A whitening composition containing oxidized resveratrol microcapsules and its preparation method and application
Through the combination of oxidized resveratrol microcapsules with specific structures, gentian extract, mutton extract and lupin extract, the problems of stability and gentleness of whitening compositions in the prior art are solved, and effective desalination and skin repair of pigmented dark circles are achieved, and suitable for sensitive skin use.
Patent Information
- Application Number
- CN202411693817.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-25
- Publication Date
- 2025-08-26
- Estimated Expiration
- 2044-11-25
AI Technical Summary
In the prior art, vitamin C is unstable, arbutin may irritate sensitive skin at high concentrations, nicotinamide whitening effect is slow, making it difficult to take into account the whitening efficacy and the stability and gentleness of the formula, especially when lightening pigmented dark circles.
Using oxidized resveratrol microcapsules with specific structures, combined with gantian extract, mullet extract and lupin extract, a whitening composition is prepared by a wall material composed of cerium oxide and β-glucan in a specific weight ratio, erectile fruit oil and sunflower seed oil as carrier oil, to enhance the whitening and repairing effect, and is suitable for sensitive skin use.
It has achieved effective desalination of pigmented dark circles, and the ingredients are gentle and not irritating. Through the slow release mechanism, the active ingredients can penetrate deep into the skin, significantly reducing the skin redness and inflammation, improving the skin barrier function, and is suitable for sensitive skin.
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Figure CN119632884B_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of cosmetics, in particular to a whitening composition containing oxidized resveratrol microcapsules, and a preparation method and application thereof. Background Art
[0002] Pigmented dark circles are primarily caused by hyperpigmentation and are common in people with darker skin and sensitive skin. Frequently staying up late, prolonged exposure to sunlight, or skin allergies can cause chronic skin inflammation, leading to post-inflammatory hyperpigmentation. The skin around the eyes is particularly thinner and more susceptible to external irritations such as allergies and friction, making the area more susceptible to hyperpigmentation. Existing technologies for treating pigmented dark circles typically use ingredients such as vitamin C, arbutin, and niacinamide. These ingredients have a whitening effect and can effectively reduce hyperpigmentation. However, vitamin C is unstable and may lose its activity during use; arbutin may irritate sensitive skin at high concentrations; and niacinamide has low irritation, but its whitening effect is limited and takes too long to show results.
[0003] Therefore, how to balance the whitening efficacy with the stability and mildness of the formula is the key to lightening pigmented dark circles. Summary of the Invention
[0004] Based on this, the purpose of the present invention is to overcome the deficiencies of the above-mentioned prior art and provide a whitening composition containing oxidized resveratrol microcapsules and a preparation method and application thereof.
[0005] To achieve the above-mentioned purpose, the technical solution adopted by the present invention is: a whitening composition, comprising the following components in parts by weight: 1-20 parts of oxidized resveratrol microcapsules, 0.01-2 parts of Yunnan Gentiana extract, 0.1-10 parts of Mullein extract, and 0.01-1 part of Lupin extract; wherein the oxidized resveratrol microcapsules include a core material, a wall material, a carrier oil and an emulsifier, and the weight ratio of the core material, wall material, carrier oil and emulsifier is core material: wall material: carrier oil: emulsifier = 1: (1-6): (1-8): (0.05-0.2); the core material is oxidized resveratrol; the wall material is a mixture of cerium oxide and β-glucan, and the weight ratio of cerium oxide to β-glucan is 1: (0.5-5); the carrier oil is a mixture of juniper fruit oil and sunflower seed oil.
[0006] The main active ingredient of Yunnan Gentiana extract is gentiopicroside, which has significant anti-inflammatory, antioxidant and repairing effects, and has a good soothing effect on the dullness caused by vascular inflammation in dark circles; Mullein extract is rich in flavonoids, such as quercetin, flavonols, etc., which have whitening and soothing effects through antioxidant, anti-inflammatory and inhibition of tyrosinase activity; Lupin extract is rich in isoflavones and peptide compounds, which have antioxidant, pigmentation and repair effects, help brighten the skin tone and enhance the skin barrier function. The above three extracts, in conjunction with the specific structure of the oxidized resveratrol microcapsules provided by the present invention, form a whitening composition with four ingredients, which comprehensively enhances the whitening and repairing effects, inhibits post-inflammatory pigmentation, and strengthens the fragile skin around the eyes. The whitening composition provided by the present invention can effectively lighten pigmented dark circles, is mild and non-irritating to the eyes, and is suitable for people with sensitive skin.
[0007] Oxidized resveratrol has antioxidant, anti-inflammatory, photoprotective, and whitening effects, but its stability is poor and it is easily affected by light, heat, and oxygen. The present invention uses a microencapsulation technology with a specific structure to effectively protect its activity, control its release, and increase its stability. Cerium oxide is an inorganic substance with good stability and safety, and has strong antioxidant and self-repair properties. It can scavenge free radicals through catalytic reactions and play a protective role in the microcapsule; β-glucan is a water-soluble polysaccharide with certain viscosity and adhesion, and has good biocompatibility, moisturizing, and immunomodulatory effects. β-glucan can provide excellent encapsulation and biocompatibility. Cerium oxide combines with β-glucan by physical adsorption, together forming the wall layer of the microcapsule. Cerium oxide particles are relatively hard, which may affect the encapsulation effect of β-glucan. If the ratio of the two is not appropriate, it may affect the stability and release characteristics of the microcapsule. The inventors have found through experiments that good stability and release characteristics can only be achieved when the weight ratio of cerium oxide to β-glucan is within the specified range of this application.
[0008] Juniper berry oil is rich in unsaturated fatty acids and vitamin E, and has the ability to promote skin regeneration and repair. It is suitable for repairing damaged skin. It also brightens and makes the skin transparent by promoting proteasome activity, inhibiting lipofuscin deposition, and improving internal turbidity of cells. Sunflower seed oil is rich in plant oleic acid, which can help repair the skin barrier, improve skin hydration, and keep the skin soft and smooth. It also has certain anti-inflammatory properties, which helps reduce skin redness and inflammation, and is suitable for sensitive skin. The inventors found through experiments that when juniper berry oil and sunflower seed oil are used together as carrier oils for oxidized resveratrol microcapsules, the oxidized resveratrol microcapsules have better stability and release characteristics.
[0009] During the preparation of oxidized resveratrol microcapsules, the components and dosage of the emulsifier are not explored in detail, and any common emulsifier in the art can be used; preferably, the emulsifier includes at least one of polyethylene glycol-100, steareth-2, steareth-21, oleth-10, glyceryl oleate, sorbitan stearate, polysorbate 60, methyl glucose sesquistearate, caprylic capric triglyceride, C14-22 alcohol, C12-20 alkyl glucoside, cetearyl glucoside, isononyl isononanoate, pentaerythritol tetraisostearate, polydimethylsiloxane, stearyl alcohol, hydroxystearic acid, polymethylsilsesquioxane, pentaerythritol distearate, and sucrose stearate.
[0010] Preferably, the whitening composition comprises the following components in parts by weight: 5-15 parts of oxidized resveratrol microcapsules, 0.1-0.5 parts of Gentiana yunnanensis extract, 1-5 parts of Mullein extract, and 0.1-0.5 parts of Lupinus officinalis extract.
[0011] Preferably, the mass percentage of oxidized resveratrol microcapsules in the whitening composition is 50-80%.
[0012] The inventors found in actual experiments that the proportion of oxidized resveratrol microcapsules, gentiana yunnanensis extract, mullein extract, and lupin extract in the whitening composition affects the whitening and repairing effect. When it is within the above range, the whitening and repairing effect is better.
[0013] Preferably, the weight ratio of the core material, wall material, carrier oil and emulsifier is core material: wall material: carrier oil: emulsifier = 1: (2-4): (2-5): (0.05-0.2).
[0014] Preferably, the weight ratio of cerium oxide to β-glucan is 1:(1-3);
[0015] And / or, the weight ratio of the juniper berry oil to the sunflower seed oil is 1:(0.5-8); preferably, the weight ratio of the juniper berry oil to the sunflower seed oil is 1:(3-4).
[0016] In actual experiments, the inventors discovered that the weight ratios of the core material, wall material, and carrier oil, the weight ratio of cerium oxide to β-glucan, and the weight ratio of juniper berry oil to sunflower seed oil all affect the stability and release characteristics of the resulting oxidized resveratrol microcapsules, thereby affecting the whitening and repairing effects of the whitening composition. When the weight ratios are within these specific ranges, the oxidized resveratrol microcapsules exhibit better stability and release characteristics.
[0017] Preferably, the β-glucan includes at least one of β-1,3 / α-1,3-glucan, β-1,3-glucan, β-1,4-glucan, β-1,6-glucan, and β-1,3(1,6)-glucan, and the molecular weight of the β-glucan is 1 million to 5 million Daltons.
[0018] Preferably, the average particle size of the cerium oxide is 0.05-10 μm; more preferably, the average particle size of the cerium oxide is 0.2-3 μm.
[0019] The inventors found in actual experiments that the average particle size of cerium oxide affects the stability and release characteristics of the finally prepared oxidized resveratrol microcapsules. When the average particle size of the cerium oxide is 0.2-3 μm, the stability and release characteristics of the oxidized resveratrol microcapsules are better.
[0020] Preferably, the method for preparing the oxidized resveratrol microcapsules comprises the following steps:
[0021] (1) Add 30-40°C water to the wall material and stir to dissolve to obtain mixture A;
[0022] (2) mixing the carrier oil and the emulsifier, heating and homogenizing to obtain a mixture B;
[0023] (3) mixing oxidized resveratrol and a solvent, adding mixture B, and homogenizing to obtain mixture C;
[0024] (4) heating the mixture C and the mixture A to homogenize, spray drying, collecting and sieving to obtain the oxidized resveratrol microcapsules.
[0025] Preferably, in step (1), the weight ratio of the wall material to water is 1:(1-2); and ultrasonic treatment is used to ensure that the material is completely dissolved or evenly dispersed.
[0026] Preferably, in step (2), the mixture is heated to 55-65° C., the homogenization speed is 1000-1300 rpm, and the homogenization time is 3-5 min.
[0027] Preferably, in step (3), the solvent is anhydrous ethanol, and the mass volume ratio of oxidized resveratrol to the solvent is 1 g: (5-6) mL; the homogenization speed is 1000-1300 rpm, and the homogenization time is 3-5 min.
[0028] Preferably, in step (4), the mixture is heated to 60-70° C., the homogenization speed is 12000-20000 rpm, and the homogenization time is 20-40 min.
[0029] Preferably, in step (3), the air inlet temperature of the spray drying tower is 120°C-150°C, and the air outlet temperature is 70°C-80°C. The microcapsule powder is collected by a collection device (e.g., an air flow separator) after spray drying. Sieving is then performed to remove large and irregular particles to obtain the desired oxidized resveratrol microcapsules.
[0030] In addition, the present invention provides the use of the whitening composition in preparing skin products.
[0031] Furthermore, the present invention provides a skin care product comprising the whitening composition.
[0032] Preferably, the skin care product further comprises an auxiliary material, wherein the auxiliary material is at least one of a moisturizer, a thickener, a pH regulator, an emulsifier, a preservative, a fragrance, and deionized water.
[0033] Preferably, the skin product comprises one of lotion, emulsion, cream, eye cream, eye mask, essence, and spray.
[0034] Optionally, the present invention provides an eye cream comprising the following components in percentage by mass: 1-15% whitening composition, 0.05-0.5% thickener, 0.5-2% moisturizer, 5-20% emulsifier, 0.5-3% preservative, 0.01-0.3% pH adjuster, and the balance deionized water.
[0035] Exemplarily, the moisturizing agent includes at least one of allantoin, sodium polyacrylate, hydrogenated lecithin, betaine, β-glucan, trehalose, caprylyl glycol, dipropylene glycol, sodium hyaluronate, 1,2-butylene glycol, glycerin, budding septor polysaccharide, and ceramide; the thickening agent includes at least one of xanthan gum, carbomer, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, ammonium acryloyldimethyl taurate / VP copolymer, sclerotium gum, and cetyl alcohol; the emulsifier includes caprylic capric triglyceride, C14-22 alcohol, C12 The invention also comprises at least one of: -20 alkyl glucoside, cetearyl glucoside, isononyl isononanoate, pentaerythritol tetraisostearate, polydimethylsiloxane, stearyl alcohol, hydroxystearic acid, polymethylsilsesquioxane, pentaerythritol distearate, and sucrose stearate; the preservative comprises at least one of 1,3-propylene glycol, 1,2-propylene glycol, 1,2-hexanediol, p-hydroxyacetophenone, and acrylates / C10-30 alkyl acrylate crosspolymer; the pH adjuster comprises at least one of arginine, tromethamine, and EDTA-disodium.
[0036] Compared with the prior art, the present invention has the following beneficial effects: (1) The whitening composition of the four ingredients, including the Yunnan gentian extract, the mullein extract, and the lupin extract, works synergistically with the oxidized resveratrol microcapsules of the specific structure provided by the present invention, comprehensively enhancing the whitening and repairing effects, inhibiting post-inflammatory pigmentation, and strengthening the fragile skin around the eyes. The whitening composition provided by the present invention can effectively lighten pigmented dark circles, and is mild and non-irritating to the eyes, making it suitable for people with sensitive skin. (2) The oxidized resveratrol microcapsules of the specific structure provided by the present invention, through a slow release mechanism, can allow the active ingredients to penetrate deeper into the skin, ensuring that they exert their best effects, rather than high-concentration stimulation in a short period of time. Compared with traditional methods, due to the mild formula and complementary ingredients, it can achieve visible whitening and repairing effects in a shorter period of time and reduce the discomfort caused by strong whitening agents. BRIEF DESCRIPTION OF THE DRAWINGS
[0037] Figure 1 These are the eye condition pictures of volunteers after using the eye creams of the blank application example and application example 1; among them, (a) is the eye condition picture of the volunteer before use, (b) is the eye condition picture of the volunteer after using the eye creams for 14 days, and (c) is the eye condition picture of the volunteer after using the eye creams for 28 days. DETAILED DESCRIPTION
[0038] In order to better illustrate the purpose, technical solutions and advantages of the present invention, the present invention will be further described below with reference to the accompanying drawings and specific examples. Its purpose is to understand the content of the present invention in detail, rather than to limit the present invention. All other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention. Unless otherwise specified, the experimental reagents and instruments designed for the implementation and comparative examples of the present invention are all commonly used ordinary reagents and instruments, which can be obtained from commercial channels. In the implementation and comparative examples, the experimental methods used are all conventional methods unless otherwise specified; and unless otherwise specified, the raw materials used in parallel experiments are from the same batch of raw materials.
[0039] The raw materials used in the present invention are further described:
[0040] Gentiana yunnanensis extract: purchased from Yunnan Yingge Biotechnology Co., Ltd.;
[0041] Mullein extract: purchased from Phenbiox, Italy;
[0042] Lupin extract: purchased from Coyen Company, France;
[0043] Safflower extract: purchased from Guangzhou Meiyi Biotechnology Co., Ltd.
[0044] Cerium oxide-1: purchased from Beijing Weiye Innovation Technology Co., Ltd., the trade name is luminescent TM , average particle size 200nm;
[0045] Cerium oxide-2: purchased from Qinghe County Tenghui Metal Materials Co., Ltd., product number HT-CeO2-2, average particle size 1 μm;
[0046] Cerium oxide-3: purchased from Shandong Desheng New Materials Co., Ltd., with an average particle size of 10 μm;
[0047] Cerium oxide-4: purchased from Qinghe County Tenghui Metal Materials Co., Ltd., product number HT-CeO2-1, average particle size 50 nm;
[0048] β-Glucan-1: purchased from Sichuan Hetai Xinguang Biotechnology Co., Ltd., with a structure of β-1,3 / α-1,3-glucan and a molecular weight of 2 million to 2.5 million Daltons;
[0049] β-Glucan-2: purchased from BASF, Germany, with a structure of β-1,3(1,6)-glucan and a molecular weight of 4.5 million to 5 million Daltons;
[0050] Juniperus chinensis fruit oil: purchased from Jiangxi Senhai Vegetable Oil Co., Ltd.
[0051] Sunflower oil: purchased from Croda, UK;
[0052] Oxidized resveratrol: purchased from Shaanxi Hongpeptide Biotechnology Co., Ltd.;
[0053] Oxidized Resveratrol Microcapsules-1
[0054] The preparation method of the oxidized resveratrol microcapsule-1 comprises the following steps:
[0055] (1) adding water at 35°C to the wall material, with the weight ratio of the wall material to water being 1:2, and performing ultrasonic treatment to ensure that the material is completely dissolved, thereby obtaining a mixture A;
[0056] (2) The carrier oil and the emulsifier were mixed, heated to 60° C., and homogenized at a speed of 1000 rpm for 3 min to obtain a mixture B;
[0057] (3) mixing oxidized resveratrol and ethanol uniformly, wherein the mass volume ratio of oxidized resveratrol to ethanol is 1 g:6 mL; adding mixture B, and homogenizing to obtain mixture C; the homogenizing speed is 1000 rpm, and the homogenization time is 5 min;
[0058] (4) Mixture C and mixture A were heated to 60°C, homogenized at a speed of 12,000 rpm for 40 minutes, and spray-dried at an air inlet temperature of 120°C and an outlet temperature of 80°C. The microcapsule powder was collected by a collection device (airflow separator) after spray drying. Large and irregular particles were then removed using a centrifugal sieve to obtain the desired oxidized resveratrol microcapsules.
[0059] The oxidized resveratrol microcapsule-1 comprises 1 part of core material, 2 parts of wall material, 5 parts of carrier oil, and 0.1 part of emulsifier; the core material is oxidized resveratrol; the wall material is a mixture of cerium oxide-1 and β-glucan-1, with a weight ratio of 1:1; the carrier oil is a mixture of juniper fruit oil and sunflower seed oil, with a weight ratio of 1:3; the emulsifier is polyethylene glycol-100;
[0060] Oxidized resveratrol microcapsules-2 to oxidized resveratrol microcapsules-21
[0061] The preparation method is exactly the same as that of the oxidized resveratrol microcapsule-1, except for the wall material and carrier oil of the oxidized resveratrol microcapsule, which are shown in Table 1.
[0062] Among them, the only difference in the wall material type of oxidized resveratrol microcapsule-19 is that it only contains β-glucan-1.
[0063] In the oxidized resveratrol microcapsules-20, only the type of wall material is different. The wall material is a mixture of β-cyclodextrin, chitosan, gum arabic, and maltodextrin, all of which are commercially available products. The ratio of maltodextrin: chitosan: gum arabic: β-cyclodextrin is 2:1:3:1.
[0064] In Oxidized Resveratrol Microcapsules-21, only the type of carrier oil is different, containing only sunflower oil.
[0065] Table 1
[0066]
[0067]
[0068]
[0069] Examples and Comparative Examples
[0070] The present application provides a whitening composition, the components and weight portions of the whitening composition are shown in Table 2-3, and the preparation method of the whitening composition is as follows: resveratrol oxide microcapsules, gentiana yunnanensis extract, mullein extract, and lupin extract are weighed according to weight, and if there are no relevant components, no relevant components are added, and the whitening composition is obtained by mixing them evenly.
[0071] Table 2
[0072]
[0073]
[0074]
[0075] Table 3
[0076]
[0077]
[0078] Application Examples
[0079] The application examples of the present invention provide an eye cream, the components (mass percentage) of the eye cream are shown in Table 4; wherein the compositions in Application Examples 1-19 are respectively the whitening compositions prepared in Examples 1-19; the whitening compositions in Comparative Application Examples 1-14 are respectively the whitening compositions prepared in Comparative Examples 1-14; for example, the whitening composition used in Application Example 1 is the whitening composition in Example 1, the whitening composition used in Application Example 5 is the whitening composition in Example 5, the whitening composition used in Application Example 15 is the whitening composition in Example 15, and so on; the whitening composition used in Application Example 20 is the whitening composition prepared in Example 1.
[0080] Table 4
[0081]
[0082] The preparation method of the eye cream provided in Application Example 1 comprises the following steps:
[0083] (1) Mix the humectant and thickener with water, heat to 85±2°C, and homogenize at 1200 rpm for 4 minutes. After homogenization, keep the mixture warm for later use to obtain prefabricated component A.
[0084] (2) Mix the emulsifier, heat to 85±2°C, and homogenize at 1200 rpm for 4 minutes. After homogenization, keep warm and set aside to obtain prefabricated component B;
[0085] (3) Mix the preservatives and heat to 60±2°C to melt to obtain prefabricated component C;
[0086] (4) Heat the preformed component A to 80±2°C, add the preformed component B at a speed of 250 rpm, stir and mix, then cool to 60±2°C, add the preformed component C at a speed of 250 rpm, stir and mix, then cool to 40°C, add the whitening composition and continue stirring for 8 minutes, finally add the remaining pH adjuster to adjust the pH to 6.0, stop stirring, discharge, and obtain eye cream.
[0087] The preparation methods of the remaining application examples are the same as that of application example 1, except that no relevant components are added.
[0088] Performance test-1 loading rate and encapsulation rate test
[0089] The present invention investigates the encapsulation efficiency and loading rate of oxidized resveratrol microcapsules 1-21, specifically comprising the following steps:
[0090] 1. Loading rate: Weigh 50.0 mg of oxidized resveratrol microcapsules, and record the mass as m t , add 20mL of methanol, ultrasonically extract at 20℃ for 20min, then centrifuge to obtain the supernatant at 8000rpm, dilute the supernatant to 25mL, and calculate the mass of oxidized resveratrol by HPLC quantitative detection, recorded as m o ; Then calculate the load rate according to the formula, load rate = (m o / m t )×100%, and record the calculated load rate in Table 5;
[0091] 2. Encapsulation efficiency: According to the above loading rate test method, m o 50.0 mg of oxidized resveratrol microcapsules were weighed and added to 20 mL of methanol. The mixture was vortexed and extracted at 20°C for 10 seconds. The supernatant was then centrifuged at 8000 rpm to obtain a volume of 25 mL. The mass of oxidized resveratrol was calculated by HPLC quantitative detection, which was recorded as m s Then the encapsulation efficiency was calculated according to the formula: Encapsulation efficiency = (m o -m s ) / m o × 100%, and the calculated encapsulation efficiency is recorded in Table 5.
[0092] Table 5
[0093]
[0094]
[0095] As can be seen from the above table, the oxidized resveratrol microcapsules prepared by selecting specific wall materials and specific carrier oils in the present invention have a loading rate of more than 10.5% and an encapsulation rate of more than 90%.
[0096] From the comparison of oxidized resveratrol microcapsules 1-4 and oxidized resveratrol microcapsules 15-16, it can be seen that the weight ratio of the core material, wall material and carrier oil in the preparation process of oxidized resveratrol microcapsules will affect the loading rate and encapsulation efficiency of the oxidized resveratrol microcapsules. When the weight ratio of the core material, wall material and carrier oil is core material: wall material: carrier oil = 1: (2-4): (2-5), the loading rate and encapsulation efficiency are higher.
[0097] Comparison of oxidized resveratrol microcapsules 1, oxidized resveratrol microcapsules 5-7, and oxidized resveratrol microcapsules 17-18 shows that when the weight ratio of cerium oxide to β-glucan in the wall material is 1:(1-3), the loading rate and encapsulation efficiency are higher.
[0098] From the comparison between oxidized resveratrol microcapsules 1 and oxidized resveratrol microcapsules 8-10, it can be seen that when the weight ratio of the juniper fruit oil to the sunflower seed oil is 1:(3-4), the loading rate and encapsulation efficiency are higher.
[0099] From the comparison between oxidized resveratrol microcapsules 1 and oxidized resveratrol microcapsules 11-14, it can be seen that the type of the wall material will affect the loading rate and encapsulation efficiency. When the average particle size of the cerium oxide is 0.2-3 μm, the loading rate and encapsulation efficiency are higher.
[0100] Performance Test-2 Stability
[0101] The present invention investigates the stability of oxidized resveratrol microcapsules 1-21, specifically comprising the following steps:
[0102] Weigh 3 portions of oxidized resveratrol microcapsules 1-21, spread them flatly on a watch glass, 2g each, and place them in an environment of 4°C, 25°C, and 50°C, with humidity controlled at 65% and 15W light on. Then, the mass of oxidized resveratrol was measured at 0 and 28 days. T0 、m T28 , the detection method is the same as m o The retention rate of oxidized resveratrol was calculated as follows: T28 / m T0 ×100%; the test results for 28 days are shown in Table 6;
[0103] Table 6
[0104]
[0105] As can be seen from the above table, the oxidized resveratrol microcapsules prepared by selecting specific wall materials and specific carrier oils in the present invention have a retention rate of more than 80% for oxidized resveratrol at 4°C, 25°C and 50°C, and can maintain good stability.
[0106] A comparison of oxidized resveratrol microcapsules 1-4 and oxidized resveratrol microcapsules 15-16 shows that the weight ratio of the core material, wall material and carrier oil in the preparation process of oxidized resveratrol microcapsules affects the retention rate of the oxidized resveratrol microcapsules. When the weight ratio of the core material, wall material and carrier oil is core material: wall material: carrier oil = 1: (2-4): (2-5), the retention rate of oxidized resveratrol is higher and the stability is better.
[0107] Comparison of oxidized resveratrol microcapsules 1, oxidized resveratrol microcapsules 5-7, and oxidized resveratrol microcapsules 17-18 shows that when the weight ratio of cerium oxide to β-glucan in the wall material is 1:(1-3), the retention rate of oxidized resveratrol is higher and the stability is better.
[0108] From the comparison between oxidized resveratrol microcapsules 1 and oxidized resveratrol microcapsules 8-10, it can be seen that when the weight ratio of the juniper fruit oil to the sunflower seed oil is 1:(3-4), the retention rate of oxidized resveratrol is higher and the stability is better.
[0109] From the comparison between oxidized resveratrol microcapsules 1 and oxidized resveratrol microcapsules 11-14, it can be seen that the type of the wall material will affect the retention rate. When the average particle size of the cerium oxide is 0.2-3 μm, the retention rate of oxidized resveratrol is higher and the stability is better.
[0110] Performance Test-3 Skin Penetration Test
[0111] The present invention investigates the skin permeability of oxidized resveratrol microcapsules 1-21, specifically comprising the following steps:
[0112] Experimental method: In vitro pig skin testing was used, and the exposed skin area in the diffusion cell was 1.5 cm 2 , the volume of the receiving chamber is 5.0mL. A phosphate buffer solution with a pH of 5.8 and anhydrous ethanol with a volume ratio of 50:50 was used as the receiving solution. Weigh the oxidized resveratrol microcapsules 1-21 respectively, add an appropriate amount of pure water, and then stir at room temperature to prepare a 1% w / v corresponding emulsion at a speed of 600rpm, then take 200μL of the corresponding emulsion and apply it evenly on the skin, and cover it with a film to prevent evaporation. The transdermal absorption of oxidized resveratrol at different time points was tested by HPLC, and the time to reach the maximum cumulative penetration (in h) and the maximum cumulative penetration (in μg / cm 2 The longer the time to reach the maximum cumulative permeation amount, the slower the release of the microcapsule; the larger the maximum cumulative permeation amount, the better the skin permeability of the microcapsule. The results are shown in Table 7 below.
[0113] Table 7
[0114]
[0115]
[0116] As can be seen from the above table, the oxidized resveratrol microcapsules prepared by selecting specific wall materials and specific carrier oils in the present invention can achieve a good sustained-release effect and have good skin permeability.
[0117] A comparison of oxidized resveratrol microcapsules 1-4 and oxidized resveratrol microcapsules 15-16 shows that the weight ratio of the core material, wall material and carrier oil in the preparation process of oxidized resveratrol microcapsules affects the sustained-release effect and skin permeability of the oxidized resveratrol microcapsules. When the weight ratio of the core material, wall material and carrier oil is core material: wall material: carrier oil = 1: (2-4): (2-5), the sustained-release effect and skin permeability of the oxidized resveratrol microcapsules are better.
[0118] Comparison of oxidized resveratrol microcapsules 1, oxidized resveratrol microcapsules 5-7, and oxidized resveratrol microcapsules 17-18 shows that when the weight ratio of cerium oxide to β-glucan in the wall material is 1:(1-3), the oxidized resveratrol microcapsules have better sustained-release effect and skin permeability.
[0119] From the comparison between oxidized resveratrol microcapsules 1 and oxidized resveratrol microcapsules 8-10, it can be seen that when the weight ratio of the juniper fruit oil to the sunflower seed oil is 1:(3-4), the oxidized resveratrol microcapsules have better sustained-release effect and skin permeability.
[0120] Comparison of oxidized resveratrol microcapsules 1 and oxidized resveratrol microcapsules 11-14 shows that the type of wall material affects the sustained release effect and skin permeability. When the average particle size of cerium oxide is 0.2-3 μm, the sustained release effect and skin permeability of the oxidized resveratrol microcapsules are better.
[0121] Performance Test-4 Melanin Production Inhibition Test
[0122] Experimental Methods: The cell line used was mouse melanoma B16F10 cells (Wuhan Saios Biotechnology Co., Ltd.). The test conditions were: incubator temperature 37±1°C, saturated humidity, 5±1% carbon dioxide. Cells were cultured and treated according to grouping, and then tested. The specific test was the determination of cellular melanin content. The test method is as follows:
[0123] (1) The cell suspension was inoculated into a 6-well plate at a culture density of 1×10 6 cells / mL, cultured in DMEM medium (Gibco) for 24 h;
[0124] (2) The blank control group was added with DMEM culture medium containing 0.1% blank application example eye cream, and the sample groups were added with DMEM culture medium containing 0.1% application example and comparison application example eye cream, respectively. After culturing for 24 hours, the cells were collected;
[0125] (3) Determination of cell melanin content: The cells were lysed at 80°C, and then the total amount of melanin in each lysate was measured at a wavelength of 405 nm using an enzyme marker. The melanin content (OD value) was calculated and adjusted based on the total protein concentration. The melanin content of the blank group (solvent control) was normalized and compared with the sample group. The melanin content inhibition rate of each example and comparative example was calculated using the following formula:
[0126] Melanin content inhibition rate (%) = (blank group OD value - sample OD value) / blank group OD value * 100%.
[0127] The results are shown in Table 8.
[0128] Table 8
[0129]
[0130]
[0131] As can be seen from the above table, the eye cream prepared in the application example of the present invention has a melanin content inhibition rate of more than 60%, and has a good effect of lightening pigmented dark circles.
[0132] Performance Test-5 Human skin patch test.
[0133] Thirty volunteers, 15 men and 15 women aged 20-50, were recruited for a closed patch test. Equal amounts (0.020 mL to 0.025 mL) of the test sample (eye cream prepared in the application example, comparative application example, and blank application example) were placed in a specific patch tester. The patch was then applied to the volunteer's arm with hypoallergenic tape, gently pressed to evenly adhere to the skin, and left for 24 hours. The blank control group received distilled water, and the blank application example used an eye cream without the whitening composition. After 24 hours, the patch tester was removed, and skin reactions were observed 0.5, 24, and 48 hours later, with the results recorded. The levels of adverse skin reactions are shown in Table 9 below.
[0134] Table 9
[0135]
[0136] After testing, the eye creams prepared in the application examples of the present invention, the comparative application examples and the blank application examples all showed negative reactions after human patch tests, indicating that they are safe and non-irritating to human skin.
[0137] Performance Test-6 Human Efficacy Tests on Lightening, Repairing and Moisturizing
[0138] Experimental Methods: Asian adult test subjects aged 28-60 with sensitive skin and pigmented dark circles were randomly divided into 35 groups of 5 participants each. The volunteers applied samples (eye creams prepared from Application Examples 1-20, Comparative Application Examples 1-14, and a blank application) around their eyes once daily, morning and evening. Data were collected on day 0 (T0), day 14 (T14), and day 28 (T28).
[0139] After the visit, the volunteers washed their faces with facial cleanser and sat quietly in an air-conditioned room with a temperature of 21±1℃ and a humidity of 50±10% for 30 minutes; the eyes were photographed and analyzed using VISIA-CR, the melanin content MI value of the dark circles was measured using a melanin skin detector Mexameter, and the transepidermal water loss value TEWL of the skin under the eyes was measured using a skin water loss test probe TewaMeter.
[0140] The ability to reduce pigmented dark circles is represented by the improvement in the MI value, and the ability to repair the skin barrier and moisturize is represented by the improvement in the TEWL value. The formula is as follows:
[0141] 14-day improvement rate = (T0-T14) / T0*100%;
[0142] 28-day improvement rate = (T0-T28) / T0*100%;
[0143] The results are shown in Table 10;
[0144] Table 10
[0145]
[0146]
[0147] As can be seen from the above table, the eye cream prepared in the application example of the present invention has an MI value improvement rate of more than 10% and a TEWL value improvement rate of more than 15% after 28 days of use. The oxidized resveratrol microcapsules with a specific structure provided by the present invention, in synergy with Yunnan Gentiana extract, Mullein extract, and Lupin extract, can allow the active ingredients to penetrate deeper into the skin through a slow release mechanism, comprehensively enhance the whitening and repair effects, and play a role in inhibiting post-inflammatory pigmentation and strengthening the fragile skin around the eyes.
[0148] Figure 1 These are the eye condition pictures of volunteers after using the eye creams of the blank application example and application example 1; among them, (a) is the eye condition picture of the volunteer before use, (b) is the eye condition picture of the volunteer after using the eye creams for 14 days, and (c) is the eye condition picture of the volunteer after using the eye creams for 28 days.
[0149] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit the scope of protection of the present invention. Although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that the technical solutions of the present invention may be modified or replaced by equivalents without departing from the essence and scope of the technical solutions of the present invention.
Claims
1. A whitening composition, characterized in that The invention comprises the following components in parts by weight: 1-20 parts of oxidized resveratrol microcapsules, 0.01-2 parts of gentiana yunnanensis extract, 0.1-10 parts of mullein extract, and 0.01-1 part of lupin extract; The oxidized resveratrol microcapsules include a core material, a wall material, a carrier oil and an emulsifier, and the weight ratio of the core material, the wall material, the carrier oil and the emulsifier is core material: wall material: carrier oil: emulsifier = 1: (1-6): (1-8): (0.05-0.2); the core material is oxidized resveratrol; the wall material is a mixture of cerium oxide and β-glucan, the weight ratio of cerium oxide to β-glucan is 1: (0.5-5), and the average particle size of cerium oxide is 0.05-10 μm; the carrier oil is a mixture of juniper fruit oil and sunflower seed oil, and the weight ratio of juniper fruit oil to sunflower seed oil is 1: (0.5-8).
2. The whitening composition according to claim 1, wherein The invention comprises the following components in parts by weight: 5-15 parts of oxidized resveratrol microcapsules, 0.1-0.5 parts of gentiana yunnanensis extract, 1-5 parts of mullein extract and 0.1-0.5 parts of lupin extract.
3. The whitening composition according to claim 1, wherein The mass percentage of the oxidized resveratrol microcapsules in the whitening composition is 50-80%.
4. The whitening composition according to claim 1, wherein The weight ratio of the core material, wall material, carrier oil and emulsifier is core material: wall material: carrier oil: emulsifier = 1: (2-4): (2-5): (0.05-0.2).
5. The whitening composition according to claim 1, wherein The weight ratio of the cerium oxide to the β-glucan is 1:(1-3).
6. The whitening composition according to claim 1, wherein The preparation method of the oxidized resveratrol microcapsules comprises the following steps: (1) Add 30-40°C water to the wall material and stir to dissolve to obtain mixture A; (2) mixing the carrier oil and the emulsifier, heating and homogenizing to obtain a mixture B; (3) mixing oxidized resveratrol and a solvent, adding mixture B, and homogenizing to obtain mixture C; (4) The mixture C and the mixture A are heated and homogenized, spray-dried, and collected and sieved to obtain the oxidized resveratrol microcapsules.
7. Use of the whitening composition according to any one of claims 1 to 6 in the preparation of skin products.
8. A skin care product, characterized in that: The skin product comprises the whitening composition according to any one of claims 1 to 6.
9. The skin care product according to claim 8, wherein The skin products include one of lotion, emulsion, cream, eye cream, eye mask, essence and spray.
Citation Information
Patent Citations
Slow-release whitening composition as well as preparation method and application thereof
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Resveratrol composition, preparation method and application thereof
US20230330029A1