An oil-soluble dissolvable skin care microcapsule and a method for preparing the same

Abstract

The present application provides an oily dissolvable skin care microcapsule and a preparation method thereof, and belongs to the field of medical, dental or cosmetic preparations. The core material and the wall material; the core material includes coenzyme Q10, tocopherol or its derivative, orchid root oil, miro oil, and sabina leaf extract; and the wall material includes gelatin and peach gum. The present application takes "antioxidation, collagen promotion, and barrier repair" as the core logic, and the component collocation is clear in hierarchy: coenzyme Q10 and tocopherol are directly used as core antioxidants to resist the root cause of aging; the orchid oil and sabina leaf extract form a two-way regulation of collagen, further enhancing the ability to promote collagen synthesis; the miro oil and orchid root oil are compounded to enhance the skin resistance by repairing the barrier and resisting inflammation; and a multi-dimensional anti-aging network is formed.

Description

Technical Field

[0001] This invention belongs to the field of medical, dental or cosmetic formulations, and particularly relates to an oil-soluble skin care microcapsule and its preparation method. Background Technology

[0002] Oil-soluble skincare microcapsules are microcapsules that encapsulate oily skincare active ingredients, such as various plant oils, fatty acid esters, and fat-soluble vitamins, within tiny capsule structures. These microcapsules typically have nanoscale or microscale dimensions and can dissolve under specific conditions, releasing the oily components inside. Their outer shell is generally made of natural or synthetic polymers, such as starch and its derivatives, cellulose and its derivatives, gelatin, and gum arabic. These materials possess good biocompatibility and stability, protecting the internal oily components from external environmental factors (such as oxygen, light, and moisture), preventing oxidation, degradation, or volatilization, extending the shelf life of skincare ingredients, and improving the dispersibility and solubility of oily components in skincare products.

[0003] In skincare, the effectiveness of oil-soluble microcapsules lies primarily in their unique dissolving properties. When a microcapsule comes into contact with oils on the skin's surface or a specific solvent in a skincare product, its outer shell gradually dissolves, slowly releasing the encapsulated oily skincare ingredients. These oily ingredients can quickly penetrate the stratum corneum, providing moisturizing, hydrating, and antioxidant benefits. For example, oil-soluble microcapsules encapsulating vitamin E release vitamin E upon dissolution, which can effectively eliminate free radicals in the skin and delay skin aging; microcapsules encapsulating olive oil replenish the skin's oils, strengthen the skin's barrier function, and prevent moisture loss.

[0004] The advantages of oil-soluble skincare microcapsules are: Improved stability of skincare ingredients: Effectively isolates oil-based skincare ingredients from external environmental influences, preventing deterioration and ensuring the product maintains its efficacy within its shelf life. Precise release: Dissolves under specific conditions according to design, achieving slow and precise release of oil-based ingredients, allowing them to work more fully and enhancing skincare effects. Improved user experience: Microcapsules improve the texture and feel of oil-based ingredients in skincare products, making them easier to apply and absorb, avoiding the greasy feeling that traditional oil-based ingredients may cause.

[0005] Oil-soluble skincare microcapsules have broad application prospects in the skincare industry. They can be used in various skincare products such as lotions, creams, serums, and masks. With the increasing demands for efficacy and safety in skincare products, and the continuous development of nanotechnology, materials science, and other related fields, the preparation technology of oil-soluble skincare microcapsules will be continuously optimized, and their performance will be continuously improved. This is expected to bring people a higher quality and more efficient skincare experience, and drive the skincare industry towards a greener and smarter direction. Summary of the Invention

[0006] The purpose of this invention is to provide an oil-soluble skin-care microcapsule and its preparation method, which achieves good effects in promoting collagen production, anti-aging, and anti-oxidation through different core material combinations. A skin-care microcapsule includes a core material and a wall material; The mass ratio of the core material to the wall material is at least 1:1.2; The core material comprises the following components by weight: Coenzyme Q10 0.10-0.15 Tocopherol or its derivatives, 0.1-0.3%. Vetiver root oil 2.0-3.0 Myrothamnus flavescentis oil 0.3-0.5 0.5-1.0g of *Sophora flavescens* leaf extract.

[0007] Preferably, the core material further includes the following components: Antioxidant 0.05-0.10, including but not limited to butylated hydroxyanisole, butylated hydroxytoluene, propyl gallate, etc.

[0008] Chelating agent 0.01-0.03, wherein the chelating agent is tetrasodium glutamate diacetate or hydroxyethylidene diphosphonic acid.

[0009] Skin feel modifier 0.5-2, wherein the skin feel modifier is at least one of the following components: glycerin, panthenol, squalane, caprylic / capric triglyceride.

[0010] Preferably, the wall material is a gelatin and peach gum composite; the mass ratio of gelatin to peach gum is 1: at least 0.8; the Bloom value of the gelatin is ≥180; and the transparency of the peach gum is ≥90%.

[0011] Another object of the present invention is to provide a method for preparing the aforementioned skin care microcapsules, comprising the following steps: S1: Dissolve the wall material in water, with a total concentration of 2-4%, and stir until completely dissolved to obtain a wall material solution; S2: Add the core material to the wall material solution and homogenize it at ≤20℃ and ≥600 bar pressure to obtain an emulsion; S3: Adjust the pH of the emulsion to 4.0±0.2 in a constant temperature water bath, and continue stirring until microcapsules appear in suspension; S4: The emulsion is cooled and solidified into microcapsules, and then the wet microcapsules are collected; S5: After drying, the wet microcapsules become skin care microcapsules.

[0012] Preferably, in step S2, Add 0.5-1% emulsifier by weight of the core material.

[0013] Preferably, in step S3, The temperature should be controlled within 40±1℃ and the stirring speed should be ≤600rpm.

[0014] Preferably, in step S4, Cool to ≤10℃ and adjust pH to 6.5±0.5; add 10%~20% of gelatin transaminase by weight.

[0015] A third objective of this invention is to provide the application of the aforementioned skincare microcapsules in the preparation of cosmetics, including but not limited to dosage forms such as serums, creams, lotions, and lyophilized powders.

[0016] The function of the core material used in this invention is as follows: 1. Coenzyme Q10 is a naturally occurring fat-soluble antioxidant found in human cells and a key substance in mitochondrial energy metabolism. As a mitochondrial energy activator, it enhances skin metabolism by increasing the efficiency of cellular ATP synthesis; at the same time, as a potent fat-soluble antioxidant, it neutralizes free radicals and inhibits lipid peroxidation, forming a synergistic regenerative cycle with tocopherol to delay photoaging damage.

[0017] 2: Tocopherol or its derivatives mainly block the lipid oxidation chain reaction, protect cell membrane integrity, enhance skin barrier function, and reduce transepidermal water loss (TEWL). When combined with Myrothamnus flabellifolia oil, it can activate the Nrf2 pathway and enhance the activity of endogenous antioxidant enzymes such as superoxide dismutase (SOD).

[0018] 3. The core active ingredient in vetiver root oil is vetivenol, which reduces collagen degradation by inhibiting the expression of collagenase MMP-1; it also regulates the TGF-β signaling pathway, directly promoting the synthesis of type I collagen. Furthermore, as a solvent, it can enhance the transdermal absorption of lipid-soluble active ingredients (such as Q10).

[0019] 4. Myrothamnus flabellifolia oil contains ergothioneine analogues and trehalose derivatives, which effectively scavenge hydroxyl radicals; activate the autophagy mechanism to clear damaged proteins; and synergistically inhibit the NF-κB inflammatory pathway with senna leaf extract to reduce UV-induced photoaging damage.

[0020] 5. Barosma betulina leaf extract contains bakuchiol, which can inhibit elastase and prevent elastic fiber breakage; regulate TRPV1 receptor sensitivity and alleviate stimulation response; and synergistically reduce the release of inflammatory factors such as prostaglandin E2 (PGE2) with vetiver oil.

[0021] 6. Antioxidants: These synthetic antioxidants primarily protect the stability of the formulation. The core material contains various unsaturated oils, which are prone to rancidity and discoloration due to oxidation. Adding antioxidants allows them to preferentially react with free radicals, protecting core active ingredients such as Coenzyme Q10 and tocopherol from premature consumption.

[0022] 7. Chelating agents: Trace amounts of metal ions (such as iron and copper) may be present in the skin environment and skincare product ingredients. These ions can catalyze oxidation reactions (such as the Fenton reaction), accelerating the degradation of active ingredients. Chelating agents, by forming stable complexes with metal ions, block their catalytic effect and further enhance the stability of the formulation.

[0023] 8. Skin feel modifiers: These ingredients mainly optimize the product user experience, such as enhancing moisturizing effects, improving skin feel, and helping to repair the skin barrier.

[0024] This invention is based on the core logic of "antioxidant, collagen promotion, and barrier repair," with a clear layering of ingredients: Coenzyme Q10 and tocopherol act as core antioxidants to directly combat the root cause of aging (free radical damage); Vetiver oil (promotes synthesis) and Senna leaf extract (prevents degradation) form a bidirectional regulation of collagen, further enhancing the ability to promote collagen synthesis; Myrothamnus flabellifolia oil and Vetiver root oil are combined to enhance skin resistance through barrier repair and anti-inflammation; thus forming a multi-dimensional anti-aging network.

[0025] To address the issue of easy oxidation of oils and active ingredients in the core material, this invention enhances stability through multiple safeguards: 1. Adding synthetic antioxidants (BHA / BHT / propyl gallate) to directly inhibit oxidation reactions; 2. Using chelating agents to block the catalytic effect of metal ions, ensuring effective release of active ingredients during storage and use; 3. Using a gelatin and gum arabic composite as the wall material, with a gelatin Bloom value ≥180 to ensure encapsulation strength and gum arabic transparency ≥90% to balance appearance and biocompatibility, controlling the slow release of the core material to prevent premature deactivation of active ingredients.

[0026] To avoid potential irritation to sensitive skin from plant essential oils such as vetiver root oil, this invention achieves a slow release effect by encapsulating the oil in a wall material, thereby reducing its irritation. Detailed Implementation

[0027] To better understand the present invention, the present invention will be further described below with reference to specific serial numbers. The terminology used in the serial numbers is for describing specific embodiments and does not constitute a limitation on the scope of protection of the present invention.

[0028] In the specific implementation methods, unless otherwise specified, the experimental methods used are all conventional methods, and the materials and reagents used are all commercially available unless otherwise specified.

[0029] Unless otherwise specified, percentages, % and so on in the specific implementation method are assumed to be mass percentages.

[0030] The raw materials used in this invention are as follows: Vetiver root oil: INCI name is Vetiveria zizanioides root oil.

[0031] Myrothamnus flabellifolia oil: INCI name Myrothamnus flabellifolia leaf extract.

[0032] Barosma betula leaf extract: This is a water-distilled extract of Barosma betula leaves.

[0033] Helichrysum oil: INCI name: Helichrysum italicum flower oil.

[0034] Frankincense oil: INCI name: Boswellia Carterii oil.

[0035] Geranium oil: INCI geranium (PELARGONIUM GRAVEOLENS) leaf oil.

[0036] Gelatin has a Bloom value ≥180; refined peach gum has a transparency ≥90%.

[0037] Example 1 The preparation of skincare microcapsules includes the following steps: S1: Weigh gelatin and peach gum at a mass ratio of 1:0.8, add them to 40℃ deionized water to make a solution with a total wall material concentration of 4%, and stir at 300rpm until completely dissolved to obtain the wall material solution. S2: Add the core material to the wall material solution and add 0.5% of Tween-80 by mass of the core material; homogenize at 20°C and 600 bar until the oil droplet size is ≤1μm; to obtain the emulsion; The mass ratio of core material to wall material is 1:1.2; the core material, calculated by mass parts, includes the following raw materials: Coenzyme Q10 0.10 Tocopherol 0.1 Vetiver root oil 2.0 Myrothamnus flabellifolia oil 0.3 0.5g of *Solanum nigrum* leaf extract; S3: The emulsion is kept at a constant temperature of 40℃ in a water bath and stirred at 600 rpm; 5% acetic acid is added dropwise to adjust the pH to 4.0, and the reaction is allowed to proceed for at least 10 minutes. Then, observe that all microcapsules are suspended and the solution changes from turbid to a semi-transparent gel state, and stop the reaction. S4: Cool the emulsion of S3 to 10℃, adjust the pH to 6.0 using 10% NaOH solution, then add 10% of the gelatin mass of transglutaminase, stir evenly and let it solidify at room temperature for 10 hours; After curing, collect the wet microcapsules using a Buchner funnel and wash them three times with pure water to obtain wet microcapsules. S5: Wet microcapsules are freeze-dried at -40℃ to obtain skin care microcapsules.

[0038] Example 2 The preparation of skincare microcapsules includes the following steps: S1: Weigh gelatin and peach gum at a mass ratio of 1:0.8, add them to 40℃ deionized water to make a solution with a total wall material concentration of 2%, and stir at 300rpm until completely dissolved to obtain the wall material solution. S2: Add the core material to the wall material solution and add 1.0% of Tween-80 by weight of the core material; homogenize at 20°C and 600 bar until the oil droplet size is ≤1μm; to obtain the emulsion; The mass ratio of core material to wall material is 1:1.2; the core material, calculated by mass parts, includes the following raw materials: Coenzyme Q10 0.12 Tocopherol acetate 0.2 Vetiver root oil 2.5 Myrothamnus flabellifolia oil 0.4 0.8g of *Solanum nigrum* leaf extract Butylated hydroxyanisole 0.05 Tetrasodium glutamate diacetate 0.01 Glycerin 0.2 0.3% squalane S3: The emulsion is kept at a constant temperature of 39℃ in a water bath and stirred at 600 rpm; 5% acetic acid is added dropwise to adjust the pH to 3.8, and the reaction is allowed to proceed for at least 10 minutes. Then, observe that all microcapsules are suspended and the solution changes from turbid to a semi-transparent gel state, and stop the reaction. S4: Cool the emulsion of S3 to 10℃, adjust the pH to 6.5 using 10% NaOH solution, then add 15% of the gelatin mass of transglutaminase, stir evenly and let it solidify at room temperature for 10 hours; After curing, collect the wet microcapsules using a Buchner funnel and wash them three times with pure water to obtain wet microcapsules. S5: Wet microcapsules are freeze-dried at -40℃ to obtain skin care microcapsules.

[0039] Example 3 The preparation of skincare microcapsules includes the following steps: S1: Weigh gelatin and peach gum at a mass ratio of 1:0.8, add them to 40℃ deionized water to make a solution with a total wall material concentration of 4%, and stir at 300rpm until completely dissolved to obtain the wall material solution. S2: Add the core material to the wall material solution and add 1.0% of Tween-80 by weight of the core material; homogenize at 20°C and 600 bar until the oil droplet size is ≤1μm; to obtain the emulsion; The mass ratio of core material to wall material is 1:1.2; the core material, calculated by mass parts, includes the following raw materials: Coenzyme Q10 0.15 Tocopherol acetate 0.3 Vetiver root oil 3.0 Myrothamnus flabellifolia oil 0.5 Senna leaf extract 1.0 Butylated hydroxytoluene 0.5 0.5g of propyl gallate Hydroxyethylidene diphosphonic acid 0.03 Panthenol 1.0 Caprylic / capric triglyceride 1.0 S3: The emulsion is kept at a constant temperature of 41℃ in a water bath and stirred at 600 rpm; 5% acetic acid is added dropwise to adjust the pH to 4.2, and the reaction is allowed to proceed for at least 10 minutes. Then, observe that all microcapsules are suspended and the solution changes from turbid to a semi-transparent gel state, and stop the reaction. S4: Cool the emulsion of S3 to 10℃, adjust the pH to 7.0 using 10% NaOH solution, then add 20% of the gelatin mass of transglutaminase, stir evenly, and let it solidify at room temperature for 10 hours. After curing, collect the wet microcapsules using a Buchner funnel and wash them three times with pure water to obtain wet microcapsules. S5: Wet microcapsules are freeze-dried at -40℃ to obtain skin care microcapsules.

[0040] The difference between Examples 4-13 and Example 1 is that the core material in step S2 is as shown in the mass parts in Table 1: Table 1. Composition ratio of skin care microcapsule core material The performance of the skin care microcapsules prepared in the aforementioned embodiments was tested, specifically including DPPH free radical scavenging experiments, in vitro fibroblast experiments, and sustained-release performance experiments: DPPH free radical scavenging experiment: DPPH methanol solution is violet in color and has a strong absorbance at 517 nm. If it binds to the sample, it will reduce the absorbance at 517 nm, thus determining the sample's ability to scavenge DPPH free radicals.

[0041] The specific method is as follows: (1) Take the samples from each embodiment, mix them with sterile water, and prepare an equal volume (2 mL) of the test solution with a concentration of 2% and 2 × 10 4 Mix the mol / L DPPH solution thoroughly (Al); (2) Take equal volumes of anhydrous ethanol (the solvent for the analyte) and 2×10 4 Mix the mol / L DPPH solution thoroughly (A2); (3) Take an equal volume of anhydrous ethanol and mix it with the test solution (A3); (4) After reacting for 40 min, the absorbance values ​​of tubes A1, A2 and A3 were measured at 517 nm.

[0042] The formula for calculating the clearance rate is: Clearance rate (%) = [1 - (A1 - A3) / A2] × 100% The test results are shown in Table 2.

[0043] Table 2 Antioxidant Test Results As shown in Table 2, vetiver root oil had the greatest impact on DPPH scavenging rate; therefore, the scavenging rates of Examples 6 and 7 were still relatively high, but due to the lack of synergistic effect, they were still lower than those of Example 1. Myrothamnus flabellifolia oil and immortelle oil contributed similarly to the scavenging rate, while frankincense oil and basil leaf extract contributed similarly but less than myrothamnus flabellifolia oil. Geranium oil contributed the least to the scavenging rate; therefore, Examples 9 and 12, dominated by geranium oil / basil leaf extract, had the lowest scavenging rates. The remaining combinations had varying scavenging rates, but all were lower than the combination in Example 1.

[0044] In vitro fibroblast experiments: ELISA, by directly quantifying the levels of COL1A1 and elastin secreted by fibroblasts, specifically reflects the promoting effect of active ingredients on the collagen synthesis pathway. The experimental steps include: 1. Cell culture and injury model establishment Human dermal fibroblasts (HDF) were seeded in 96-well plates (density 1×10⁶). 4 (cells / well), incubated at 37°C and 5% CO2 for 24 hours; UVA damage group and experimental group: After washing with PBS and covering with a quartz coverslip, they were irradiated with UVA (10 J / cm²). 2 ); After irradiation, replace the culture medium containing the sample and continue culturing for 48 hours.

[0045] Specifically, there are the following groups: Blank control group (basal culture medium) UVA damage group (10 J / cm) 2 Irradiation) Experimental group (UVA irradiation + samples from each embodiment, diluted to 2%) Positive control group (UVA irradiation + 0.1 μM retinol) 2. Collagen and elastin extraction Intracellular collagen: Lyse cells (RIPA buffer), centrifuge and collect the supernatant; Extracellular collagen: Collect the culture supernatant and filter it through a 0.22 μm filter membrane.

[0046] 3. ELISA Testing Procedure COL1A1 (type I collagen α1 chain) target was detected using the Human COL1A1 ELISA Kit (Abcam, ab210966). Elastin targets were detected using the Human Elastin ELISA Kit (R&D Systems, DEI007).

[0047] 3. Data Analysis and Result Validation Follow the kit instructions for serial dilution and plot a standard curve; then calculate the collagen synthesis amount using the following formula: The results are shown in Table 3 below: Table 3 Results of in vitro fibroblast experiments Sustained-release performance experiment: The sustained-release performance was tested by using the Franz diffusion cell method to simulate skin release, measuring the cumulative release rate over 24 hours and the burst release effect (release rate <15% over 0.5 hours); samples from Examples 1-3 were also measured.

[0048] Some parameters are: Diffusion area: 1.77cm 2 (Standard Pool) Receptor pool volume: 7 mL Artificial membrane: cellulose acetate membrane (0.45μm) Receptor mediator: pH 7.4 PBS buffer and 30% ethanol; The results are shown in Table 4.

[0049] Table 4 Results of sustained-release performance experiments The above detailed description is a specific description of one of the feasible embodiments of the present invention. This embodiment is not intended to limit the patent scope of the present invention. All equivalent implementations or modifications that do not depart from the present invention should be included within the scope of the technical solution of the present invention.

Claims

1. A skincare microcapsule, characterized in that, Includes core and wall materials; The mass ratio of the core material to the wall material is 1:1.2; The core material comprises the following components by weight: Coenzyme Q10 0.10-0.15 Tocopherol or tocopherol acetate 0.1-0.3 Vetiver root oil 2.0-3.0 Myrothamnus flavescentis oil 0.3-0.5 Extract of *Solanum nigrum* leaves: 0.5-1.0g; The Myrothamnus flabellifolia oil is an extract from the leaves of the Myrothamnus flabellifolia tree.

2. The skin care microcapsule according to claim 1, characterized in that, The core material also includes the following components: Antioxidant 0.05-0.

10.

3. The skin care microcapsule according to claim 1, characterized in that, The core material also includes the following components: Chelating agent 0.01-0.03, The chelating agent is tetrasodium glutamate diacetate or hydroxyethylidene diphosphonic acid.

4. The skin care microcapsule according to claim 1, characterized in that, The core material also includes the following components: Skin feel modifier 0.5-2.

5. The skin care microcapsule according to claim 4, characterized in that, The skin feel modifier is at least one of the following ingredients: glycerin, panthenol, squalane, caprylic / capric triglyceride.

6. The skin care microcapsule according to claim 1, characterized in that, The wall material is a composite of gelatin and peach gum; the mass ratio of gelatin to peach gum is 1:0.8; the Bloom value of the gelatin is 180; and the transparency of the peach gum is ≥90%.

7. The method for preparing skin care microcapsules according to any one of claims 1-6, characterized in that, Includes the following steps: S1: Dissolve the wall material in water, with a total concentration of 2-4%, and stir until completely dissolved to obtain a wall material solution; S2: Add the core material to the wall material solution and homogenize it at ≤20℃ and 600 bar pressure to obtain an emulsion; S3: Adjust the pH of the emulsion to 4.0±0.2 in a constant temperature water bath, and continue stirring until microcapsules appear in suspension; S4: The emulsion is cooled and solidified into microcapsules, and then the wet microcapsules are collected; S5: After drying, the wet microcapsules become skin care microcapsules.

8. The method for preparing skin care microcapsules according to claim 7, characterized in that, In step S2, 0.5-1% of the core material mass of emulsifier is added.

9. The method for preparing skin care microcapsules according to claim 7, characterized in that, In step S3, the temperature is controlled within 40±1℃ and the stirring rate is ≤600rpm.

10. The method for preparing skin care microcapsules according to claim 7, characterized in that, In step S4, the temperature is lowered to ≤10℃ and the pH is adjusted to 6.5±0.5; 10%~20% of the gelatin mass of transglutaminase is added.

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