A composition based on a combination of centella asiatica extract and olea europaea extract and its use in a facial mask
By modifying the combination of Centella asiatica extract and olive extract, a mask sheet of nano-sized liposomes and nanocrystals was prepared, which solved the problems of insufficient transdermal absorption rate and stability, and achieved long-lasting anti-inflammatory and antioxidant effects and excellent user experience.
Patent Information
- Application Number
- CN202510679795.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-05-26
- Publication Date
- 2026-02-10
- Estimated Expiration
- 2045-05-26
AI Technical Summary
Existing compositions containing Centella asiatica extract and olive extract are insufficient in terms of transdermal absorption and stability, resulting in the inability of the active ingredients to penetrate effectively and achieve long-lasting sustained release.
By combining modified Centella asiatica extract and olive extract, and utilizing modified olive dispersion, nano-titanium dioxide dispersion, chitosan quaternary ammonium salt, hyaluronic acid, and other ingredients, a mask fabric with nano-scale liposomes and nanocrystals is prepared using a specific process, forming a multi-level dispersion system that enhances the stability of the ingredients and transdermal absorption.
It significantly improves the transdermal absorption rate and stability of Centella Asiatica extract and olive extract, enhances anti-inflammatory and antioxidant effects, improves the moisturizing properties of the mask sheet and the user experience, and is suitable for sensitive skin care.
Abstract
Description
Technical Field
[0001] This invention relates to the field of cosmetic technology, specifically to a composition based on Centella asiatica extract and olive oil extract and its application in facial mask fabric. Background Technology
[0002] Centella asiatica, also known as Gotu Kola or Centella asiatica, is a perennial herbaceous plant belonging to the Apiaceae family. The active ingredients in Centella asiatica extract mainly include asiaticoside, asiaticoside, asiatic acid, quercetin, amino acids, volatile oils, and carotene. Centella asiatica extract can accelerate epidermal cell regeneration, reduce scar formation, relieve skin inflammation such as eczema and dermatitis, reduce redness and itching, enhance skin elasticity, reduce wrinkles, and improve dull skin. Therefore, it is widely used in skincare products such as creams, serums, masks, and gels. Olive leaf extract is an active ingredient extracted from the leaves of the olive tree. Its main active components are oleuropein, hydroxytyrosol, luteolin, apigenin, chlorogenic acid, caffeic acid, and other phenolic acids. It has anti-inflammatory, acne-reducing, antioxidant, anti-aging, and soothing effects, and is also widely used in skincare products such as masks.
[0003] However, the transdermal absorption rate of triterpenoids such as asiaticoside, hydroxyasiaticoside, asiatic acid, and hydroxyasiatic acid in Centella asiatica extract is low; polyphenols such as hydroxytyrosol and oleuropein in olive extract are easily oxidized and deactivated, making long-term sustained release impossible; traditional cotton and silk mask sheets have poor compatibility with hydrophilic extracts (such as asiaticoside) and fat-soluble components (such as oleuropein), resulting in insufficient penetration of active ingredients. Therefore, the transdermal absorption rate and stability of active ingredients in compositions containing Centella asiatica extract and olive extract prepared by existing technologies still need to be improved. Summary of the Invention
[0004] The purpose of this invention is to provide a composition based on Centella asiatica extract and olive oil extract and its application in facial mask fabric, thereby solving the following technical problems:
[0005] The transdermal absorption rate and stability of the active ingredients in existing compositions containing Centella asiatica extract and olive extract are not ideal.
[0006] The objective of this invention can be achieved through the following technical solutions:
[0007] A composition based on Centella asiatica extract and olive extract, comprising the following raw materials: 15-16 parts of modified olive dispersion, 10-10.8 parts of caprylic / capric glyceride, 2.5-2.7 parts of nano-titanium dioxide dispersion, 0.7-0.9 parts of chitosan quaternary ammonium salt, 0.5-0.55 parts of hyaluronic acid, 5-5.5 parts of modified Centella asiatica extract, 5-5.5 parts of Centella asiatica nanocrystals, 300-340 parts of silk fibroin complex, 6-6.6 g of ε-polylysine, and 70-75 parts of deionized water.
[0008] Preferably, the modified olive oil dispersion is prepared as follows:
[0009] A1: Mix phospholipids and cholesterol, then react at 37-40℃, 26-28MPa, and CO2 flow rate of 25L / min for 85-95min. After reducing the pressure to atmospheric pressure by 1-2MPa / min, add citrate buffer, stir for 2-2.2h, and then sonicate for 10-15min. Finally, filter through a 0.2μm polycarbonate membrane to obtain a liposome suspension.
[0010] A2: Add olive leaf extract and trehalose to deionized water and stir for 15-20 min. Then add liposome suspension. Perform high-pressure homogenization three times at 600-800 bar for 2-3 min each time, and then perform high-pressure homogenization three to five times at 1600-1800 bar for 2-3 min each time. Finally, filter the mixture under a sterile nitrogen atmosphere first through a 1.2 μm filter membrane and then through a 0.22 μm filter membrane to obtain modified olive dispersion.
[0011] The ratio of phospholipids, cholesterol, and citrate buffer solution described in A1 is 20-22g: 5-5.5g: 500-550mL;
[0012] The citrate buffer solution described in A1 has a temperature of 45-50℃ and a pH of 5.5;
[0013] The ratio of deionized water, olive leaf extract, trehalose, and liposome suspension described in A2 is 100mL: 5.8-6.2g: 0.28-0.3g: 500mL.
[0014] Preferably, the preparation method of the nano-titanium dioxide dispersion is as follows:
[0015] Nano-titanium dioxide was added to deionized water and then subjected to ultrasonic treatment for 10-15 minutes to obtain a nano-titanium dioxide dispersion.
[0016] The ratio of deionized water to nano-titanium dioxide is 5 mL: 2-2.5 g.
[0017] Preferably, the modified Centella asiatica extract is prepared as follows:
[0018] Disodium EDTA was added to an aqueous solution of glycyrrhizic acid, followed by the addition of Centella asiatica solution while stirring. After stirring for 40-60 min, mannitol and trehalose were added, and the mixture was sonicated for 20-30 min. The mixture was then evaporated under reduced pressure to 180-200 mL at 40-50℃ and -0.09-0.08 MPa. The mixture was then centrifuged at 3000-3500 r / min for 8-10 min, followed by centrifugation at 4800-5000 r / min for 10-20 min. Finally, the mixture was pre-frozen at -50-40℃ for 2-4 h, then freeze-sublimated at -60-50℃ and 0.08 Pa for 20-24 h, and finally desorbed and dried at -35-30℃ and 0.01 Pa for 20-24 h to obtain the modified Centella asiatica extract.
[0019] The ratio of glycyrrhizic acid aqueous solution, disodium EDTA, Centella asiatica solution, mannitol, and trehalose is 180-200 mL: 0.18-0.2 g: 100 mL: 0.08-0.1 g: 0.02-0.03 g;
[0020] The glycyrrhizic acid aqueous solution has a mass fraction of 1%-2%.
[0021] Preferably, the preparation method of the Centella asiatica nanocrystals is as follows:
[0022] Lecithin was added to the Centella asiatica solution, and after high-pressure homogenization, it was pre-frozen at -50 to -40℃ for 2-4 hours. Then, the temperature was increased to 25℃ at 5℃ / h, and then dried at 25℃ and 0.01Pa for 8-9 hours to obtain Centella asiatica nanocrystals.
[0023] The ratio of Centella asiatica solution to lecithin is 100mL: 0.1-0.12g.
[0024] Preferably, the method for preparing the Centella asiatica solution is as follows:
[0025] Centella asiatica extract was added to an ethanol-water solution at 34-36℃ and stirred for 35-40 min at 25-30 MPa, 44-46℃ and CO2 flow rate of 28-30 L / min to obtain a Centella asiatica solution.
[0026] The ratio of the ethanol aqueous solution to Centella asiatica extract is 200mL: 24-30g;
[0027] The ethanol aqueous solution has a mass fraction of 50%-60%.
[0028] Preferably, the silk fibroin composite solution is prepared as follows:
[0029] Silk fibroin was added to an acetic acid solution and stirred for 2-2.2 h. Then, cellulose nanocrystal aqueous dispersion was added and the pH was adjusted to 6.5-7.0 with 0.1 mol / L sodium hydroxide solution. The mixture was homogenized at 9500-10000 r / min for 5-6 min and then allowed to stand at -0.08 MPa for 30-40 min to degas, thus obtaining a silk fibroin composite solution.
[0030] The ratio of the acetic acid solution, silk fibroin, and cellulose nanocrystal aqueous dispersion is 250-300 mL: 12.5-15 g: 80-100 mL;
[0031] The concentration of the acetic acid solution is 0.1 mol / L;
[0032] The cellulose nanocrystal dispersion has a mass fraction of 2%.
[0033] Preferably, the preparation method of the composition based on Centella asiatica extract and olive extract is as follows:
[0034] S1: Add chitosan quaternary ammonium salt to deionized water at 43-47℃ and stir for 15-20 min. Then, while stirring, add hyaluronic acid, followed by modified Centella asiatica extract and Centella asiatica nanocrystals, and disperse at 2000-2500 r / min for 10-12 min. Adjust the pH to 5.5-6.0 with 1 mol / L citric acid aqueous solution to obtain the aqueous phase.
[0035] S2: Mix the modified olive oil dispersion, caprylic / capric glyceride, and nano titanium dioxide dispersion, and then stir at 47-53℃ and -0.08MPa for 30-40 min to obtain the oil phase;
[0036] S3: While homogenizing at 2800-3000 r / min, add the aqueous phase at 38-42℃ dropwise to the oil phase. Continue homogenizing for 20-25 min, then perform ultrasonic treatment for 30-35 min at a power of 380-400W with a pulse of 3s and a pause of 2s. Then, add genipin ethanol solution while stirring. Stir at 36-38℃ for 2-2.2 h, then add sodium thiosulfate solution to obtain the combined solution.
[0037] S4: After mixing the combined solution with the silk fibroin complex solution, ε-polylysine was added, and then the conductivity was adjusted to 800-1000 μS / cm with sodium chloride solution to obtain a composition based on Centella asiatica extract and olive extract.
[0038] Preferably, the ratio of deionized water, chitosan quaternary ammonium salt, hyaluronic acid, modified Centella asiatica extract, and Centella asiatica nanocrystals in S1 is 150mL:1.5-2g:1-1.2g:10-12g:10-12g;
[0039] The ratio of the modified olive oil dispersion, caprylic / capric glyceride, and nano-titanium dioxide dispersion in S2 is 30-35 mL: 20 mL: 5 mL;
[0040] The volume ratio of oil phase, aqueous phase, genipin ethanol solution, and sodium thiosulfate solution in S3 is 55-60 mL: 150 mL: 0.5-0.8 mL: 0.4-0.6 mL;
[0041] The mass fraction of the genipin ethanol solution in S3 is 0.3%;
[0042] The concentration of the sodium thiosulfate solution in S3 is 0.1 mol / L;
[0043] The ratio of the combined solution, silk fibroin complex solution, and ε-polylysine in S4 is 100-110 mL: 300-340 mL: 6-6.6 g;
[0044] The concentration of the sodium chloride solution mentioned in S4 is 0.5 mol / L.
[0045] The application of a composition based on Centella asiatica extract and olive oil extract in a facial mask sheet, the application method being as follows:
[0046] At 0.3-0.4 MPa, the mask sheet is immersed in a composition based on Centella asiatica extract and olive extract at 38-42℃, subjected to pulse treatment for 6-8 min, followed by ultrasonic-assisted impregnation for 4-6 min, and then subjected to gradient drying to obtain a mask sheet containing the composition.
[0047] The ratio of the mask sheet to the composition based on Centella asiatica extract and olive extract is 40-45g: 400-450mL.
[0048] The vacuum degree during pulse processing is -0.01 MPa, and the pulse frequency is 5-10 times / min;
[0049] The gradient drying process is as follows: first, dry at 45-50℃ and 30%-33% relative humidity for 20-30 minutes, and then dry at 64-66℃ and 12%-15% relative humidity for 2-3 hours.
[0050] As a further aspect of the present invention.
[0051] The beneficial effects of this invention are:
[0052] This invention provides a composition based on Centella asiatica extract and olive extract and its application in a facial mask sheet. The invention effectively improves the transdermal absorption rate and stability of the composition based on Centella asiatica extract and olive extract through the following methods.
[0053] (1) The glycyrrhizic acid in the modified Centella asiatica extract of the present invention has significant anti-inflammatory, anti-allergic and antioxidant activities. It can work synergistically with the asiaticoside, hydroxyasiaticoside and other components in Centella asiatica to enhance the anti-aging and repair, soothing and sensitive effects of the composition, inhibit the release of inflammatory factors, reduce skin redness and irritation, and is especially suitable for sensitive skin care. At the same time, glycyrrhizic acid will also encapsulate the effective components such as asiaticoside in Centella asiatica extract to form micelles, which will significantly improve the stability, water solubility, skin permeability and retention capacity of asiaticoside. In the subsequent preparation process, glycyrrhizic acid and chitosan quaternary ammonium salt will also form a complex through electrostatic interaction, which will improve the film-forming properties of the mask cloth, so that the essence forms a tighter moisturizing film on the skin surface and prolong the action time of the active ingredients. The specific ratio of mannitol and trehalose can form a glassy matrix during freeze-drying, preventing the active ingredients of Centella asiatica from being deactivated by ice crystals and maintaining their biological activity; they can also enhance the hygroscopic capacity of the composition by binding with water molecules through hydroxyl groups, thus strengthening the long-lasting moisturizing effect of the mask sheet; and they can reduce the surface tension of cell membranes, promoting the penetration of ingredients such as asiaticoside into the stratum corneum of the skin, thereby increasing the transdermal absorption rate of active ingredients. Centrifugation can effectively remove large molecular impurities such as proteins and polysaccharide aggregates from Centella asiatica extract, improving the purity of active ingredients and reducing the stickiness and potential allergic risks when using the mask sheet.
[0054] (2) The Centella asiatica nanocrystals prepared by the specific process of this invention have a high specific surface area. Compared with traditional Centella asiatica extracts, they can penetrate the stratum corneum of the skin more efficiently and penetrate into the dermis through channels such as hair follicles and sweat glands or intercellular spaces. This allows active ingredients such as asiaticoside and hydroxyasiaticoside to act directly on the deep layers of the skin, improving the bioavailability of anti-inflammatory, repair, and collagen synthesis-promoting effects. The added lecithin can form an amphiphilic coating layer on the surface of the nanocrystals. On the one hand, it avoids crystal aggregation, and on the other hand, it promotes the transmembrane transport of active ingredients through similar compatibility with skin cell membranes. This carrier characteristic allows the Centella asiatica nanocrystals to release active ingredients in a targeted manner when in contact with the skin in the mask fabric, reducing epidermal retention and loss. When Centella asiatica nanocrystals are added to the aqueous phase, they stabilize the system through steric hindrance, inhibiting the aggregation of macromolecules such as hyaluronic acid and chitosan quaternary ammonium salts. Simultaneously, they form a nano-to-submicron multi-level dispersion system with modified Centella asiatica extract, enhancing the composition's resistance to stratification and sedimentation during storage. Furthermore, their combination with modified Centella asiatica extract creates a hydrophilic-lipophilic biphasic delivery system, covering the absorption needs of different polar areas of the skin. They also complement liposome suspensions with a flexible-rigid structure, jointly improving the balanced release of multiple active ingredients in the mask sheet. Centella asiatica nanocrystals also act as a nano-reinforcing filler embedded in the silk fibroin-cellulose nanocrystal network structure, enhancing the tensile strength, flexibility, and liquid retention capacity of the mask sheet. The rigid support of the nanocrystals ensures that the mask sheet maintains a good three-dimensional porous structure even after drying, absorbing more of the essence and releasing it evenly to the skin. The high specific surface area of nanocrystals and the lecithin coating can slow down the release rate of active ingredients, allowing the mask sheet to continuously release Centella Asiatica active ingredients during the application process, avoiding waste or irritation caused by sudden release, and achieving long-lasting anti-inflammatory and antioxidant effects.
[0055] (3) The modified olive oil dispersion of this invention utilizes phospholipids and cholesterol to prepare liposome suspensions under supercritical CO2 conditions, forming a bilayer phospholipid structure similar to a cell membrane. This encapsulates lipophilic components such as oleuropein and hydroxytyrosol from olive leaf extract within the liposomes or membrane layers, protecting phenolic compounds and flavonoids in the olive oil extract from light, heat, and oxidative degradation, especially maintaining their activity during subsequent high-temperature or ultrasonic treatments. The amphiphilic structure of the liposomes allows them to fuse with the stratum corneum of the skin, promoting transdermal absorption of active ingredients. Multi-stage high-pressure homogenization refines the liposome particle size to the nanoscale and uniformly disperses the water-soluble components in the olive oil extract, enabling the nanoscale liposomes to penetrate into the dermis, avoiding retention in the stratum corneum of the epidermis and prolonging the sustained-release time of active ingredients. The negative charge on the surface of the liposomes can also bind to the positive charge sites on the surface of skin cells, targeting and delivering anti-inflammatory components to the inflamed area, reducing capillary dilation and histamine release, and improving redness in sensitive skin. Trehalose prevents liposome aggregation during subsequent freeze-drying or storage, improving the long-term stability of the composition. The mixture of nano-titanium dioxide dispersion and liposome dispersion forms a "liposome-inorganic nanoparticle" composite system. The photoprotective effect of titanium dioxide reduces UV damage to the liposome membrane, indirectly protecting the antioxidant activity of olive extract. The liposome membrane components in the modified olive dispersion form a cross-linked network with chitosan quaternary ammonium salt and hyaluronic acid in the aqueous phase, creating a hydrophobic protective layer on the surface of the mask fabric fibers. This slows down the rate of water evaporation, extending the moisturizing time during application. It also enhances the adsorption of the composition on the fiber surface, preventing essence dripping and improving the user experience. During application, the liposomes gradually rupture as water is released, continuously releasing olive extract, avoiding short-term high-concentration stimulation and prolonging the duration of action.
[0056] (4) The nano-titanium dioxide in the titanium dioxide dispersion of this invention can exert a physical sun protection effect by reflecting, scattering and absorbing ultraviolet rays. Under ultraviolet light irradiation, nano-titanium dioxide will generate a photocatalytic effect, generating hydroxyl radicals and superoxide anions, clearing free radicals on the skin surface, inhibiting oxidative stress reaction, and forming a synergistic effect with the natural antioxidant components of Centella asiatica extract and olive extract, enhancing the anti-aging and repair effect. Nano-titanium dioxide will be embedded in the matrix network of silk fibroin, cellulose nanocrystals and other materials, improving the tensile strength and tear resistance of the mask cloth through particle-polymer interface interaction, while maintaining softness and fit, improving the user experience. The small size of nano-titanium dioxide particles can help open the gaps in the stratum corneum of the skin, promote the transdermal absorption of ingredients such as Centella asiatica extract and olive extract in the mask cloth, and improve the bioavailability of effective ingredients. Chitosan quaternary ammonium salt has cationic antibacterial properties and can form multiple antibacterial protections in synergy with nano-titanium dioxide.
[0057] (5) The silk fibroin in the silk fibroin composite liquid of the present invention has excellent biocompatibility and mechanical strength, and can form a uniform and flexible film, improving the tensile strength and skin adhesion of the mask cloth and reducing essence dripping. Silk fibroin is rich in hydrophilic amino acids such as glycine and alanine, and has excellent moisture absorption and moisturizing ability, which can delay the evaporation of water in the mask and prolong the action time of the active ingredients on the skin surface. The amphiphilic structure of silk fibroin can improve the compatibility of the oil phase and the water phase, reduce phase separation, and enhance the stability of the composite system. Silk fibroin has natural biodegradability and low immunogenicity, which can reduce the irritation of the mask to the skin and is suitable for sensitive skin. The amino acid residues it contains can promote skin cell proliferation and assist in the repair of damaged stratum corneum. The high viscosity and shear thinning properties of the silk fibroin composite liquid can improve the coating performance of the composition, making it easier to evenly impregnate the mask cloth and avoid local liquid accumulation or drying. Cellulose nanocrystals can work synergistically with silk fibroin to form a high-strength, highly stable network structure, further optimizing the physical properties of the mask fabric and ensuring that it maintains its good shape in both dry and wet conditions. The surface hydroxyl groups of cellulose nanocrystals can bind with hydrophilic components such as hyaluronic acid and chitosan quaternary ammonium salts through hydrogen bonding to form a stable network structure, preventing the aggregation of active ingredients and ensuring their uniform distribution in the mask fabric.
[0058] Therefore, the composition based on Centella asiatica extract and olive extract prepared by this invention has excellent transdermal absorption rate and stability. When applied to a mask sheet, this composition can also effectively improve the tensile strength, moisturizing time, skin adhesion, and broad application prospects of the mask sheet. Detailed Implementation
[0059] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0060] Unless otherwise specified, the following information pertains to some of the raw materials used in the following embodiments and comparative examples of this invention:
[0061] Centella asiatica extract was purchased from Hubei Yongkuo Technology Co., Ltd., item number: YK0414; glycyrrhizic acid was purchased from Nanjing Jiadi Biotechnology Co., Ltd., CAS: 1405-86-3; mannitol was purchased from Wuhan Dongkangyuan Technology Co., Ltd., CAS: 87-78-5; trehalose was purchased from Chengdu Mansite Biotechnology Co., Ltd., CAS: 99-20-7; lecithin (soybean lecithin) was purchased from Shanghai Yuanye Biotechnology Co., Ltd., item number: B28313; olive leaf extract (oleuropein) was purchased from Shanghai Yuanye Biotechnology Co., Ltd., item number: B20425; phospholipids were purchased from Jiangsu Yuanzhiyuan Biotechnology Co., Ltd., CAS: 123465-35-0; cholesterol was purchased from Henan Qiande Pharmaceutical Co., Ltd., CAS: 57-88-5; citrate buffer (pH=6.0) was purchased from Shanghai Yunguan Electromechanical Equipment Co., Ltd. Limited Company, Product No.: CP-20516-1; Chitosan Quaternary Ammonium Salt was purchased from Shaanxi Runfeng Biotechnology Co., Ltd., CAS: 9012-76-4; Hyaluronic Acid was purchased from Suzhou Senfeda Chemical Co., Ltd., CAS: 9004-61-9; Nano Titanium Dioxide (particle size 25nm) was purchased from (Klamar) Shanghai Puzhen Biotechnology Co., Ltd.; Caprylic / Capric Glyceryl Acetate was purchased from Hubei Qifei Pharmaceutical Chemical Co., Ltd., Product No.: QF4051; Genipin was purchased from Hubei Xinkang Pharmaceutical Chemical Co., Ltd., Product No.: XK0099; Silk Fiber Protein (Pharmaceutical Grade) was purchased from Wuhan Xinxin Jiali Biotechnology Co., Ltd., CAS: 96690-41-4; Cellulose Nanocrystals were purchased from Shanghai Mairui Biochemical Technology Co., Ltd., Product No.: M81812; Facial Mask Fabric was purchased from Dongguan Zhangmutou Hongji Plastic Chemical Trading Co., Ltd., Product No.: 00120.
[0062] Example 1: A method for preparing a composition based on Centella asiatica extract and olive oil extract and its application in a facial mask sheet is as follows:
[0063] S1: Add 24g of Centella asiatica extract to 200mL of 50% ethanol aqueous solution at 34℃ and stir at 200r / min for 35min at 25MPa, 44℃ and CO2 flow rate of 28L / min to obtain Centella asiatica solution.
[0064] S2: Add 0.18 g of disodium ethylenediaminetetraacetate to 180 mL of 1% glycyrrhizic acid aqueous solution. Then, while stirring at 300 r / min, add 100 mL of Centella asiatica solution dropwise at 1 mL / min. Continue stirring for 40 min, then add 0.08 g of mannitol and 0.02 g of trehalose and sonicate at 200 W for 20 min. Evaporate under reduced pressure at 40℃ and -0.09 MPa to 180 mL, centrifuge at 3000 r / min for 8 min, then centrifuge at 4800 r / min for 10 min. Finally, pre-freeze at -50℃ for 2 h, then freeze-sublimate at -60℃ and 0.08 Pa for 20 h, and finally desorb and dry at -35℃ and 0.01 Pa for 20 h to obtain modified Centella asiatica extract.
[0065] S3: Add 0.1g lecithin to 100mL of Centella asiatica solution, perform high-pressure homogenization at 1500bar for 3 times for 1min each time, pre-freeze at -50℃ for 2h, then raise the temperature to 25℃ at 5℃ / h, and then dry at 25℃ and 0.01Pa for 8h to obtain Centella asiatica nanocrystals.
[0066] S4: Mix 20g phospholipids and 5g cholesterol, then react at 37℃, 26MPa, and CO2 flow rate of 25L / min for 85min. After reducing the pressure to atmospheric pressure by 1MPa / min, add 500mL citrate buffer at pH 5.5 at 45℃, stir at 800r / min for 2h, and then sonicate at 280W for 10min. Finally, filter through a 0.2μm polycarbonate membrane to obtain a liposome suspension.
[0067] S5: Add 5.8g olive leaf extract and 0.28g trehalose to 100mL deionized water and stir at 400r / min for 15min. Then add 500mL liposome suspension. Then perform high-pressure homogenization three times at 600bar for 2min each time, and then perform high-pressure homogenization three times at 1600bar for 2min each time. Finally, filter the mixture under sterile nitrogen atmosphere first through a 1.2μm filter membrane and then through a 0.22μm filter membrane to obtain the modified olive dispersion.
[0068] S6: Add 1.5g of chitosan quaternary ammonium salt to 150mL of deionized water at 43℃ and stir at 600r / min for 15min. Then, while stirring at 600r / min, add 1g of hyaluronic acid in two equal portions (5min interval between each addition). Next, add 10g of modified Centella asiatica extract and 10g of Centella asiatica nanocrystals and disperse at 2000r / min for 10min. Adjust the pH to 5.5 with 1ml / L citric acid aqueous solution to obtain the aqueous phase.
[0069] S7: Add 2g of nano-titanium dioxide to 5mL of deionized water, and then perform ultrasonic treatment at 280W for 10min to obtain nano-titanium dioxide dispersion.
[0070] S8: Mix 30 mL of modified olive oil dispersion, 20 mL of caprylic / capric glyceride and 5 mL of nano titanium dioxide dispersion, and then stir at 400 r / min for 30 min at 47℃ and -0.08 MPa to obtain the oil phase;
[0071] S9: While homogenizing at 2800 r / min, 150 mL of aqueous phase at 38℃ was added dropwise to 55 mL of oil phase at 40 mL / min. After homogenizing for 20 min, ultrasonic treatment was performed for 30 min at 380 W with a pulse of 3 s and a pause of 2 s. Then, while stirring at 300 r / min, 0.5 mL of 0.3% genipin ethanol solution was added. After stirring at 300 r / min at 36℃ for 2 h, 0.4 mL of 0.1 mol / L sodium thiosulfate solution was added to obtain the combined solution.
[0072] S10: Add 12.5g of silk fibroin to 250mL of 0.1mol / L acetic acid solution and stir at 500r / min for 2h. Then add 80mL of 2% cellulose nanocrystal aqueous dispersion and adjust the pH to 6.5 with 0.1mol / L sodium hydroxide solution. Homogenize at 9500r / min for 5min and then let stand at -0.08MPa for 30min to remove bubbles, to obtain silk fibroin composite solution.
[0073] S11: Mix 100 mL of the combined solution with 300 mL of the silk fibroin complex solution, add 6 g of ε-polylysine, and then adjust the conductivity to 800 μS / cm with 0.5 mol / L sodium chloride solution to obtain a composition based on Centella asiatica extract and olive extract.
[0074] S12: At 0.3 MPa, 40 g of facial mask cloth was immersed in 400 mL of a composition based on Centella asiatica extract and olive oil extract at 38 °C. After 6 min of pulse treatment at a vacuum of -0.01 MPa with a pulse frequency of 5 times / min, it was subjected to ultrasonic assisted impregnation at a power of 300 W for 4 min. Then, it was dried at 45 °C and 30% relative humidity for 20 min, and then dried at 64 °C and 12% relative humidity for 2 h to obtain a facial mask cloth containing the composition.
[0075] Example 2: A method for preparing a composition based on Centella asiatica extract and olive oil extract and its application in a facial mask sheet is as follows:
[0076] S1: Add 27g of Centella asiatica extract to 200mL of 55% ethanol aqueous solution at 35℃ and stir at 230r / min for 38min at 28MPa, 45℃ and CO2 flow rate of 29L / min to obtain Centella asiatica solution.
[0077] S2: 0.19 g of disodium ethylenediaminetetraacetate was added to 190 mL of 1.5% glycyrrhizic acid aqueous solution. Then, while stirring at 350 r / min, 100 mL of Centella asiatica solution was added dropwise at 1.5 mL / min. After stirring for 50 min, 0.09 g of mannitol and 0.025 g of trehalose were added, and the mixture was sonicated at 250 W for 25 min. The mixture was evaporated under reduced pressure at 45℃ and -0.085 MPa to 190 mL. It was then centrifuged at 3300 r / min for 9 min and then at 4900 r / min for 15 min. Finally, it was pre-frozen at -45℃ for 3 h, then freeze-sublimated at -55℃ and 0.08 Pa for 22 h, and then desorbed and dried at -33℃ and 0.01 Pa for 22 h to obtain the modified Centella asiatica extract.
[0078] S3: Add 0.11g lecithin to 100mL of Centella asiatica solution, perform high-pressure homogenization at 1500bar for 3 times for 1.5min each time, pre-freeze at -45℃ for 3h, then raise the temperature to 25℃ at 5℃ / h, and dry at 25℃ and 0.01Pa for 8.5h to obtain Centella asiatica nanocrystals;
[0079] S4: Mix 21g of phospholipids and 5.3g of cholesterol, then react at 38℃, 27MPa, and CO2 flow rate of 25L / min for 90min. After reducing the pressure to atmospheric pressure by 1.5MPa / min, add 530mL of citrate buffer at pH 5.5 at 48℃, stir at 830r / min for 2.1h, and then sonicate at 290W for 13min. Finally, filter through a 0.2μm polycarbonate membrane to obtain a liposome suspension.
[0080] S5: Add 6g of olive leaf extract and 0.29g of trehalose to 100mL of deionized water and stir at 450r / min for 18min. Then add 500mL of liposome suspension. Then perform high-pressure homogenization three times at 700bar for 2.5min each time, and then perform high-pressure homogenization four times at 1700bar for 2.5min each time. Finally, filter the mixture under sterile nitrogen atmosphere first through a 1.2μm filter membrane and then through a 0.22μm filter membrane to obtain the modified olive dispersion.
[0081] S6: Add 1.7g of chitosan quaternary ammonium salt to 150mL of deionized water at 45℃ and stir at 700r / min for 18min. Then, while stirring at 700r / min, add 1.1g of hyaluronic acid in two equal portions (5.5min interval between each addition). Next, add 11g of modified Centella asiatica extract and 11g of Centella asiatica nanocrystals and disperse at 2300r / min for 11min. Adjust the pH to 5.7 with 1ml / L citric acid aqueous solution to obtain the aqueous phase.
[0082] S7: Add 2.3g of nano-titanium dioxide to 5mL of deionized water, and then perform ultrasonic treatment at 290W for 13min to obtain a nano-titanium dioxide dispersion.
[0083] S8: Mix 33 mL of modified olive oil dispersion, 20 mL of caprylic / capric glyceride and 5 mL of nano titanium dioxide dispersion, and then stir at 430 r / min for 35 min at 50 °C and -0.08 MPa to obtain the oil phase;
[0084] S9: While homogenizing at 2900 r / min, 150 mL of aqueous phase at 40℃ was added dropwise at 5 mL / min to 58 mL of oil phase. After homogenization for 23 min, ultrasonic treatment was performed for 33 min at 390 W with a pulse of 3 s and a pause of 2 s. Then, 0.65 mL of 0.3% genipin ethanol solution was added while stirring at 330 r / min. After stirring at 310 r / min for 2.1 h at 37℃, 0.5 mL of 0.1 mol / L sodium thiosulfate solution was added to obtain the combined solution.
[0085] S10: Add 13.75g of silk fibroin to 275mL of 0.1mol / L acetic acid solution and stir at 530r / min for 2.1h. Then add 90mL of 2% cellulose nanocrystal aqueous dispersion and adjust the pH to 6.8 with 0.1mol / L sodium hydroxide solution. Homogenize at 9800r / min for 5.5min and then let stand at -0.08MPa for 35min to remove bubbles, to obtain silk fibroin composite solution.
[0086] S11: Mix 105 mL of the combined solution with 320 mL of the silk fibroin complex solution, add 6.3 g of ε-polylysine, and then adjust the conductivity to 900 μS / cm with 0.5 mol / L sodium chloride solution to obtain a composition based on Centella asiatica extract and olive extract.
[0087] S12: At 0.35 MPa, 42.5 g of facial mask cloth was immersed in 425 mL of a composition based on Centella asiatica extract and olive extract at 40 °C. After 7 min of pulse treatment at a vacuum of -0.01 MPa with a pulse frequency of 8 times / min, it was subjected to ultrasonic-assisted impregnation at a power of 330 W for 5 min. Then, it was dried at 47 °C and 32% relative humidity for 25 min, and then dried at 65 °C and 14% relative humidity for 2.5 h to obtain a facial mask cloth containing the composition.
[0088] Example 3: A method for preparing a composition based on Centella asiatica extract and olive extract and its application in a facial mask sheet is as follows:
[0089] S1: Add 30g of Centella asiatica extract to 200mL of 60% ethanol aqueous solution at 36℃ and stir at 250r / min for 40min at 30MPa, 46℃ and CO2 flow rate of 30L / min to obtain Centella asiatica solution.
[0090] S2: Add 0.2g of disodium ethylenediaminetetraacetate to 200mL of 2% glycyrrhizic acid aqueous solution. Then, while stirring at 400r / min, add 100mL of Centella asiatica solution dropwise at 2mL / min. Continue stirring for 60min, then add 0.1g of mannitol and 0.03g of trehalose and sonicate at 300W for 30min. Evaporate under reduced pressure to 200mL at 50℃ and -0.08MPa. Centrifuge at 3500r / min for 10min, then centrifuge at 5000r / min for 20min. Finally, pre-freeze at -40℃ for 4h, then freeze-sublimate at -50℃ and 0.08Pa for 24h, and finally desorb and dry at -30℃ and 0.01Pa for 24h to obtain modified Centella asiatica extract.
[0091] S3: Add 0.12g of lecithin to 100mL of Centella asiatica solution, perform high-pressure homogenization at 1500bar for 2min each time, pre-freeze at -40℃ for 4h, then raise the temperature to 25℃ at 5℃ / h, and dry at 25℃ and 0.01Pa for 9h to obtain Centella asiatica nanocrystals.
[0092] S4: Mix 22g phospholipids and 5.5g cholesterol, then react at 40℃, 28MPa, and CO2 flow rate of 25L / min for 95min. After reducing the pressure to atmospheric pressure by 2MPa / min, add 550mL citrate buffer at pH 5.5 at 50℃, stir at 850r / min for 2.2h, and then sonicate at 300W for 15min. Finally, filter through a 0.2μm polycarbonate membrane to obtain a liposome suspension.
[0093] S5: Add 6.2g olive leaf extract and 0.3g trehalose to 100mL deionized water and stir at 500r / min for 20min. Then add 500mL liposome suspension. Then perform high-pressure homogenization three times at 800bar for 3min each time, and then perform high-pressure homogenization five times at 1800bar for 3min each time. Finally, filter the mixture under sterile nitrogen atmosphere first through a 1.2μm filter membrane and then through a 0.22μm filter membrane to obtain modified olive dispersion.
[0094] S6: Add 2g of chitosan quaternary ammonium salt to 150mL of deionized water at 47℃ and stir at 800r / min for 20min. Then, while stirring at 800r / min, add 1.2g of hyaluronic acid in three equal portions (6min intervals each time). Then add 12g of modified Centella asiatica extract and 12g of Centella asiatica nanocrystals and disperse at 2500r / min for 12min. Adjust the pH to 6.0 with 1ml / L citric acid aqueous solution to obtain the aqueous phase.
[0095] S7: Add 2.5g of nano-titanium dioxide to 5mL of deionized water, and then perform ultrasonic treatment at 300W for 15min to obtain a nano-titanium dioxide dispersion.
[0096] S8: Mix 35 mL of modified olive oil dispersion, 20 mL of caprylic / capric glyceride and 5 mL of nano titanium dioxide dispersion, and then stir at 450 r / min for 40 min at 53℃ and -0.08 MPa to obtain the oil phase;
[0097] S9: While homogenizing at 3000 r / min, 150 mL of aqueous phase at 42℃ was added dropwise to 60 mL of oil phase at 50 mL / min. After homogenization for 25 min, ultrasonic treatment was performed for 35 min at 400 W with a pulse of 3 s and a pause of 2 s. Then, 0.8 mL of 0.3% genipin ethanol solution was added while stirring at 350 r / min. After stirring at 320 r / min at 38℃ for 2.2 h, 0.6 mL of 0.1 mol / L sodium thiosulfate solution was added to obtain the combined solution.
[0098] S10: Add 15g of silk fibroin to 300mL of 0.1mol / L acetic acid solution and stir at 550r / min for 2.2h. Then add 100mL of 2% cellulose nanocrystal aqueous dispersion and adjust the pH to 7.0 with 0.1mol / L sodium hydroxide solution. Homogenize at 10000r / min for 6min and then let stand at -0.08MPa for 40min to remove bubbles, to obtain silk fibroin composite solution.
[0099] S11: Mix 110 mL of the combined solution with 340 mL of the silk fibroin complex solution, add 6.6 g of ε-polylysine, and then adjust the conductivity to 1000 μS / cm with 0.5 mol / L sodium chloride solution to obtain a composition based on Centella asiatica extract and olive extract.
[0100] S12: At 0.4 MPa, 45 g of facial mask cloth was immersed in 450 mL of a composition based on Centella asiatica extract and olive extract at 42 °C. After 8 min of pulse treatment at a vacuum of -0.01 MPa with a pulse frequency of 10 times / min, it was subjected to 6 min of ultrasonic-assisted impregnation with a power of 350 W. Then, it was dried at 50 °C and 33% relative humidity for 30 min, and then dried at 66 °C and 15% relative humidity for 3 h to obtain a facial mask cloth containing the composition.
[0101] Comparative Example 1:
[0102] Compared with Example 1, this comparative example only omits the addition of "0.08g mannitol and 0.02g trehalose" during the preparation of the modified Centella asiatica extract in S2. All other steps and parameters are the same, and will not be repeated here. The final product is a mask sheet containing the composition.
[0103] Comparative Example 2:
[0104] Compared with Example 1, this comparative example only replaces "0.08g mannitol and 0.02g trehalose" added during the preparation of modified Centella asiatica extract in S2 with "0.1g mannitol". All other steps and parameters are the same, and will not be repeated in this comparative example. Finally, a mask cloth containing the composition is obtained.
[0105] Comparative Example 3:
[0106] Compared with Example 1, this comparative example only replaces "10g modified Centella asiatica extract and 10g Centella asiatica nanocrystals" added in the aqueous phase preparation process of S6 with "20g modified Centella asiatica extract". All other steps and parameters are the same, and will not be repeated in this comparative example. Finally, a mask cloth containing the composition is obtained.
[0107] Comparative Example 4:
[0108] Compared with Example 1, this comparative example only replaces "10g modified Centella asiatica extract and 10g Centella asiatica nanocrystals" added in the aqueous phase preparation process of S6 with "20g Centella asiatica nanocrystals". All other steps and parameters are the same, and will not be repeated in this comparative example. Finally, a mask cloth containing the composition is obtained.
[0109] Comparative Example 5:
[0110] Compared with Example 1, this comparative example only replaces the "30 mL modified olive dispersion" added in the oil phase preparation process of S8 with "30 mL deionized water and 1.74 g olive leaf extract". All other steps and parameters are the same, and will not be repeated in this comparative example. Finally, a mask cloth containing the composition is obtained.
[0111] Comparative Example 6:
[0112] Compared with Example 1, this comparative example only replaces the "5 mL nano titanium dioxide dispersion" added in the oil phase preparation process of S8 with "5 mL deionized water". All other steps and parameters are the same, and will not be repeated in this comparative example. Finally, a mask cloth containing the composition is obtained.
[0113] Comparative Example 7:
[0114] Compared with Example 1, this comparative example only replaces "80 mL of 2% cellulose nanocrystal aqueous dispersion" added in the preparation process of silk fibroin composite liquid in S10 with "80 mL of deionized water". All other steps and parameters are the same, and will not be repeated in this comparative example. Finally, a mask cloth containing the composition is obtained.
[0115] Comparative Example 8:
[0116] Compared with Example 1, this comparative example only differs in that the "300mL silk fibroin complex liquid" added in the preparation process of the composition based on Centella asiatica extract and olive extract in S11 is replaced with "300mL deionized water". All other steps and parameters are the same, and will not be repeated in this comparative example. Finally, a mask cloth containing the composition is obtained.
[0117] Comparative Example 9:
[0118] Compared with Example 1, this comparative example only differs in that the "composition based on Centella asiatica extract and olive oil extract" was not added in the preparation process of the mask sheet containing the composition in S12, and was replaced with "deionized water". All other steps and parameters are the same, and will not be repeated in this comparative example. Finally, a mask sheet containing the composition was obtained.
[0119] Performance testing:
[0120] Determination of transdermal absorption rate:
[0121] A Franz diffusion cell (Yuyan Instruments TR-3000) made of quartz glass with an effective diffusion area of 2.8 cm² and a receiving cell volume of 7 mL was prepared. A skin model was obtained from an isolated pig abdomen with a thickness of 0.5 mm and a skin cell viability of 95%, after removing subcutaneous fat and hair, and cleaning with physiological saline. A phosphate buffer solution containing 0.1% sodium dodecyl sulfate at pH 7.4 was used as the receiving solution. The composition containing asiaticoside and oleuropein was diluted to a concentration of 0.5 mg / mL (based on asiaticoside) with pH 5.5 phosphate buffer. Methanol solutions of asiaticoside (10 μg / mL) and oleuropein (20 μg / mL) were then prepared as standard curve controls. The pretreated pig skin was first fixed between the donor and recipient chambers of the diffusion cell, with the stratum corneum facing upwards. Then, 7 mL of the receiving solution was added to the recipient chamber and stirred at 500 rpm for 30 minutes to equilibrate the temperature. Finally, 0.5 mL of the diluted composition was added to the donor chamber, and the diffusion cell was sealed. At time points of 0.5, 1, 2, 4, 6, 8, 12, and 24 hours, 0.5 mL of the receiving solution was aspirated from the recipient chamber, and an equal volume of fresh receiving solution was added simultaneously. The concentrations of asiaticoside and oleuropein in the receiving solution were then analyzed by HPLC. The mobile phase was acetonitrile-2 mmol / L β-cyclodextrin solution (gradient elution: 0-30 min, 21%→23% acetonitrile; 30-60 min, 23%→25% acetonitrile), with a flow rate of 1.0 mL / min and a column temperature of 30 °C. A linear regression equation was established with the concentrations of asiaticoside and oleuropein as the x-axis and the peak area as the y-axis. The corresponding transdermal absorption efficiency (%) was then calculated. The transdermal absorption efficiencies (%) of asiaticoside (glycoside 1) and oleuropein (glycoside 2) in the compositions based on Centella asiatica extract and olive extract prepared in Examples 1-3 and Comparative Examples 1-9 of this invention were determined using this method, and the results are shown in Table 1.
[0122] Stability determination:
[0123] First, the contents (ppm) of asiaticoside and oleuropein in the composition based on Centella asiatica extract and olive extract were determined within 1 hour of preparation. Then, the contents (ppm) of asiaticoside and oleuropein in the composition based on Centella asiatica extract and olive extract were determined after the composition was sealed and placed in an environment of 25°C and 50% relative humidity for 36 hours. The decrease rate (%) of the contents of asiaticoside and oleuropein were then calculated to reflect the stability of the composition; the lower the decrease rate, the better the stability. The stability (%) of asiaticoside (glycoside 1) and oleuropein (glycoside 2) in the compositions based on Centella asiatica extract and olive extract prepared in Examples 1-3 and Comparative Examples 1-9 of this invention were determined according to this method. The results are shown in Table 1.
[0124] Determination of tensile strength:
[0125] Referring to GB / T 24218.3-2010 "Textiles - Nonwovens - Test Methods - Part 3: Determination of Breaking Strength and Elongation at Break (Strip Method)", rectangular specimens with a width of 50 mm and a length of 200 mm were cut from the mask fabric. The specimens were equilibrated at 20°C and 65% relative humidity for 24 hours. Afterward, the pretreated specimens were vertically clamped into a fixture, ensuring the specimens were wrinkle-free and tension-free. The specimens were then stretched at a tensile speed of 100 mm / min until breakage. The following parameters were recorded: breaking strength (unit: N, the maximum load at breakage) and tensile strength (unit: N / 50 mm, breaking strength / 50 mm). The tensile strength (N / 50 mm) of the mask fabrics containing the composition prepared in Examples 1-3 and Comparative Examples 1-9 of this invention were determined using this method. The results are shown in Table 1.
[0126] Determination of moisture loss rate:
[0127] The mask sheet was cut into 5cm × 5cm squares, and the initial weight was recorded. The sample was then immersed in 10mL of deionized water until fully saturated. After immersion, the sample was removed, the surface moisture was blotted dry with filter paper, and the saturated weight was recorded. The sample was then suspended in a constant temperature and humidity chamber at 25℃, 40% relative humidity, and 0.3m / s wind speed. After 2 hours, the final weight of the sample was recorded, and the moisture loss rate of the mask sheet within 2 hours was calculated (in %, the moisture loss rate is the difference between the saturated weight and the final weight / the difference between the saturated weight and the initial weight × 100%). The moisture loss rate (%) of the mask sheets containing the composition prepared in Examples 1-3 and Comparative Examples 1-9 of this invention was determined using this method, and the results are shown in Table 1.
[0128] Skin adhesion:
[0129] Referring to GB / T 2792-1998 "Test Method for 180° Peel Strength of Pressure-Sensitive Adhesive Tapes", the mask sheet was cut into strips 25mm wide, immersed in 10mL of deionized water, and after complete saturation, removed and placed at 25℃ and 50% RH for 2 hours. Then, it was laid flat on a 125mm×50mm silicone rubber (Dow Corning® 732 medical silicone rubber) with a surface roughness of Ra=0.4μm, and rolled three times with a 2kg roller at a speed of 300mm / min to ensure a tight fit between the mask sheet and the skin. After standing for 20 minutes, a tensile testing machine was used to perform a 180° peel at a speed of 300mm / min, and the maximum peel force (unit: N / 25mm) was recorded as the skin adhesion force of the mask sheet. The greater the maximum peel force, the better the skin adhesion of the mask sheet. The skin adhesion force (N / cm) of the mask fabrics containing the composition prepared in Examples 1-3 and Comparative Examples 1-9 of this invention was measured according to this method, and the results are shown in Table 1.
[0130] Table 1: Performance test results of Examples 1-3 and Comparative Examples 1-9
[0131] ;
[0132] Data Analysis:
[0133] As can be seen from Table 1, the composition based on Centella asiatica extract and olive extract prepared in the embodiments of the present invention has excellent transdermal absorption rate and stability of asiaticoside and oleuropein. When this composition is applied to a mask sheet, it can also effectively improve the tensile strength, moisturizing time and skin adhesion of the mask sheet.
[0134] The foregoing has provided a detailed description of one embodiment of the present invention, but this description is merely a preferred embodiment and should not be construed as limiting the scope of the invention. All equivalent variations and modifications made within the scope of the claims of this invention should still fall within the patent coverage of this invention.
Claims
1. The application of a composition based on Centella asiatica extract and olive oil extract in a facial mask sheet, characterized in that, The application method is as follows: S1: Add 24g of Centella asiatica extract to 200mL of 50% ethanol aqueous solution at 34℃ and stir at 200r / min for 35min at 25MPa, 44℃ and CO2 flow rate of 28L / min to obtain Centella asiatica solution. S2: Add 0.18 g of disodium ethylenediaminetetraacetate to 180 mL of 1% glycyrrhizic acid aqueous solution. Then, while stirring at 300 r / min, add 100 mL of Centella asiatica solution dropwise at 1 mL / min. Continue stirring for 40 min, then add 0.08 g of mannitol and 0.02 g of trehalose and sonicate at 200 W for 20 min. Evaporate under reduced pressure at 40℃ and -0.09 MPa to 180 mL, centrifuge at 3000 r / min for 8 min, then centrifuge at 4800 r / min for 10 min. Finally, pre-freeze at -50℃ for 2 h, then freeze-sublimate at -60℃ and 0.08 Pa for 20 h, and finally desorb and dry at -35℃ and 0.01 Pa for 20 h to obtain modified Centella asiatica extract. S3: Add 0.1g lecithin to 100mL of Centella asiatica solution, perform high-pressure homogenization at 1500bar for 3 times for 1min each time, pre-freeze at -50℃ for 2h, then raise the temperature to 25℃ at 5℃ / h, and then dry at 25℃ and 0.01Pa for 8h to obtain Centella asiatica nanocrystals. S4: Mix 20g phospholipids and 5g cholesterol, then react at 37℃, 26MPa, and CO2 flow rate of 25L / min for 85min. After reducing the pressure to atmospheric pressure by 1MPa / min, add 500mL citrate buffer at pH 5.5 at 45℃, stir at 800r / min for 2h, and then sonicate at 280W for 10min. Finally, filter through a 0.2μm polycarbonate membrane to obtain a liposome suspension. S5: Add 5.8g olive leaf extract and 0.28g trehalose to 100mL deionized water and stir at 400r / min for 15min. Then add 500mL liposome suspension. Then perform high-pressure homogenization three times at 600bar for 2min each time, and then perform high-pressure homogenization three times at 1600bar for 2min each time. Finally, filter the mixture under sterile nitrogen atmosphere first through a 1.2μm filter membrane and then through a 0.22μm filter membrane to obtain the modified olive dispersion. S6: Add 1.5g of chitosan quaternary ammonium salt to 150mL of deionized water at 43℃ and stir at 600r / min for 15min. Then, while stirring at 600r / min, add 1g of hyaluronic acid in two equal portions with an interval of 5min between each addition. Next, add 10g of modified Centella asiatica extract and 10g of Centella asiatica nanocrystals and disperse at 2000r / min for 10min. Adjust the pH to 5.5 with 1ml / L citric acid aqueous solution to obtain the aqueous phase. S7: Add 2g of nano-titanium dioxide to 5mL of deionized water, and then perform ultrasonic treatment at 280W for 10min to obtain nano-titanium dioxide dispersion. S8: Mix 30 mL of modified olive oil dispersion, 20 mL of caprylic / capric glyceride and 5 mL of nano titanium dioxide dispersion, and then stir at 400 r / min for 30 min at 47℃ and -0.08 MPa to obtain the oil phase; S9: While homogenizing at 2800 r / min, 150 mL of aqueous phase at 38℃ was added dropwise to 55 mL of oil phase at 40 mL / min. After homogenizing for 20 min, ultrasonic treatment was performed for 30 min at 380 W with a pulse of 3 s and a pause of 2 s. Then, while stirring at 300 r / min, 0.5 mL of 0.3% genipin ethanol solution was added. After stirring at 300 r / min at 36℃ for 2 h, 0.4 mL of 0.1 mol / L sodium thiosulfate solution was added to obtain the combined solution. S10: Add 12.5g of silk fibroin to 250mL of 0.1mol / L acetic acid solution and stir at 500r / min for 2h. Then add 80mL of 2% cellulose nanocrystal aqueous dispersion and adjust the pH to 6.5 with 0.1mol / L sodium hydroxide solution. Homogenize at 9500r / min for 5min and then let stand at -0.08MPa for 30min to remove bubbles, to obtain silk fibroin composite solution. S11: Mix 100 mL of the combined solution with 300 mL of the silk fibroin complex solution, add 6 g of ε-polylysine, and then adjust the conductivity to 800 μS / cm with 0.5 mol / L sodium chloride solution to obtain a composition based on Centella asiatica extract and olive extract. S12: At 0.3 MPa, 40 g of facial mask cloth was immersed in 400 mL of a composition based on Centella asiatica extract and olive oil extract at 38 °C. After 6 min of pulse treatment at a vacuum of -0.01 MPa with a pulse frequency of 5 times / min, it was subjected to ultrasonic assisted impregnation at a power of 300 W for 4 min. Then, it was dried at 45 °C and 30% relative humidity for 20 min, and then dried at 64 °C and 12% relative humidity for 2 h to obtain a facial mask cloth containing the composition.
Citation Information
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