Anti-aging microemulsion essence and preparation method thereof

Abstract

This invention relates to the field of cosmetic technology, and particularly to an anti-aging microemulsion essence and its preparation method. The raw materials, by weight percentage (100%), include: 0.8-1.2% green liquid crystal emulsifier, 0.2-0.4% polyacrylate crosspolymer-6, 0.03-0.08% hydroxyethyl deacetylated chitosan, 5-7% butylene glycol, 1.5-2.5% 1,2-pentanediol, 0.8-1.2% 1,2-hexanediol, 0.03-0.08% disodium EDTA, 0.15-0.25% hydrolyzed sodium hyaluronate, 0.8-1.2% squalane, 0.4-0.6% meadowfoam seed oil, 0.5-0.7% tocopherol, 1.5-2.5% Sichuan pepper fruit extract, 1.5-2.5% edelweiss flower / leaf extract, and 0.8-1.2%... The invention comprises a compound of *Pseudomonas aeruginosa* fermentation product extract, 0.4-0.6% *Inula japonica* extract, 0.2-0.4% *Pseudostellaria heterophylla* extract, 1.2-1.8% *Astragalus membranaceus* root extract, 0.03-0.08% tetrahydropiperine, and the balance being 100% deionized water. This invention utilizes a process strategy combining gradient cooling liquid crystal induction molding with dynamic homogenization rate control to successfully construct and maintain a layered liquid crystal structure in a complex matrix rich in polyols, supplemented by low-speed stirring during the cooling process.

Description

Technical Field

[0001] This invention relates to the field of cosmetic technology, and in particular to an anti-aging microemulsion essence and its preparation method. Background Technology

[0002] Anti-aging microemulsion serum is a daily skincare product for addressing skin's anti-aging needs. It is applied directly to areas of skin requiring anti-wrinkle and firming care, such as the face and neck. Consumers expect this serum to have a refreshing, non-greasy feel, absorb quickly, and provide visible improvement in fine lines and skin firming effects.

[0003] In recent years, liquid crystal emulsification technology has been widely recognized as a promising skincare delivery technology due to its ability to form nanoemulsions with a layered liquid crystal structure highly similar to the lipid bilayer structure of the stratum corneum. This structure can delay or prevent the thinning and rupture of droplet films when droplets meet, demonstrating significant advantages in improving the transdermal absorption efficiency of active ingredients, enhancing skin feel, and increasing emulsion stability. Meanwhile, anti-aging active ingredients derived from natural plants are favored by the industry for their gentleness and multi-target mechanisms of action. Small molecule active peptides, such as Codonopsis pilosula cyclic peptide, possess anti-inflammatory and immunomodulatory activities, and their heat-sensitive structure can be effectively protected through freeze-drying. Extracts from plants such as Zanthoxylum bungeanum, Edelweiss, and Inula japonica contribute differentiated effects such as promoting microcirculation, anti-oxidation, and anti-inflammation. Therefore, current research attempts to combine liquid crystal microemulsion delivery systems with various natural plant extracts to develop serums with both highly efficient transdermal absorption and multiple anti-aging mechanisms.

[0004] For example, application number 202210155833.X discloses a moisturizing and anti-wrinkle face cream with a layered liquid crystal structure and its preparation method. By compounding a specific amount of natural liquid crystal emulsifier with specific solid oils, liquid oils, water, and carbomer, and encapsulating retinol and hydroxypinazone retinoic acid ester in the layered liquid crystal structure, the irritation of retinol can be effectively reduced, while also promoting the penetration of retinol and hydroxypinazone retinoic acid ester into the stratum corneum of the skin, which can effectively improve skin roughness, skin elasticity, and fine lines. Application number 202411968868.0 discloses an anti-aging microemulsion composition, microemulsion, preparation method, and application, which achieves anti-aging by regulating the synthesis of adipocytes and the extracellular matrix, with stronger targeting and specificity. However, this combination scheme faces multiple and interconnected technical obstacles in actual research and development: On the one hand, polyols can form hydrated groups with water through hydrogen bonds. When these hydrated groups enter the liquid crystal layer, these polar small molecules compete for interfacial adsorption sites, causing the molecules that disrupt the liquid crystal structure to arrange themselves in an orderly manner, making the liquid crystal structure loose or even disappear. At the same time, various plant extracts may undergo intermolecular association through hydrophobic interactions or hydrogen bonds during the blending process, further disrupting the packing density and charge state of the interfacial film. The direct consequence of this interference is that the droplet size increases from the nanometer scale to the submicron or even micrometer scale, and the system gradually loses the transparent or translucent appearance that the microemulsion should have, and may even experience layering or precipitation. The destruction of the liquid crystal structure also means that the transdermal absorption advantage is significantly reduced. On the one hand, while the freeze-dried powder made from Codonopsis pilosula extract effectively protects the cyclic peptide active ingredients, the resolution of the freeze-dried powder in an aqueous medium is not a molecular-level dispersion. After resolution, a small amount of high molecular weight polysaccharide impurities and insufficiently depolymerized particles still exist. When this resolution solution is added to the microemulsion host that has formed a liquid crystal structure, these particles lack sufficient compatibility with the liquid crystal film. At best, this leads to a slow increase in the turbidity of the system and a decrease in light transmittance, damaging the clear appearance that the microemulsion essence should have. At worst, it causes phase separation, manifested as visible flocculents or sediments. In addition, the polyglycerol emulsifiers used in the essence generally have low tolerance to mechanical force, and excessively high homogenization speed and cooling stirring speed will affect the formation of the liquid crystal structure.

[0005] Therefore, there is an urgent need to provide an anti-aging microemulsion essence with a clear appearance, long-term stability and high transdermal efficiency, which can effectively combine liquid crystal microemulsion technology with a variety of natural extracts, especially the active components of Codonopsis pilosula derived from freeze-drying. Summary of the Invention

[0006] The purpose of this invention is to provide an anti-aging microemulsion essence and its preparation method. By constructing a nanoscale microemulsion delivery system through liquid crystal emulsification technology, a multi-source natural plant extract and fermentation product are scientifically compounded to achieve multi-target and multi-dimensional anti-aging effects on the skin. This solves the problems of poor stability, clarity and transdermal absorption efficiency of active ingredients in microemulsion systems under the current conditions of high content polyols and complex plant extracts.

[0007] To achieve the above objectives, the present invention adopts the following technical solution: This invention provides an anti-aging microemulsion essence, comprising, by weight percentage (100%): 0.8-1.2% green liquid crystal emulsifier, 0.2-0.4% polyacrylate crosspolymer-6, 0.03-0.08% hydroxyethyl deacetylated chitosan, 5-7% butylene glycol, 1.5-2.5% 1,2-pentanediol, 0.8-1.2% 1,2-hexanediol, 0.03-0.08% disodium EDTA, 0.15-0.25% hydrolyzed sodium hyaluronate, 0.8-1.2% squalane, 0.4-0.6% meadowfoam seed oil, 0.5-0.7% tocopherol, 1.5-2.5% Sichuan pepper extract, 1.5-2.5% edelweiss flower / leaf extract, 0.8-1.2% *Pseudomonas aeruginosa* fermentation product extract, and 0.4-0.6% [unclear - possibly a specific ingredient or ingredient]. Ingredients: Eurasian Inula extract, 0.2-0.4% Codonopsis pilosula extract, 1.2-1.8% Astragalus membranaceus root extract compound, 0.03-0.08% tetrahydropiperine, balance to 100% water.

[0008] Furthermore, the green liquid crystal emulsifier, by mass percentage, comprises: 8-12% sucrose stearate, 18-22% glyceryl stearate, 5-10% sorbitan stearate, 8-12% butanediol, 18-22% sorbitol, and the balance being up to 100% deionized water.

[0009] Furthermore, the preparation method of the green liquid crystal emulsifier includes the following steps: A1. Mix sucrose stearate, glyceryl stearate, sorbitan stearate and butanediol, heat to 70~80℃, stir to dissolve evenly, and form an oil phase mixture; A2. Add sorbitol to deionized water, heat to 70-80℃, stir to dissolve evenly, and form an aqueous mixture. A3. At 70~80℃, slowly add the oil phase mixture to the water phase mixture, homogenize at 5000~8000rpm for 5~10min, and cool to room temperature to obtain the green liquid crystal emulsifier.

[0010] Furthermore, the preparation method of the Sichuan pepper extract includes the following steps: B1. Pulverize the dried Sichuan pepper fruits to 40-60 mesh and put them into the extraction vessel of a supercritical carbon dioxide extraction device for extraction. Control the extraction pressure to 15-35 MPa, temperature to 40-55℃, carbon dioxide flow rate to 8-25 kg / h, and extraction time to 0.5-4 hours to obtain a carbon dioxide fluid carrying the active ingredients of Sichuan pepper. B2. Pass the carbon dioxide fluid carrying the active ingredients of Sichuan pepper obtained in step B1 into the separation vessel, control the pressure of the separation vessel to be 3~8MPa, and the separation temperature to be 30~50℃, so that the active ingredients of Sichuan pepper dissolved in the carbon dioxide fluid are precipitated in the separation vessel and separated from the carbon dioxide gas, and collect the crude extract at the bottom of the separation vessel. B3. Dissolve the crude extract obtained in step B2 in a mixed solvent of butanediol and 1,2-hexanediol, and stir at 40~50℃ to dissolve evenly, so that the active ingredients of Sichuan pepper are fully transferred to the polyol solvent system to obtain a solution containing the active ingredients of Sichuan pepper. B4. Transfer the solution obtained in step B3 to a molecular distillation apparatus and remove low-boiling-point volatile oils and unpleasant odor substances under conditions of 50-60℃ and vacuum degree of 1-10Pa. Collect the heavy phase fraction, then add activated carbon to the solution after molecular distillation, stir and adsorb at 40-50℃ for 1-2 hours, filter to remove activated carbon, and remove pigments and unpleasant odor components to obtain a clear and transparent pepper fruit extract solution. B5. After decolorizing and deodorizing the Sichuan pepper fruit extract solution obtained in step B4, the filtrate is concentrated under reduced pressure at 40~50℃ and -0.06~-0.08MPa to 1 / 5~1 / 3 of the original volume to obtain Sichuan pepper extract.

[0011] Furthermore, the mass ratio of the dried Sichuan pepper fruit, the 1,2-hexanediol, and the butanediol is 1:1:(12~18).

[0012] Furthermore, the preparation method of the Edelweiss flower / leaf extract includes the following steps: The dried flowers / leaves of Edelweiss were pulverized to 40-60 mesh, added to a mixed solvent of butanediol and deionized water, and extracted by reflux at 50-60℃ for 2-4 hours. The filtrate was then filtered. The filtrate was then concentrated under reduced pressure at 50-60℃ and -0.06-0.08MPa to 1 / 4-1 / 2 of its original volume to obtain the Edelweiss flower / leaf extract.

[0013] Furthermore, the mass ratio of the dried edelweiss flowers / leaves, the butanediol, and the deionized water is (4~6):(60~70):(25~35).

[0014] Furthermore, the *Pseudomonas aeruginosa* fermentation product extract, by weight percentage (100%), comprises: 10-15% *Pseudomonas aeruginosa* fermentation broth, 18-22% 1,3-propanediol, 0.5-0.7% xanthan gum, 0.4-0.6% glyceryl caprylate, and the balance being up to 100% deionized water.

[0015] Furthermore, the method for preparing the *Pseudomonas alterniflora* fermentation product extract includes the following steps: Pseudomonas alterniflora was inoculated into a fermentation medium and fermented at 25-30℃ and pH 7.0-7.5 for 24-48 hours. The supernatant of the fermentation product was collected by centrifugation. The supernatant of the fermentation product was concentrated under reduced pressure at 60~70℃ and -0.06~-0.08MPa to 1 / 10~1 / 5 of the original volume to obtain the Pseudomonas alterniflora fermentation broth. Then, 1,3-propanediol, xanthan gum, glyceryl caprylate and deionized water were added and stirred until homogeneous to obtain the Pseudomonas alterniflora fermentation product extract.

[0016] Furthermore, the preparation method of the Eurasian Inula extract includes the following steps: C1. Pulverize dried Eurasian Inula japonica into 40-60 mesh, add 20-70% ethanol aqueous solution, heat and reflux for 1.5-3 hours, filter and collect the filtrate, repeat the extraction of the residue 1-2 times, and combine the filtrates to obtain crude extract. C2. The crude extract from step C1 is concentrated under reduced pressure at 60~70℃ and -0.06~-0.08MPa to 1 / 5~1 / 3 of its original volume to obtain a concentrated solution. C3. The concentrate from step C2 is purified by passing it through a macroporous adsorption resin (D101 or AB-8 type). Impurities are removed by washing with deionized water and low-concentration ethanol in sequence, and then eluted with 50-80% ethanol. The eluent is collected. C4. Add activated carbon to the eluent from step C3, stir at 50-60℃ for 1-2 hours for adsorption and decolorization, filter, add hydroxypropyl cyclodextrin to the filtrate, stir at 40-50℃ to dissolve evenly, and obtain the inclusion complex solution. C5. The inclusion complex solution from step C4 is concentrated under reduced pressure at 50~60℃ and -0.06~-0.08MPa to 1 / 3~1 / 2 of its original volume, then spray-dried and the dried powder is collected to obtain the Eurasian Inula extract. The inlet air temperature of the spray dryer is 160~190℃ and the outlet air temperature is 80~100℃.

[0017] Furthermore, the mass ratio of the dried Eurasian Inula japonica to the hydroxypropyl cyclodextrin is 1:(8~10).

[0018] Furthermore, the preparation method of the Codonopsis pilosula extract includes the following steps: D1. Select dried roots of Codonopsis pilosula, crush them to 40-60 mesh, add 3-10 times the weight of the medicinal material in deionized water, soak for 30-60 minutes, heat to a gentle boil and decoct for 30-90 minutes, filter to obtain the dregs and decoction. D2. Repeat the decoction of the dregs from step D1 once, filter, combine the two decoctions, let stand and cool to room temperature to obtain the extract of Codonopsis pilosula. D3. The extract of Codonopsis pilosula obtained in step D2 is concentrated under reduced pressure at 50~60℃ and -0.06~-0.08MPa to 1 / 5~1 / 3 of the original volume. The precipitate is removed by centrifugation, and the supernatant extract is collected. D4. Add maltodextrin to the supernatant extract from step D3, stir and dissolve evenly to obtain a mixture. Pre-freeze the mixture at -35℃ to -40℃ for 2 to 3 hours, and place it in a freeze dryer. Sublime dry for 10 to 15 hours at a shelf temperature of -5℃ ± 5℃ and a front chamber vacuum of 10 to 30 Pa. Then dry for 5 to 10 hours at a shelf temperature of 20℃ ± 5℃ and a vacuum of 10 to 30 Pa until the moisture content is less than 5% to obtain Codonopsis pilosula cyclic peptide freeze-dried blocks. D5. Crush the freeze-dried block of Codonopsis pilosula cyclic peptide from step D4 through a 40-60 mesh sieve to obtain Codonopsis pilosula extract.

[0019] Furthermore, the mass ratio of the dried root of Codonopsis pilosula to the maltodextrin is 1:(0.8~1.2).

[0020] Furthermore, the compound of Astragalus membranaceus root extract, by mass percentage, comprises: 4-6% Astragalus membranaceus root extract, 4-6% Polygonum cuspidatum extract, 4-6% Citronella pericarp extract, 2.5-3% Forsythia suspensa extract, 0.8-1.2% Centella asiatica extract, 0.4-0.6% p-hydroxyacetophenone, 0.4-0.6% 1,2-hexanediol, 58-62% butylene glycol, and 18-22% deionized water.

[0021] Furthermore, the preparation method of the compound of Astragalus membranaceus root extract includes the following steps: Mix the root extract of Astragalus membranaceus, Polygonum cuspidatum, Citronella pericarp extract, Forsythia suspensa extract and Centella asiatica extract, add butylene glycol and deionized water, and stir at 40~50℃ to dissolve evenly. Then add p-hydroxyacetophenone and 1,2-hexanediol, and continue stirring until completely dissolved to obtain the compound extract of Astragalus membranaceus root.

[0022] Another aspect of the present invention provides a method for preparing an anti-aging microemulsion essence, comprising the following steps: S1. Preparation of Codonopsis pilosula pre-reconstituted solution: Weigh Codonopsis pilosula extract, add 3-5 times the mass of Codonopsis pilosula extract deionized water, stir and reconstitute in a water bath at 30-40℃ for 15-30 minutes to obtain Codonopsis pilosula pre-reconstituted solution; S2. Oil phase preparation: Green liquid crystal emulsifier, squalane, meadowfoam seed oil and tocopherol are heated and dissolved at 70~80℃ and stirred until completely dissolved and homogeneous to form an oil phase; S3. Preparation of aqueous phase one: Dissolve 40-60% of deionized water, butanediol, and disodium EDTA at 70-80°C by heating and stirring at 200-400 rpm until completely dissolved and homogeneous to form aqueous phase one. S4. Preparation of aqueous phase II: Take the remaining deionized water, add polyacrylate crosslinking polymer-6 and hydrolyzed sodium hyaluronate, and stir and disperse evenly at 200~400 rpm under room temperature to form a transparent gel-like aqueous phase II. S5. Liquid crystal emulsification and molding: Under the condition of 70~80℃, the oil phase obtained in step S2 is slowly added to the aqueous phase I obtained in step S3, and homogenized at 5000~8000 rpm for 5~10 min to form a preliminary emulsion. Then, the temperature is gradually reduced to 45~50℃ at a rate of 1~2℃ / min, and low-speed stirring at 300~500 rpm is carried out during the cooling process to obtain the emulsion system. S6. Addition of polymer and polyol: After cooling to 45~50℃, add the aqueous phase II obtained in step S4 to the emulsion system obtained in step S5, and stir at 200~400rpm for 5~8min to make the system uniform, and obtain the microemulsion system. S7. Addition of active ingredients: After thoroughly mixing the pre-reconstituted Codonopsis pilosula solution obtained in step S1 with the compound of hydroxyethyl deacetylated chitosan, Zanthoxylum bungeanum fruit extract, Edelweiss flower / leaf extract, Pseudomonas aeruginosa fermentation product extract, Inula japonica extract, and Astragalus membranaceus root extract, and maintaining the temperature at 45~50℃, add it to the microemulsion system in step S6 to obtain a mixture containing active ingredients. S8. Add tetrahydropiperine, 1,2-pentanediol and 1,2-hexanediol sequentially to the active ingredient mixture obtained in step S7, stir at 200-400 rpm for 10-15 min, then continue to cool to room temperature, reduce the homogenization speed to 200-300 rpm and maintain for 3-5 min to obtain the anti-aging microemulsion essence.

[0023] Compared with the prior art, the present invention has the following beneficial effects: This invention utilizes a process strategy combining gradient cooling liquid crystal-induced molding with dynamic homogenization rate control to successfully construct and maintain a layered liquid crystal vesicle structure in a complex matrix rich in polyols. During the cooling process, low-speed stirring is employed to allow emulsifier molecules sufficient time to align orderly at the oil-water interface, avoiding defects in the liquid crystal vesicle structure caused by rapid cooling. By adjusting the cooling rate and reducing the final high-shear treatment, the risk of mechanical damage to the liquid crystal structure during molding is reduced. Furthermore, pre-reconstituted Codonopsis pilosula freeze-dried powder, mixed with some aqueous components, and then added to the liquid crystal microemulsion system via low-temperature addition and low-shear mixing effectively solves the problem of poor compatibility between the reconstituted Codonopsis pilosula freeze-dried powder particles and the liquid crystal film. Pre-resolution treatment fully hydrates and depolymerizes the cyclic peptide-maltodextrin complex, while low-temperature, low-rate addition reduces interfacial disturbance of the liquid crystal film by microparticles, avoiding phase separation and turbidity increase. Molecular distillation is introduced during the preparation of Sichuan pepper fruit extract to pre-remove volatile oils and unpleasant odor substances, reducing the adsorption load on activated carbon and allowing it to focus more on pigment removal. This ensures decolorization while reducing non-selective loss of active amide components, resulting in an extract with light color, mild odor, and stable active ingredient content. Furthermore, stepwise addition and differentiated process design enable stable coexistence of plant extracts and fermentation products from various sources within the liquid crystal microemulsion system. The product has a clear appearance, uniform particle size, and good shelf-life stability. The liquid crystal structure endows the product with excellent transdermal absorption and sustained-release effects, achieving effective delivery and efficacy expression of anti-aging active ingredients. Attached Figure Description

[0024] To more clearly illustrate the technical solutions in the embodiments of this application or the prior art, the drawings used in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments recorded in this invention. For those skilled in the art, other drawings can be obtained based on these drawings.

[0025] Figure 1 This is a schematic diagram of a polarized light microscope image of the anti-aging microemulsion essence of the present invention.

[0026] Figure 2 This is a schematic diagram of the particle distribution of the anti-aging microemulsion essence of the present invention. Detailed Implementation

[0027] The technical solution of the present invention will be clearly and completely described below with reference to specific embodiments. However, those skilled in the art will understand that the embodiments described below are some embodiments of the present invention, but not all embodiments, and are only used to illustrate the present invention, and should not be regarded as limiting the scope of the present invention. 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. Where specific conditions are not specified in the embodiments, conventional conditions or conditions recommended by the manufacturer shall be followed. Where the manufacturers of reagents or instruments are not specified, they are all conventional products that can be purchased commercially.

[0028] Unless otherwise specified, the post-processing operations described below, such as "mixing", "extraction", "heating", "distillation", "adsorption", "stirring", "filtration", "depressurized concentration", "centrifugation", "drying", and "cooling", can be selected by those skilled in the art based on actual conditions, and are not further limited.

[0029] The raw materials and preparation tools used in the following preparation examples, embodiments, and comparative examples are all commercially available industrial products, including: green liquid crystal emulsifier purchased from Richen Vitamin Co., Ltd.; butylene glycol purchased from Daicel; disodium EDTA purchased from Nolan New Materials (Suzhou) Co., Ltd.; hydrolyzed sodium hyaluronate (molecular weight <5000 Da) purchased from Lushan Freda Pharmaceutical Co., Ltd.; meadowfoam seed oil purchased from Xianting (Guangzhou) Trading Co., Ltd.; polyacrylate crosspolymer-6 purchased from Sepik; squalane purchased from Baikaisheng (Shanghai) Biotechnology Co., Ltd.; tocopherol (vitamin E) purchased from Wilmar Biotechnology (Jiangsu) Co., Ltd.; hydroxyethyl deacetylated chitosan purchased from Beijing Zhongke Houpu Traditional Chinese Medicine Research Institute Co., Ltd.; Sichuan pepper extract purchased from Chenfeng Natural Herbs (Beijing) Technology Co., Ltd.; edelweiss flower / leaf extract purchased from DSM; edelweiss flower / leaf extract purchased from LipoTrue. SL; Eurasian Inula extract was purchased from Shanghai Jiakai Biotechnology Co., Ltd. (a biotechnology company); Codonopsis pilosula extract was purchased from Guizhou Keyichuang Biotechnology Co., Ltd.; Astragalus membranaceus root extract compound was purchased from Tonghua Naibo New Materials Co., Ltd.; Tetrahydropiperine was purchased from Zhengzhou Kema Biotechnology Co., Ltd.; Deionized water was purchased from Shandong Kangmei Pharmaceutical Co., Ltd.

[0030] Preparation Example 1 The preparation method of green liquid crystal emulsifier includes the following steps: A1. Mix 10 parts by weight of sucrose stearate, 20 parts by weight of glyceryl stearate, 8 parts by weight of sorbitan stearate and 10 parts by weight of butanediol, heat to 75°C, stir and dissolve evenly to form an oil phase mixture. A2. Add 20 parts by weight of sorbitol to 32 parts by weight of deionized water, heat to 75°C, stir and dissolve evenly to form an aqueous mixture; A3. At 75°C, the oil phase mixture is slowly added to the water phase mixture, homogenized at 6500 rpm for 8 minutes, and then cooled to room temperature to obtain the green liquid crystal emulsifier.

[0031] Preparation Example 2 The preparation method of Sichuan pepper extract includes the following steps: B1. Pulverize 6 parts by weight of dried Sichuan pepper fruit to 50 mesh and put them into the extraction vessel of a supercritical carbon dioxide extraction device for extraction. Control the extraction pressure at 25 MPa, the temperature at 48℃, the carbon dioxide flow rate at 16 kg / h, and the extraction time at 2.2 h to obtain a carbon dioxide fluid carrying the active ingredients of Sichuan pepper. B2. Pass the carbon dioxide fluid carrying the active ingredients of Sichuan pepper obtained in step B1 into the separation vessel, control the pressure of the separation vessel to 5 MPa and the separation temperature to 40°C, so that the active ingredients of Sichuan pepper dissolved in the carbon dioxide fluid precipitate in the separation vessel and separate from the carbon dioxide gas, and collect the crude extract at the bottom of the separation vessel. B3. Dissolve the crude extract obtained in step B2 in a mixed solvent of 88 parts by mass of butanediol and 6 parts by mass of 1,2-hexanediol, and stir at 45°C until it is completely dissolved, so that the active ingredients of Sichuan pepper are fully transferred to the polyol solvent system to obtain a solution containing the active ingredients of Sichuan pepper. B4. Transfer the solution obtained in step B3 to a molecular distillation apparatus and remove low-boiling-point volatile oils and unpleasant odor substances at 55°C and a vacuum of 6Pa. Collect the heavy phase fraction, then add activated carbon to the solution after molecular distillation and stir and adsorb at 45°C for 1.5 hours. Filter to remove the activated carbon in order to remove pigments and unpleasant odor components and obtain a clear and transparent pepper fruit extract solution. B5. The filtrate of the Sichuan pepper fruit extract solution obtained in step B4 after decolorization and deodorization is concentrated under reduced pressure at 45℃ and -0.07MPa to 1 / 4 of the original volume to obtain the Sichuan pepper fruit extract.

[0032] Preparation Example 3 The preparation method of Edelweiss flower / leaf extract includes the following steps: Five parts by weight of dried Edelweiss flowers / leaves were pulverized to 50 mesh and added to a mixed solvent of 65 parts by weight of butylene glycol and 30 parts by weight of deionized water. The mixture was refluxed at 55°C for 3 hours and filtered to obtain the filtrate. The filtrate was then concentrated under reduced pressure at 55°C and -0.07 MPa to 1 / 3 of its original volume to obtain the Edelweiss flower / leave extract.

[0033] Preparation Example 4 The method for preparing the extract of Pseudomonas alterniflora fermentation product includes the following steps: *Pseudomonas alterniflora* was inoculated into a fermentation medium and fermented at 28°C and pH 7.2 for 36 h. The supernatant of the fermentation product was collected by centrifugation and then concentrated under reduced pressure at 65°C and -0.07 MPa to 1 / 8 of the original volume to obtain *Pseudomonas alterniflora* fermentation broth. 0.12 parts by weight of the *Pseudomonas alterniflora* fermentation broth were taken, and 20 parts by weight of 1,3-propanediol, 0.6 parts by weight of xanthan gum, 0.5 parts by weight of glyceryl caprylate, and 78.78 parts by weight of deionized water were added. The mixture was stirred until homogeneous to obtain the *Pseudomonas alterniflora* fermentation product extract.

[0034] Preparation Example 5 The preparation method of Eurasian Inula extract includes the following steps: C1. Pulverize 10 parts by weight of dried Eurasian Inula japonica to 50 mesh, add 45% ethanol aqueous solution, heat and reflux for 2.2 h, filter and collect the filtrate, repeat the extraction twice with the residue, and combine the filtrates to obtain crude extract. C2. The crude extract from step C1 is concentrated under reduced pressure at 65℃ and -0.07MPa to 1 / 4 of its original volume to obtain a concentrated solution. C3. The concentrate from step C2 is purified by passing it through a macroporous adsorption resin (D101 type). Impurities are removed by washing with deionized water and low-concentration ethanol in sequence, and then eluted with 65% ethanol. The eluent is collected. C4. Add activated carbon to the eluent from step C3, stir at 55°C for 1.5 hours to adsorb and decolorize, filter, add 90 parts by mass of hydroxypropyl cyclodextrin to the filtrate, stir at 45°C to dissolve evenly, and obtain an inclusion complex solution. C5. The inclusion complex solution from step C4 is concentrated to 1 / 3 of its original volume under reduced pressure at 55°C and -0.07 MPa, and then spray-dried (inlet air temperature 175°C, outlet air temperature 90°C). The dried powder is collected to obtain the Eurasian Inula extract.

[0035] Preparation Example 6 The preparation method of Codonopsis pilosula extract includes the following steps: D1. Select 50 parts by weight of dried roots of Codonopsis pilosula, crush them to 50 mesh, add 6 times the weight of the medicinal material in deionized water, soak for 45 minutes, heat to a gentle boil and decoct for 600 minutes, filter to obtain the dregs and decoction. D2. Repeat the decoction of the dregs from step D1 once, filter, combine the two decoctions, let stand and cool to room temperature to obtain the extract of Codonopsis pilosula. D3. The extract of Codonopsis pilosula obtained in step D2 is concentrated under reduced pressure at 55℃ and -0.07MPa to 1 / 4 of the original volume. The precipitate is removed by centrifugation, and the supernatant extract is collected. D4. Add 50 parts by weight of maltodextrin to the supernatant extract from step D3, stir and dissolve evenly to obtain a mixture. Pre-freeze the mixture at -38℃ for 2.5h, and place it in a freeze dryer. Sublime dry for 12h under the conditions of shelf temperature -5℃ and front chamber vacuum degree 20Pa, and then dry for 8h under the conditions of shelf temperature 20℃ and vacuum degree 20Pa until the moisture content is less than 5% to obtain Codonopsis pilosula cyclic peptide freeze-dried block. D5. Crush the freeze-dried block of Codonopsis pilosula cyclic peptide from step D4 through a 50-mesh sieve to obtain Codonopsis pilosula extract.

[0036] Preparation Example 7 The preparation method of the compound extract of Astragalus membranaceus root includes the following steps: Five parts by weight of Astragalus membranaceus root extract, five parts by weight of Polygonum cuspidatum extract, five parts by weight of Citronella pericarp extract, 2.8 parts by weight of Forsythia suspensa extract, and one part by weight of Centella asiatica extract were mixed. Sixty parts by weight of butylene glycol and 20.2 parts by weight of deionized water were added, and the mixture was stirred at 45°C until dissolved. Then, 0.5 parts by weight of p-hydroxyacetophenone and 0.5 parts by weight of 1,2-hexanediol were added, and the mixture was stirred until completely dissolved to obtain the Astragalus membranaceus root extract compound.

[0037] Example 1 An anti-aging microemulsion essence, by weight percentage, comprises the following ingredients: 1.0% green liquid crystal emulsifier, 0.3% polyacrylate crosspolymer-6, 0.05% hydroxyethyl deacetylated chitosan, 6% butylene glycol, 2% 1,2-pentanediol, 1.0% 1,2-hexanediol, 0.05% disodium EDTA, 0.2% hydrolyzed sodium hyaluronate, 1.0% squalane, 0.5% meadowfoam seed oil, 0.6% tocopherol, 2.0% zanthoxylum bungeanum fruit extract, 2.0% edelweiss flower / leaf extract, 1.0% *Pseudomonas aeruginosa* fermentation product extract, 0.5% *Inula japonica* extract, 0.3% *Pseudostellaria heterophylla* extract, 1.5% *Astragalus membranaceus* root extract complex, 0.05% tetrahydropiperine, and 79.95% deionized water.

[0038] A method for preparing an anti-aging microemulsion essence includes the following steps: S1. Preparation of Codonopsis pilosula pre-reconstituted solution: Weigh Codonopsis pilosula extract, add deionized water equivalent to 4 times the mass of Codonopsis pilosula extract, stir and reconstitute in a 35℃ water bath for 22 min to obtain Codonopsis pilosula pre-reconstituted solution; S2. Oil phase preparation: Green liquid crystal emulsifier, squalane, meadowfoam seed oil and tocopherol are heated to 75°C and dissolved, and stirred until completely dissolved and homogeneous to form an oil phase; S3. Preparation of aqueous phase one: Dissolve 50% of deionized water, butanediol, and disodium EDTA at 75°C by heating and stirring at 300 rpm until completely dissolved and homogeneous to form aqueous phase one. S4. Preparation of aqueous phase II: Take the remaining deionized water, add polyacrylate crosslinking polymer-6 and hydrolyzed sodium hyaluronate, and stir and disperse evenly at 300 rpm at room temperature to form a transparent gel-like aqueous phase II. S5. Liquid crystal emulsification and molding: At 75°C, the oil phase obtained in step S2 is slowly added to the aqueous phase I obtained in step S3, and homogenized at 6500 rpm for 8 min to form a preliminary emulsion. Then, the temperature is gradually reduced to 48°C at a rate of 1.5°C / min, and low-speed stirring at 400 rpm is performed during the cooling process to obtain the emulsion system. S6. Addition of polymer and polyol: After cooling to 48°C, add the aqueous phase II obtained in step S4 to the emulsion system obtained in step S5, and stir at 300 rpm for 7 min to make the system uniform, thus obtaining a microemulsion system. S7. Addition of active ingredients: After thoroughly mixing the pre-reconstituted Codonopsis pilosula solution obtained in step S1 with the compound of hydroxyethyl deacetylated chitosan, Zanthoxylum bungeanum fruit extract, Edelweiss flower / leaf extract, Pseudomonas aeruginosa fermentation product extract, Inula japonica extract, and Astragalus membranaceus root extract, and maintaining the temperature at 48°C, add it to the microemulsion system in step S6 to obtain a mixture containing active ingredients. S8. Add tetrahydropiperine, 1,2-pentanediol and 1,2-hexanediol to the active ingredient mixture obtained in step S7 in sequence. Stir at 300 rpm for 12 min, then continue to cool to room temperature and reduce the homogenization speed to 250 rpm for 4 min to obtain the anti-aging microemulsion essence.

[0039] Example 2 An anti-aging microemulsion essence, by weight percentage, comprises the following ingredients: 0.8% green liquid crystal emulsifier, 0.2% polyacrylate crosspolymer-6, 0.03% hydroxyethyl deacetylated chitosan, 5% butylene glycol, 1.5% 1,2-pentanediol, 0.8% 1,2-hexanediol, 0.03% disodium EDTA, 0.15% hydrolyzed sodium hyaluronate, 0.8% squalane, 0.4% meadowfoam seed oil, 0.5% tocopherol, 1.5% Sichuan pepper fruit extract, 1.5% edelweiss flower / leaf extract, 0.8% *Pseudomonas aeruginosa* fermentation product extract, 0.4% *Inula japonica* extract, 0.2% *Pseudostellaria heterophylla* extract, 1.2% *Astragalus membranaceus* root extract complex, 0.03% tetrahydropiperine, and 84.16% deionized water.

[0040] A method for preparing an anti-aging microemulsion essence includes the following steps: S1. Preparation of Codonopsis pilosula pre-reconstituted solution: Weigh Codonopsis pilosula extract, add deionized water equivalent to 3 times the mass of Codonopsis pilosula extract, stir and reconstitute in a 30℃ water bath for 15 min to obtain Codonopsis pilosula pre-reconstituted solution; S2. Oil phase preparation: Green liquid crystal emulsifier, squalane, meadowfoam seed oil and tocopherol are heated to 70°C and dissolved, and stirred until completely dissolved and homogeneous to form an oil phase; S3. Preparation of aqueous phase one: Dissolve 40% of the total amount of deionized water, butanediol, and disodium EDTA at 70°C and stir at 200 rpm until completely dissolved and homogeneous to form aqueous phase one. S4. Preparation of aqueous phase II: Take the remaining deionized water, add polyacrylate crosslinking polymer-6 and hydrolyzed sodium hyaluronate, and stir and disperse evenly at 200 rpm at room temperature to form a transparent gel-like aqueous phase II. S5. Liquid crystal emulsification molding: Under the condition of 70℃, the oil phase obtained in step S2 is slowly added to the aqueous phase I obtained in step S3, and homogenized at 5000 rpm for 10 min to form a preliminary emulsion. Then, the temperature is gradually reduced to 45℃ at a rate of 1℃ / min, and low-speed stirring at 300 rpm is carried out during the cooling process to obtain the emulsion system. S6. Addition of polymer and polyol: After cooling to 45°C, add the aqueous phase II obtained in step S4 to the emulsion system obtained in step S5, and stir at 200 rpm for 5 min to make the system uniform, thus obtaining a microemulsion system. S7. Addition of active ingredients: After thoroughly mixing the pre-reconstituted Codonopsis pilosula solution obtained in step S1 with the compound of hydroxyethyl deacetylated chitosan, Zanthoxylum bungeanum fruit extract, Edelweiss flower / leaf extract, Pseudomonas aeruginosa fermentation product extract, Inula japonica extract, and Astragalus membranaceus root extract, and maintaining the temperature at 45°C, add it to the microemulsion system in step S6 to obtain a mixture containing active ingredients. S8. Add tetrahydropiperine, 1,2-pentanediol and 1,2-hexanediol sequentially to the active ingredient mixture obtained in step S7. Stir at 200 rpm for 10 min, then continue to cool to room temperature. Reduce the homogenization speed to 200 rpm and maintain for 5 min to fix the liquid crystal structure and complete the construction of the microemulsion system, thus obtaining the anti-aging microemulsion essence.

[0041] Example 3 An anti-aging microemulsion essence, by weight percentage, comprises the following ingredients: 1.2% green liquid crystal emulsifier, 0.4% polyacrylate crosspolymer-6, 0.08% hydroxyethyl deacetylated chitosan, 7% butylene glycol, 2.5% 1,2-pentanediol, 1.2% 1,2-hexanediol, 0.08% disodium EDTA, 0.25% hydrolyzed sodium hyaluronate, 1.2% squalane, 0.6% meadowfoam seed oil, 0.7% tocopherol, 2.5% zanthoxylum bungeanum fruit extract, 2.5% edelweiss flower / leaf extract, 1.2% *Pseudomonas aeruginosa* fermentation product extract, 0.6% *Inula japonica* extract, 0.4% *Pseudostellaria heterophylla* extract, 1.8% *Astragalus membranaceus* root extract complex, 0.08% tetrahydropiperine, and 75.71% deionized water.

[0042] A method for preparing an anti-aging microemulsion essence includes the following steps: S1. Preparation of Codonopsis pilosula pre-reconstituted solution: Weigh Codonopsis pilosula extract, add deionized water equivalent to 5 times the mass of Codonopsis pilosula extract, stir and reconstitute in a 40℃ water bath for 15 min to obtain Codonopsis pilosula pre-reconstituted solution; S2. Oil phase preparation: Green liquid crystal emulsifier, squalane, meadowfoam seed oil and tocopherol are heated to 80°C and dissolved, and stirred until completely dissolved and homogeneous to form an oil phase; S3. Preparation of aqueous phase one: Dissolve 60% of the total amount of deionized water, butanediol, and disodium EDTA at 80°C and stir at 400 rpm until completely dissolved and homogeneous to form aqueous phase one. S4. Preparation of aqueous phase II: Take the remaining deionized water, add polyacrylate crosslinking polymer-6 and hydrolyzed sodium hyaluronate, and stir and disperse evenly at 400 rpm at room temperature to form a transparent gel-like aqueous phase II. S5. Liquid crystal emulsification and molding: Under the condition of 80°C, the oil phase obtained in step S2 is slowly added to the aqueous phase I obtained in step S3, and homogenized at 8000 rpm for 5 min to form a preliminary emulsion. Then, the temperature is gradually reduced to 50°C at a rate of 2°C / min, and low-speed stirring at 500 rpm is carried out during the cooling process to obtain the emulsion system. S6. Addition of polymer and polyol: After cooling to 50°C, add the aqueous phase II obtained in step S4 to the emulsion system obtained in step S5, and stir at 400 rpm for 5 min to make the system uniform, thus obtaining a microemulsion system. S7. Addition of active ingredients: After thoroughly mixing the pre-reconstituted Codonopsis pilosula solution obtained in step S1 with the compound of hydroxyethyl deacetylated chitosan, Zanthoxylum bungeanum fruit extract, Edelweiss flower / leaf extract, Pseudomonas aeruginosa fermentation product extract, Inula japonica extract, and Astragalus membranaceus root extract, and maintaining the temperature at 45~50℃, add it to the microemulsion system in step S6 to obtain a mixture containing active ingredients. S8. Add tetrahydropiperine, 1,2-pentanediol and 1,2-hexanediol sequentially to the active ingredient mixture obtained in step S7. Stir at 400 rpm for 10 min, then continue to cool to room temperature. Reduce the homogenization speed to 300 rpm and maintain for 3 min to stabilize the liquid crystal structure and complete the construction of the microemulsion system, thus obtaining the anti-aging microemulsion essence.

[0043] Example 4 An anti-aging microemulsion essence and its preparation method are described. The specific implementation method is the same as in Example 1, except that some raw materials are used: 0.8% green liquid crystal emulsifier and 7% butanediol.

[0044] Example 5 An anti-aging microemulsion essence and its preparation method are described. The specific implementation method is the same as that in Example 1, except that the amount of some raw materials used is 1.2% green liquid crystal emulsifier and 5% butanediol.

[0045] Comparative Example 1 An anti-aging microemulsion essence and its preparation method are described. The specific implementation method is the same as in Example 1, except that no green liquid crystal emulsifier is added.

[0046] Comparative Example 2 An anti-aging microemulsion essence and its preparation method are described. The specific implementation method is the same as in Example 1, except that butylene glycol is not added to the raw materials of the anti-aging microemulsion essence.

[0047] Comparative Example 3 An anti-aging microemulsion essence and its preparation method are described. The specific implementation method is the same as in Example 1, except that no Codonopsis pilosula extract is added.

[0048] Comparative Example 4 An anti-aging microemulsion essence and its preparation method are disclosed. The specific raw materials and their amounts are the same as in Example 1. The difference is that step S1 is omitted, that is, the pre-reconstituted solution of Codonopsis pilosula is not prepared, and the freeze-dried powdered Codonopsis pilosula extract is directly added in step S7.

[0049] Comparative Example 5 An anti-aging microemulsion essence and its preparation method are disclosed. The specific raw materials and their amounts are the same as in Example 1. The difference is that in step S5, gradient cooling is not performed. Instead, the preliminary emulsion is placed directly in an ice-water bath and rapidly cooled to room temperature at a cooling rate of 15°C / min.

[0050] Comparative Example 6 An anti-aging microemulsion essence and its preparation method are disclosed. The specific raw materials and their amounts are the same as in Example 1, except that the homogenization speed in step S5 is increased to 10,000 rpm.

[0051] Comparative Example 7 An anti-aging microemulsion essence and its preparation method are disclosed. The specific raw materials and their amounts are the same as in Example 1. The difference is that the gradient cooling rate in step S5 is too fast, which is 5℃ / min, exceeding the limit of 1~2℃ / min.

[0052] Performance testing: (1) Particle size and polydispersity index (PDI) testing: Refer to ISO 22412:2017 "Particle size analysis—Dynamic light scattering method". Dynamic light scattering method was used to measure the particle size using a Zetasizer Nano ZS nanoparticle size analyzer (Malvin Instruments Ltd., UK). The measurement parameters were set as follows: temperature 25℃, equilibration time 120 seconds, scattering angle 173°. The hydrodynamic diameter of the particles was calculated using the Stokes-Einstein equation. The polydispersity index (PDI) reflects the width of the particle size distribution, and the smaller the PDI value (<0.2), the more uniform the particle size distribution.

[0053] (2) Accelerated stability test: In accordance with the relevant requirements for stability testing in Part IV "Physicochemical Testing Methods" of the Cosmetic Safety Technical Specifications (2015 edition), each sample was stored for 90 days under high temperature (45±1℃), room temperature (25±1℃) and low temperature (-15±1℃) conditions respectively; samples were taken every 15 days to observe changes in appearance (whether there is layering, precipitation, discoloration, or odor change), and the particle size change rate was measured on the 90th day. The particle size change rate was calculated as follows: Particle size change rate (%) = (particle size at 90 days - initial particle size) / initial particle size × 100%.

[0054] (3) Transdermal Absorption Test: Referring to the group standard "Test Methods for Transdermal Absorption of Cosmetics" (T / SHRH 006-2018), the transdermal absorption performance of the samples was determined using the Franz diffusion cell method. A TK-12D Franz diffusion cell (Shanghai Kaikai Technology & Trade Co., Ltd.) was used; excised pig skin (taken from the back of SPF-grade Bama miniature pigs, subcutaneous fat removed, approximately 0.5 mm thick, and soaked in physiological saline before use); a high-performance liquid chromatograph (Agilent 1260 Infinity II, Agilent Technologies, USA) was used. The sample was evenly coated onto the pig skin surface, with a coating area of ​​approximately 1.0 cm². 2 The coating amount is approximately 0.1 g / cm³. 2Pigskin was fixed between the supply and receiving cells of a Franz diffusion cell, with the cuticle facing upwards towards the supply cell. The receiving cell was filled with pH 7.4 phosphate buffer (containing 0.02% sodium azide for antibacterial purposes), and a constant temperature water bath was maintained at 32°C with stirring at 300 rpm. 1.0 mL samples were taken from the receiving cell at 1, 6, 12, and 24 hours, and an equal volume of fresh receiving solution was added simultaneously. High-performance liquid chromatography (HPLC) was then performed (chromatographic conditions: The chromatographic column was a C18 column (250 mm × 4.6 mm, 5 μm), the mobile phase was acetonitrile-water (55:45, v / v), the detection wavelength was 270 nm, the flow rate was 1.0 mL / min, the column temperature was 30 ℃, and the injection volume was 20 μL. The concentration of total amides of Zanthoxylum bungeanum fruit (with hydroxy-α-piperidine as a marker) in the receiving solution was determined. The cumulative transdermal penetration rate (%) was calculated as follows: (total amount of active ingredient in the receiving solution) / (total amount of active ingredient in the coated sample) × 100%.

[0055] (4) Test of residual particulate matter after reconstitution of Codonopsis pilosula lyophilized powder: The pre-reconstituted Codonopsis pilosula solution diluted with deionized water to the same volume was vacuum filtered through a 0.45 μm mixed cellulose ester filter membrane (diameter 47 mm, pre-weighed) and dried at 105 °C to constant weight. The filter membrane weight gain (i.e., the mass of residue) was calculated. The residual particulate matter rate (%) = (filter membrane weight gain) / (mass of Codonopsis pilosula extract added) × 100%.

[0056] (5) Stability test of active ingredient content: The content of total amides of Zanthoxylum bungeanum fruit (with hydroxy-α-piperazine as a marker) and Codonopsis pilosula cyclic peptide A as representative active ingredients was determined by high performance liquid chromatography; the content of total amides of Zanthoxylum bungeanum fruit was determined according to the relevant content determination methods of Zanthoxylum bungeanum and Codonopsis pilosula cyclic peptide in the Chinese Pharmacopoeia (2020 edition). The test parameters were: C18 column (250mm×4.6mm, 5μm), mobile phase was acetonitrile-water-phosphoric acid (45:55:0.1, v / v / v), and detection wave was [not specified]. The flow rate was 1.0 mL / min and the column length was 270 nm. The cyclic peptide A of Codonopsis pilosula was determined (test parameters: C18 column (250 mm × 4.6 mm, 5 μm), mobile phase was acetonitrile-0.1% phosphoric acid aqueous solution (30:70, v / v), detection wavelength was 203 nm, and flow rate was 0.8 mL / min). The samples were placed at 25 ℃ and 45 ℃ respectively, and the residual rate of active ingredients was determined after 6 months. The residual rate (%) = (content in month n / initial content) × 100%.

[0057] Each embodiment and comparative example was tested according to the above method, and the test results are shown in Table 1-2.

[0058] Table 1 Table 2 Analysis of Test Results: According to the performance test results in Tables 1-2 above, firstly, based on the particle size and polydispersity index (PDI) test data, the average particle size of Examples 1-5 is 48.7-55.1 nm, and the PDI is in the range of 0.118-0.135. This indicates that the anti-aging microemulsion essence prepared in the examples has nanoscale particle size and extremely uniform distribution. As for Comparative Example 1, without the addition of green liquid crystal emulsifier, a stable emulsion system could not be formed. The oil and water phases rapidly underwent macroscopic stratification after emulsification, and the particle size could not be determined. This directly proves that the green liquid crystal emulsifier is a key component in forming a stable microemulsion system. Comparative Example 2, without the addition of butylene glycol, had a particle size increased to 68.4 nm and a PDI increased to 0.198. This indicates that the lack of butylene glycol led to insufficient hydration of the hydrophilic head groups of the emulsifier molecules, resulting in a loose interfacial film arrangement and a certain degree of droplet aggregation. Comparative Example 3, without the addition of Codonopsis pilosula extract, had a particle size and PDI close to those of Example 1. This indicates that the addition of Codonopsis pilosula extract... The sample size had no significant negative impact on the particle size. In Comparative Example 4, the lyophilized powder of Codonopsis pilosula was added directly in powder form without pre-reconstitution treatment, resulting in a particle size increase to 134.2 nm and a PDI increase to 0.387. This confirmed that the insufficiently depolymerized particles in the lyophilized powder of Codonopsis pilosula existed as foreign particles in the system. In Comparative Example 5, direct rapid cooling resulted in a particle size increase to 186.5 nm and a PDI of 0.412. This was because rapid cooling prevented the emulsifier molecules from arranging themselves in an orderly manner at the oil-water interface, leading to insufficient liquid crystal structure development, insufficient interfacial film strength, and significant droplet aggregation. In Comparative Example 6, high shear treatment at a homogenization speed of 10,000 rpm resulted in the largest particle size and the widest PDI. This confirmed that excessive shear force destroyed the formed liquid crystal structure, causing the interfacial film to rupture and a large number of droplets to aggregate. In Comparative Example 7, the cooling rate was too fast (5℃ / min), resulting in a particle size increase to 158.4 nm and a PDI of 0.398. This indicated that an excessively fast cooling rate also resulted in insufficient liquid crystal structure development.

[0059] Secondly, analysis of accelerated stability test data showed that Examples 1-5 maintained a clear appearance under all three storage conditions, without stratification, precipitation, or discoloration. The particle size change rate after 90 days was less than 10% under different temperature conditions (e.g., 7.5%-8.9% at high temperature, 2.8%-3.5% at room temperature, and 4.2%-4.8% at low temperature). This indicates that the anti-aging microemulsion essence prepared by this invention has excellent long-term stability. Comparative Example 1 lacked a liquid crystal structure, had extremely low strength, and could not resist temperature stress and gravity, rapidly stratifying under various conditions. Comparative Example 2, although capable of forming a liquid crystal structure, had an incomplete interfacial film strength lower than the examples, with a particle size change rate of 28.6% under high-temperature accelerated conditions and 12.4% at room temperature. Comparative Example 3 had a liquid crystal structure... The structural stability was comparable to that of Example 1, indicating that the Codonopsis pilosula extract itself does not reduce the stability of the system; its negative impact only exists when not properly treated. In Comparative Example 4, the particles slowly settled in the system, and the particle size change rate reached 38.5% after 90 days of storage at 45°C, compared to 18.7% at room temperature, with visible particle settling at the bottom. In Comparative Example 5, the liquid crystal structure was not fully developed, and slight stratification occurred after 90 days of storage at 45°C, with a particle size change rate of 45.6%. In Comparative Example 6, the liquid crystal structure was completely destroyed, and the interface film was a simple surfactant monolayer or disordered multilayer structure, exhibiting the worst resistance to temperature stress. After 90 days of storage at 45°C, stratification occurred, with a particle size change rate as high as 68.2%. In Comparative Example 7, the liquid crystal structure was incomplete, and stratification occurred after 90 days of storage at 45°C, with a particle size change rate of 52.3%.

[0060] Then, analysis of the transdermal absorption test data showed that the cumulative transdermal absorption rates of Examples 1-5 all reached over 70% after 24 hours. This is due to the synergistic effect of the liquid crystal structure's fusion-promoting permeation mechanism, the high specific surface area release effect of nano-sized particles, and the gradient slow-release effect of the liquid crystal film, which is significantly higher than all comparative examples. Comparative Example 1 had a transdermal absorption rate of only 12.6% after 24 hours, indicating that simple mixtures without liquid crystal structures are difficult to penetrate the stratum corneum barrier. The transdermal absorption rate of Comparative Example 2 was 45.8%, lower than that of the examples, indicating that butylene glycol, in addition to its moisturizing function, also indirectly promotes transdermal absorption by regulating the hydration state of the stratum corneum. The transdermal absorption rate of Comparative Example 4 was 42.3%, indicating that the disturbance of the liquid crystal structure by the particles reduced the fusion-promoting permeation efficiency of the liquid crystal film. The transdermal absorption rates of Comparative Examples 5-7 ranged from 31.2% to 38.4%, all significantly lower than those of the examples, indicating that the integrity of the liquid crystal structure is positively correlated with the transdermal absorption efficiency.

[0061] Furthermore, the analysis of the residual particle count from the reconstituted lyophilized *Codonopsis pilosula* powder showed that the most important results were in Example 1 (3.2%) and Comparative Example 4 (17.3%). This confirms that the pre-reconstituted treatment significantly reduced the number of insoluble particles after reconstitution of the lyophilized *Codonopsis pilosula* powder. This is because during the freeze-drying process, the cyclic peptide-maltodextrin complex undergoes microphase separation due to ice crystal growth during the pre-freezing stage, forming a partially phase-separated structure between the cyclic peptide molecules and maltodextrin. The solid structure after freeze-drying contains both maltodextrin-rich and cyclic peptide-rich regions. When directly added to the microemulsion system, these microregions are difficult to fully hydrate and depolymerize, forming insoluble particles. However, the pre-reconstituted treatment, through advance hydration, allows water molecules to fully penetrate into the microporous structure of the lyophilized powder. After the maltodextrin matrix dissolves, the cyclic peptide molecules are released, achieving molecular-level dispersion and thus significantly reducing the residual amount of insoluble particles.

[0062] Finally, based on the analysis of the stability test data of the active ingredient content, after 6 months of storage at 25°C in Examples 1-5, the residual rates of the two active ingredients remained between 91.8% and 94.1%, and after 6 months of storage at 45°C, the residual rates were 84.3% to 87.2%. This indicates that the anti-aging microemulsion essence prepared by the present invention has excellent protective effects on the active ingredients. In Comparative Example 1, the residual rates of the two active ingredients after 6 months (at 25°C) were 65.4% and 62.8%, respectively, which were much lower than those in the Examples (approximately 93%), and even lower at 45°C, at 42.8% and 40.2%. This result shows that without a liquid crystal structure, the active ingredients are directly exposed to the aqueous phase and cannot obtain the protection of the interfacial film, resulting in a significantly accelerated oxidative degradation rate. The residual rates (at 25°C) of Comparative Example 2 were 82.5% (Zanthoxylum bungeanum fruit) and 80%. The percentage of 4% (Codonopsis pilosula cyclic peptide A) was lower than that of the examples, indicating that in addition to its moisturizing function, butylene glycol in this invention also slows down the oxidation reaction rate by forming hydrogen bonds with water to reduce the activity coefficient of dissolved oxygen in the aqueous phase. The residual rates of active ingredients (at 25°C) in Comparative Example 4 were 82.1% (Zanthoxylum bungeanum fruit) and 80.4% (Codonopsis pilosula cyclic peptide A). This is because the Codonopsis pilosula cyclic peptide in the unredissolved particles was in a solid microcrystalline state and could not be fully released and distributed. At the same time, the adsorption at the particle interface caused some active ingredients to be encapsulated in the precipitate. In addition, the disturbance of the liquid crystal film by the particles weakened the interfacial barrier function, which accelerated the oxidative degradation of the total amides in Zanthoxylum bungeanum fruit. The residual rates of Comparative Examples 5 to 7 were all lower than those of the examples, consistent with the results of stability tests and particle size tests, further confirming the positive role of the integrity of the liquid crystal structure in protecting the active ingredients.

[0063] In summary, the anti-aging microemulsion essence prepared in this application, through a process strategy of gradient cooling liquid crystal induction molding combined with dynamic homogenization rate control, and the technical means of pre-reconstitution treatment of Codonopsis pilosula freeze-dried powder, successfully prepared an anti-aging microemulsion essence with a complete liquid crystal structure, nanoscale particle size, excellent stability and high transdermal absorption performance.

[0064] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any way. Although the present invention has been disclosed above with reference to preferred embodiments, it is not intended to limit the present invention. Any person skilled in the art can make some modifications or alterations to the above-disclosed technical content to create equivalent embodiments without departing from the scope of the present invention. Any simple modifications, equivalent changes, and alterations made to the above embodiments based on the technical essence of the present invention without departing from the scope of the present invention shall still fall within the scope of the present invention.

Claims

1. An anti-aging microemulsion essence, characterized in that, The raw materials, by weight percentage (100%), include: 0.8-1.2% green liquid crystal emulsifier, 0.2-0.4% polyacrylate crosspolymer-6, 0.03-0.08% hydroxyethyl deacetylated chitosan, 5-7% butanediol, 1.5-2.5% 1,2-pentanediol, 0.8-1.2% 1,2-hexanediol, 0.03-0.08% disodium EDTA, 0.15-0.25% hydrolyzed sodium hyaluronate, 0.8-1.2% squalane, 0.4-0.6% meadowfoam seed oil, 0.5-0.7% tocopherol, 1.5-2.5% Sichuan pepper extract, 1.5-2.5% edelweiss flower / leaf extract, 0.8-1.2% *Pseudomonas aeruginosa* fermentation product extract, and 0.4-0.6% [unclear - possibly a specific ingredient or ingredient]. A compound of Eurasian Inula extract, 0.2-0.4% Codonopsis pilosula extract, 1.2-1.8% Astragalus membranaceus root extract, 0.03-0.08% tetrahydropiperine, balance to 100% deionized water.

2. The anti-aging microemulsion essence according to claim 1, characterized in that, The green liquid crystal emulsifier, by mass percentage, comprises: 8-12% sucrose stearate, 18-22% glyceryl stearate, 5-10% sorbitan stearate, 8-12% butanediol, 18-22% sorbitol, and the balance being 100% deionized water.

3. The anti-aging microemulsion essence according to claim 2, characterized in that, The preparation method of the green liquid crystal emulsifier includes the following steps: A1. Mix sucrose stearate, glyceryl stearate, sorbitan stearate and butanediol, heat to 70~80℃, stir to dissolve evenly, and form an oil phase mixture; A2. Add sorbitol to deionized water, heat to 70-80℃, stir to dissolve evenly, and form an aqueous mixture. A3. At 70~80℃, slowly add the oil phase mixture to the water phase mixture, homogenize at 5000~8000rpm for 5~10min, and cool to room temperature to obtain the green liquid crystal emulsifier.

4. The anti-aging microemulsion essence according to claim 1, characterized in that, The preparation method of the Sichuan pepper extract includes the following steps: B1. Pulverize the dried Sichuan pepper fruits to 40-60 mesh and put them into the extraction vessel of a supercritical carbon dioxide extraction device for extraction. Control the extraction pressure to 15-35 MPa, temperature to 40-55℃, carbon dioxide flow rate to 8-25 kg / h, and extraction time to 0.5-4 h to obtain a carbon dioxide fluid carrying the active ingredients of Sichuan pepper. B2. Pass the carbon dioxide fluid carrying the active ingredients of Sichuan pepper obtained in step B1 into the separation vessel, control the pressure of the separation vessel to be 3~8MPa, and the separation temperature to be 30~50℃, so that the active ingredients of Sichuan pepper dissolved in the carbon dioxide fluid are precipitated in the separation vessel and separated from the carbon dioxide gas, and collect the crude extract at the bottom of the separation vessel. B3. Dissolve the crude extract obtained in step B2 in a mixed solvent of butanediol and 1,2-hexanediol, and stir at 40~50℃ to dissolve evenly, so that the active ingredients of Sichuan pepper are fully transferred to the polyol solvent system to obtain a solution containing the active ingredients of Sichuan pepper. B4. Transfer the solution obtained in step B3 to a molecular distillation apparatus and remove low-boiling-point volatile oils and unpleasant odor substances under conditions of 50-60℃ and vacuum degree of 1-10Pa. Collect the heavy phase fraction, then add activated carbon to the solution after molecular distillation, stir and adsorb at 40-50℃ for 1-2 hours, filter to remove activated carbon, and remove pigments and unpleasant odor components to obtain a clear and transparent pepper fruit extract solution. B5. After decolorizing and deodorizing the Sichuan pepper fruit extract solution obtained in step B4, the filtrate is concentrated under reduced pressure at 40~50℃ and -0.06~-0.08MPa to 1 / 5~1 / 3 of the original volume to obtain Sichuan pepper extract.

5. The anti-aging microemulsion essence according to claim 4, characterized in that, The mass ratio of the dried Sichuan pepper fruit, the 1,2-hexanediol, and the butanediol is 1:1:(12~18).

6. The anti-aging microemulsion essence according to claim 1, characterized in that, The preparation method of the Eurasian Inula extract includes the following steps: C1. Pulverize dried Eurasian Inula japonica into 40-60 mesh, add 20-70% ethanol aqueous solution, heat and reflux for 1.5-3 hours, filter and collect the filtrate, repeat the extraction of the residue 1-2 times, and combine the filtrates to obtain crude extract. C2. The crude extract from step C1 is concentrated under reduced pressure at 60~70℃ and -0.06~-0.08MPa to 1 / 5~1 / 3 of its original volume to obtain a concentrated solution. C3. The concentrate from step C2 is purified by passing it through a macroporous adsorption resin. Impurities are removed by washing with deionized water and low-concentration ethanol in sequence, and then eluted with 50-80% ethanol. The eluent is collected. C4. Add activated carbon to the eluent from step C3, stir at 50-60℃ for 1-2 hours for adsorption and decolorization, filter, add hydroxypropyl cyclodextrin to the filtrate, stir at 40-50℃ to dissolve evenly, and obtain the inclusion complex solution. C5. The inclusion complex solution from step C4 is concentrated under reduced pressure at 50~60℃ and -0.06~-0.08MPa to 1 / 3~1 / 2 of its original volume, then spray-dried and the dried powder is collected to obtain the Eurasian Inula extract. The inlet air temperature of the spray dryer is 160~190℃ and the outlet air temperature is 80~100℃.

7. The anti-aging microemulsion essence according to claim 6, characterized in that, The mass ratio of the dried Eurasian Inula japonica to the hydroxypropyl cyclodextrin is 1:(8~10).

8. The anti-aging microemulsion essence according to claim 1, characterized in that, The preparation method of the Codonopsis pilosula extract includes the following steps: D1. Select dried roots of Codonopsis pilosula, crush them to 40-60 mesh, add 3-10 times the weight of the medicinal material in deionized water, soak for 30-60 minutes, heat to a gentle boil and decoct for 30-90 minutes, filter to obtain the dregs and decoction. D2. Repeat the decoction of the dregs from step D1 once, filter, combine the two decoctions, let stand and cool to room temperature to obtain the extract of Codonopsis pilosula. D3. The extract of Codonopsis pilosula obtained in step D2 is concentrated under reduced pressure at 50~60℃ and -0.06~-0.08MPa to 1 / 5~1 / 3 of the original volume. The precipitate is removed by centrifugation, and the supernatant extract is collected. D4. Add maltodextrin to the supernatant extract from step D3, stir and dissolve evenly to obtain a mixture. Pre-freeze the mixture at -35℃ to -40℃ for 2 to 3 hours, and place it in a freeze dryer. Sublime dry for 10 to 15 hours at a shelf temperature of -5℃ ± 5℃ and a front chamber vacuum of 10 to 30 Pa. Then dry for 5 to 10 hours at a shelf temperature of 20℃ ± 5℃ and a vacuum of 10 to 30 Pa until the moisture content is less than 5% to obtain Codonopsis pilosula cyclic peptide freeze-dried blocks. D5. Crush the freeze-dried block of Codonopsis pilosula cyclic peptide from step D4 through a 40-60 mesh sieve to obtain Codonopsis pilosula extract.

9. The anti-aging microemulsion essence according to claim 8, characterized in that, The mass ratio of the dried root of Codonopsis pilosula to the maltodextrin is 1:(0.8~1.2).

10. A method for preparing an anti-aging microemulsion essence according to any one of claims 1-9, characterized in that, Includes the following steps: S1. Preparation of Codonopsis pilosula pre-reconstituted solution: Weigh Codonopsis pilosula extract, add 3-5 times the mass of Codonopsis pilosula extract deionized water, stir and reconstitute in a water bath at 30-40℃ for 15-30 minutes to obtain Codonopsis pilosula pre-reconstituted solution; S2. Oil phase preparation: Green liquid crystal emulsifier, squalane, meadowfoam seed oil and tocopherol are heated and dissolved at 70~80℃ and stirred until completely dissolved and homogeneous to form an oil phase; S3. Preparation of aqueous phase one: Dissolve 40-60% of deionized water, butanediol, and disodium EDTA at 70-80°C by heating and stirring at 200-400 rpm until completely dissolved and homogeneous to form aqueous phase one. S4. Preparation of aqueous phase II: Take the remaining deionized water, add polyacrylate crosslinking polymer-6 and hydrolyzed sodium hyaluronate, and stir and disperse evenly at 200~400 rpm under room temperature to form a transparent gel-like aqueous phase II. S5. Liquid crystal emulsification and molding: At 70~80℃, the oil phase obtained in step S2 is added to the aqueous phase I obtained in step S3, and homogenized at 5000~8000 rpm for 5~10 min to form a preliminary emulsion. Then, the temperature is gradually reduced to 45~50℃ at a rate of 1~2℃ / min, and low-speed stirring at 300~500 rpm is carried out during the cooling process to obtain the emulsion system. S6. Addition of polymer and polyol: After cooling to 45~50℃, add the aqueous phase II obtained in step S4 to the emulsion system obtained in step S5, and stir at 200~400rpm for 5~8min to make the system uniform, and obtain the microemulsion system. S7. Addition of active ingredients: After thoroughly mixing the pre-reconstituted Codonopsis pilosula solution obtained in step S1 with the compound of hydroxyethyl deacetylated chitosan, Zanthoxylum bungeanum fruit extract, Edelweiss flower / leaf extract, Pseudomonas aeruginosa fermentation product extract, Inula japonica extract, and Astragalus membranaceus root extract, and maintaining the temperature at 45~50℃, add it to the microemulsion system in step S6 to obtain a mixture containing active ingredients. S8. Add tetrahydropiperine, 1,2-pentanediol and 1,2-hexanediol sequentially to the active ingredient mixture obtained in step S7, stir at 200-400 rpm for 10-15 min, then continue to cool to room temperature, reduce the homogenization speed to 200-300 rpm and maintain for 3-5 min to obtain the anti-aging microemulsion essence.

Images