli BL21(DE3) / pET28a-SPase: inoculating the recombinant E. coli BL21(DE3) / pET28a-SPase into the LB liquid culture medium containing 50 μg / mL kanamycin for cultivation, so as to obtain a seed liquid; inoculating the seed liquid into the fermentation culture medium containing 50 μg / mL kanamycin for cultivation; when the biomass of the bacterial liquid in the fermentation culture medium reaches OD 600 15, adding IPTG to induce the reaction for 15 h, centrifuging, and collecting a bacterial precipitate;

[0088] (4) whole-cell transformation synthesis: taking the bacterial precipitate as a biological catalyst, taking sucrose and L-ascorbic acid as substrates to form a transformation system, and performing a transformation reaction, so as to obtain a reaction liquid;

[0089] (5) yeast cultivation: adding yeast to the reaction liquid for cultivation, so as to obtain a cultivation liquid; filtering to remove solid substances in the cultivation liquid, so as to obtain a supernatant;

[0090] (6) concentration and drying: sequentially performing concentration, crystallization, washing and drying on the supernatant, so as to obtain the ascorbic acid glucoside.

[0091] The ascorbic acid glucoside prepared by the preparation method has high yield and good stability.

[0092] The basic conditions of the ascorbic acid glucoside prepared by the preparation method are shown in Table 2.

[0093] Table 2 Basic conditions of ascorbic acid glucoside

[0094]

[0095] I. Fine line eye creams prepared by different formulations / preparation processes Example 1-2 and Comparative Example 1-4

[0096] Example 1-2 (S1-2) and Comparative Example 1-4 (D1-4) each provide a cream, and the specific formulations of the fine line eye creams provided in each example are shown in Table 3 below.

[0097] Table 3 Formulation of fine line eye cream (% w / w)

[0098]

[0099] The preparation method of each example of fine line eye cream is as follows:

[0100] The preparation method of the fine line eye creams of S1-S2 and D1 includes the following steps:

[0101] (1) Mix all the raw materials of the A component, dissolve at 80°C, and stir uniformly to obtain the A phase;

[0102] (2) Mix all the raw materials of the B component, dissolve at 80°C, and stir uniformly to obtain the B phase;

[0103] (3) Mix all the raw materials of the C component uniformly to obtain the C phase;

[0104] (4) Dissolve the D component in the buffer solution first, then add 0.02wt% of vitamin E and 0.05wt% of EDTA-2Na, and stir uniformly to obtain the D phase;

[0105] (5) Maintain the B phase at 75°C, add the A phase to the B phase under homogenization, continue to homogenize for 5min after adding, cool down to 55°C at a speed gradient of 3°C per minute, keep for 10min, add the C phase, homogenize for 5min, then add the pH adjuster to adjust the pH to 6.2, continue to cool down to 45°C at a speed gradient of 2°C per minute, keep for 10min, add the D phase and stir until mixed uniformly, and naturally cool down to obtain the fine line eye cream.

[0106] The preparation method of the fine line eye cream of D2 includes the following steps:

[0107] (1) Mix all the raw materials of the A component, dissolve at 80°C, and stir uniformly to obtain the A phase;

[0108] (2) Mix all the raw materials of the B component, dissolve at 80°C, and stir uniformly to obtain the B phase;

[0109] (3) Mix all the raw materials of the C component uniformly to obtain the C phase;

[0110] (4) Dissolve the D component in the buffer solution first, then add 0.02wt% of vitamin E and 0.05wt% of EDTA-2Na and stir until uniform, to obtain the D phase;

[0111] (5) Maintain the B phase at 75°C, add the A phase to the B phase under homogenization, continue to homogenize for 5 min after adding, naturally cool to 55°C, then add the C phase, homogenize for 5 min, then add the pH regulator to adjust the pH to 6.2, continue to naturally cool to 45°C, maintain for 10 min, add the D phase and stir until uniform, and then naturally cool, to obtain the fine line eye cream.

[0112] The preparation method of the fine line eye cream of D3 includes the following steps:

[0113] (1) Mix all the raw materials of the A component, dissolve at 80°C, and stir until uniform, to obtain the A phase;

[0114] (2) Mix all the raw materials of the B component, dissolve at 80°C, and stir until uniform, to obtain the B phase;

[0115] (3) Mix all the raw materials of the C component uniformly, to obtain the C phase;

[0116] (4) Dissolve the D component in the buffer solution first, and stir until uniform, to obtain the D phase;

[0117] (5) Maintain the B phase at 75°C, add the A phase to the B phase under homogenization, continue to homogenize for 5 min, cool to 55°C at a gradient of 3°C per minute, maintain for 10 min, add the C phase, homogenize for 5 min, then add the pH regulator to adjust the pH to 6.2, continue to gradient cooling at a gradient of 2°C per minute to 45°C, maintain for 10 min, add the D phase and stir until uniform, and then naturally cool, to obtain the fine line eye cream.

[0118] The preparation method of the fine line eye cream of D4 includes the following steps:

[0119] (1) Mix all the raw materials of the A component, dissolve at 80°C, and stir until uniform, to obtain the A phase;

[0120] (2) Mix all the raw materials of the B component, dissolve at 80°C, and stir until uniform, to obtain the B phase;

[0121] (3) Mix all the raw materials of the C component uniformly, to obtain the C phase;

[0122] (4) Mix all the raw materials of the D component uniformly, to obtain the D phase;

[0123] (5) maintaining B phase at 75°C, adding A phase into B phase under homogenization, continuing to homogenize for 5 min after adding, naturally warming to 55°C, adding C phase, homogenizing for 5 min, then adding pH regulator to adjust pH to 6.2, naturally cooling to 45°C, adding D phase and stirring until mixed uniformly, and naturally cooling to obtain the light wrinkle cream.

[0124] II. Performance / effect test of each example light wrinkle cream

[0125] 1. Ascorbyl glucoside loss rate test

[0126] 1) Reagents

[0127] Ascorbyl glucoside standard, purity ≥98%.

[0128] Trifluoroacetic acid, analytical pure.

[0129] 2) Instruments

[0130] Liquid chromatograph: with ultraviolet detector;

[0131] Chromatographic column: Elite Hypersil ODS2 5μm 4.6mm×250mm.

[0132] 3) Chromatographic conditions

[0133] Mobile phase: 0.1% trifluoroacetic acid aqueous solution (accurately take 1 mL of trifluoroacetic acid and dilute to 1000 mL with deionized water);

[0134] Wavelength: 236 nm;

[0135] Flow rate: 0.5 ml / min;

[0136] Injection volume: 5uL;

[0137] Column temperature: 30°C.

[0138] 4) Detection steps

[0139] (1) Preparation of standard solution

[0140] The ascorbyl glucoside standard was dissolved in water to prepare a 1000 mg / L standard stock solution; a certain volume of the standard stock solution was removed and prepared into a 100 mg / L mixed standard solution with 0.02 mol / L potassium dihydrogen phosphate solution (pH 3.0), and the mixed standard solution was prepared immediately before use.

[0141] (2) Preparation of sample solution

[0142] Samples: the initial light wrinkle creams prepared in Examples 1-2 and Comparative Examples 2-4 and the creams after being stored at 25°C and 45°C for 45 d.

[0143] Preparation: Accurately weigh 0.250 g of sample into a 50 mL stoppered colorimetric tube, add 1.0 mL of dichloromethane, vortex until the sample is uniformly dispersed, then accurately add 25 mL of 0.02 mol / L potassium dihydrogen phosphate solution (pH 3.0), and vortex for 2 min. After mixing, transfer 10 mL of the solution to a 15 mL centrifuge tube and centrifuge at 10℃ and 12000 r / min for 10 min. Filter the supernatant through a 0.22 μm filter membrane; the filtrate is the sample to be tested.

[0144] (3) Determination: After the instrument baseline stabilizes, continuously inject samples and calculate the average value of the peak areas. Based on the obtained peak area values, determine the concentration of ascorbate glucoside in the sample solution from the standard curve.

[0145] (4) Calculation

[0146] First, calculate the ascorbate glucoside content:

[0147] The ascorbate glucoside content in the sample is expressed as a mass fraction W1, and the value is expressed as a percentage (%), calculated using the following formula:

[0148]

[0149] In the formula:

[0150] A standard – the average peak area of ​​ascorbate glucoside in the standard solution;

[0151] Sample A ----- The average peak area of ​​ascorbate glucoside in the sample solution;

[0152] m represents the mass of ascorbate glucoside standard, in grams.

[0153] m_sample — Mass of the sample, in grams;

[0154] P—mass fraction of ascorbate glucoside in the standard, % (m / m);

[0155] Secondly, calculate the loss rate of ascorbate glucoside:

[0156] Ascorbate glucoside loss rate = (Ascorbate glucoside content in the initial sample - Ascorbate glucoside content in the sample after storage) / Ascorbate glucoside content in the initial sample × 100%.

[0157] (5) Calculation results

[0158] The results of the ascorbate glucoside loss rate of each group of wrinkle-reducing eye creams are shown in Table 4 below.

[0159] Table 4. Loss rate of ascorbate glucoside in anti-wrinkle eye cream

[0160]

[0161] As can be seen from Table 4, the loss rate S2 of ascorbic acid glucoside < S1 < D1, indicating that the present application can reduce the loss rate of ascorbic acid glucoside to some extent by compounding sodium acetylated hyaluronic acid, astragalus extract and motherwort extract with ascorbic acid glucoside as active substances, which may be because the compatibility of ascorbic acid glucoside loss rate in the whole cream is improved by the interaction of some ingredients, thereby improving the stability. At the same time, as the loss rate S1 is less than D2-D4, the ascorbic acid glucoside is dissolved and prepared first and then mixed with the remaining ingredients, combined with gradient cooling, which can effectively improve the stability of ascorbic acid glucoside, not only can reduce the loss of ascorbic acid glucoside in the preparation process, but also can reduce the loss in the preservation process.

[0162] 2. Efficacy verification

[0163] (1) Subjects: Select healthy women with dry, rough, loose skin, lack of elasticity and obvious wrinkles around the eyes and corners of the mouth. The subjects have no allergic diseases, no history of allergy to cosmetics and other external preparations, and are daily users of basic moisturizing lotion and emulsion / cream. A total of 60 subjects, aged 40-50 years old. The subjects are divided into 6 groups, 10 people in each group.

[0164] (2) Test products: Example 1-2 and Comparative Example 1-4 lightening eye cream.

[0165] (3) Test method: After the subjects clean their faces and use the lotion every night, take an appropriate amount of eye cream and evenly apply it around the eyes, gently point and apply it to the skin around the eyes and the nasolabial folds, and use the massage head to gently massage the skin around the eyes from inside to outside and from bottom to top until it is absorbed. Once a day, for 28 consecutive days. Statistical analysis is made on the changes of the subjects' eye skin before and after the test, and the change rate is obtained.

[0166] (4) Test items

[0167] Skin keratin layer moisture content: Corneometer CM 825 skin keratin layer moisture content tester is used to test the skin keratin layer moisture content;

[0168] Skin elasticity and tightness: Cutometer MPA580 skin elasticity tester is used to test the skin elasticity and tightness.

[0169] Periorbital wrinkle depth improvement rate: Evaskin-S5 skin rapid optical imaging system is used to test the improvement effect of each wrinkle.

[0170] (5) Calculation method

[0171] Improvement rate (%) after using product = (data after using - data before using) / data before using * 100%. The efficacy determination results are shown in Table 5.

[0172] Table 5: Efficacy determination results of each group of fine line eye cream

[0173]

[0174] As shown in Table 5, the fine line eye cream efficacy of S2 is better than that of S1, and the fine line eye cream efficacy of S1 is better than that of D1, which shows that, by compounding sodium acetylated hyaluronic acid, radix astragali extract and motherwort extract with ascorbic acid glucoside as active substances, the application can interact to improve the care effect of eye skin. The fine line eye cream efficacy of D2-D4 is worse than that of S1, which may be because the loss rate of ascorbic acid glucoside is relatively large during the preparation process of the fine line eye cream of D2-D4, resulting in a low active residual rate of ascorbic acid glucoside in the prepared eye cream, thereby making the eye skin care effect worse.

Claims

1. A light line eye cream containing ascorbic acid glucoside, characterized by, The light line eye cream comprises A component, B component, C component, D component and water; wherein: The A component comprises first emulsifier, emollient, first thickening agent and first antioxidant; The B component comprises first moisturizer, second thickening agent, chelating agent and second emulsifier; The C component comprises second antioxidant and second moisturizer; The D component comprises active substance, which comprises ascorbic acid glucoside and acetylated sodium hyaluronate.

2. The light line eye cream containing ascorbic acid glucoside according to claim 1, wherein, The first emulsifier comprises a mixture of glyceryl stearate, cetearyl alcohol and sodium stearoyl lactylate and / or tris(ceteareth-4) phosphate; the emollient comprises dimethicone and / or isononyl isononanoate; the first thickening agent comprises calcium starch octenyl succinate and / or cetearyl alcohol; and the first antioxidant comprises tocopheryl acetate; The first moisturizer comprises glycerin and / or erythritol; the second thickening agent comprises hydroxypropyl guar and / or polyacryloyldimethyltaurine sodium; the chelating agent comprises disodium EDTA; and the second emulsifier comprises a mixture of polyacryloyldimethyltaurine sodium, hydrogenated polydecene and trideceth-10; The second antioxidant comprises p-hydroxyacetophenone; and the second moisturizer comprises 1,2-hexanediol and / or butylene glycol.

3. The ascorbyl glucoside-containing fine line cream according to claim 1, characterized by, The mass percentage of each component of the light line eye cream is as follows: 1.5-2.0% of the first emulsifier, 5.5-6.5% of the emollient, 4.5-5.5% of the first thickening agent, 0.4-0.6% of the first antioxidant, 6.5-7.5% of the first moisturizer, 0.4-0.6% of the second thickening agent, 0.04-0.06% of the chelating agent, 0.4-0.6% of the second emulsifier, 0.5-0.7% of the second antioxidant, 6.5-7.0% of the second moisturizer, 0.9-1.2% of ascorbic acid glucoside and 0.1-0.2% of acetylated sodium hyaluronate, and the rest is water.

4. The ascorbyl glucoside-containing fine line cream according to claim 1, characterized in that, The active substance further comprises radix astragali extract and motherwort extract.

5. The ascorbic acid glucoside-containing fine line cream of claim 4, wherein the ascorbic acid glucoside is ascorbic acid 2-glucoside. The mass percentage of the radix astragali extract and the motherwort extract is 0.1-0.2% and 0.05-0.10%, respectively.

6. The method for preparing the ascorbyl glucoside-containing light line eye cream according to any one of claims 1 to 5, characterized by, The method comprises the following steps: (1) mixing all raw materials of the A component, dissolving at 75-80℃, stirring uniformly to obtain A phase; (2) mixing all raw materials of the B component, dissolving at 75-80℃, stirring uniformly to obtain B phase; (3) mixing all raw materials of the C component uniformly to obtain C phase; (4) dissolving the D component in buffer solution first, then adding vitamin E and EDTA-2Na, stirring uniformly to obtain D phase; (5) maintaining B phase at 75℃, adding A phase into B phase under homogenization, continuing homogenization for 3-5 min after adding, gradient cooling to 55-60℃, then adding C phase, homogenizing for 3-5 min, adding pH regulator to adjust pH to 6.0-6.5, continuing gradient cooling to 45-50℃, then adding D phase, stirring until mixed uniformly, and naturally cooling to obtain the light line eye cream.

7. The method for preparing an eye cream containing ascorbate glucoside for reducing wrinkles according to claim 6, characterized in that, In step (4), the mass percentage of vitamin E is 0.02-0.05%, the mass percentage of EDTA-2Na is 0.05-0.07%; and the buffer is a citric acid / citrate buffer.

8. The method for preparing an eye cream containing ascorbate glucoside for reducing wrinkles according to claim 6, characterized in that, In step (5), the gradient cooling process is: from 75℃ to 55-60℃, cooling at a rate of 2-3℃ per minute, and maintaining for 10-15 minutes after cooling; and then from 55-60℃ to 45-50℃, cooling at a rate of 1-2℃ per minute, and maintaining for 10-15 minutes after cooling.

9. The method for preparing an eye cream containing ascorbate glucoside for reducing wrinkles according to claim 6, characterized in that, In step (5), the pH regulator is triethanolamine.

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