Composite essence oil functional core ball steady-state delivery system and preparation method and application of essence emulsion of composite essence oil functional core ball steady-state delivery system

Abstract

The invention discloses a composite essence oil functional core ball steady-state delivery system and a preparation method and application of essence emulsion of the composite essence oil functional core ball steady-state delivery system, and belongs to the technical field of cosmetics. The invention innovatively researches and develops a composite essence oil efficacy core ball steady-state delivery system of'unstable small molecule active ingredients + biosynthetic active macromolecules + penetration enhancer molecules + functional small molecules + essence oil ', and the composite essence oil efficacy core ball has excellent spherical appearance, smooth ball surface, excellent dissolution dispersibility and porosity of 90% or more; when the composite essence oil is dispersed into the essence oil, pores of the functional core ball are rapidly filled with the essence oil, and the composite essence oil functional core ball is obtained. Meanwhile, the invention further develops a whole-process low-temperature production and processing technology based on liquid nitrogen quick freezing, it is ensured that the activity of small-molecule active ingredients is not affected by the technology, and high-quality production of the functional core balls is ensured.

Description

Technical Field

[0001] The present invention relates to a steady-state delivery system for composite essence oil efficacy core balls and a preparation method and application of an essence emulsion thereof, belonging to the technical field of cosmetics. Background Art

[0002] Functional active ingredients are widely used in industries such as cosmetics and health foods. However, many active ingredients have problems such as instability, peculiar smell, poor compatibility, and low bioavailability, which seriously restrict their applications in cosmetics and foods.

[0003] In water-based formula products, such as creams, eye creams, essence liquids, beverages, etc., the stability, compatibility, and utilization of active ingredients face greater challenges, especially the problem of biological activity attenuation during the shelf life. Many active substances almost lose their activity within a shelf life of 1 - 3 years.

[0004] Therefore, advanced steady-state delivery technologies and innovative product designs are needed to solve these pain points, thereby promoting the product upgrade and innovative development of cosmetics and health foods. Summary of the Invention

[0005] In order to overcome the above technical defects, the present invention has developed a steady-state delivery system for composite essence oil efficacy core balls and a preparation method and application of an essence liquid thereof, successfully solving the pain point problem of instability in applications.

[0006] The composite freeze-dried efficacy core ball steady-state delivery system described in the present invention has an excellent spherical appearance, a smooth ball surface, excellent dissolution and dispersion properties, and a porosity of more than 90%. When it is dispersed in essence oil, the essence oil quickly fills the pores of the efficacy core balls, obtaining composite essence oil efficacy core balls.

[0007] Firstly, a steady-state delivery system for composite essence oil efficacy core balls of "unstable small molecule active ingredient + biosynthetic active macromolecule + penetration enhancer molecule + functional small molecule + essence oil" is innovatively developed. The above small molecule active ingredient, active macromolecule, penetration enhancer molecule, and functional small molecule form an ordered and stable nano-assembled steady-state structure system through multiple intermolecular interactions, solving the stability and compatibility problems of small molecule active ingredients. Secondly, a skin care essence oil is developed. When the efficacy core balls are dispersed in the essence oil, the essence oil quickly fills the pores of the efficacy core balls, obtaining composite essence oil efficacy core balls, further enhancing the stability of active ingredients, the mechanical strength of the efficacy core balls, and the shelf stability. Thirdly, penetration enhancer molecules, such as phloretin, cyclodextrin, menthol, etc., can further enhance the transdermal absorption rate of small molecules. Fourthly, a solvent liquid is developed. By mixing the solvent liquid with the essence oil efficacy core balls and gently shaking to mix evenly, a freshly prepared efficacy skin care essence emulsion can be obtained. Finally, a full-process low-temperature production and processing technology based on liquid nitrogen quick-freezing was developed to ensure that the activity of small molecule active ingredients is not affected by the process and to ensure the high-quality production of efficacy core balls.

[0008] The steady-state delivery system of the composite essence oil efficacy core ball described in the present invention includes: unstable small molecule active ingredients, biosynthetic active macromolecules, penetration enhancers, functional small molecules, and essence oil.

[0009] In the above steady-state delivery system of the composite essence oil efficacy core ball, the small molecule active ingredients, active macromolecules, penetration enhancers, and functional small molecules form an orderly and stable nano-assembled steady-state structure system through multiple intermolecular interactions, successfully solving application pain points such as the stability, compatibility, and absorbability of small molecule active ingredients.

[0010] Furthermore, in the above technical solution, the unstable small molecule active ingredients include one or more of active ingredients such as ergothioneine, glutathione, anthocyanin, blue copper peptide, vitamin C (hereinafter referred to as Vc), ethylbisiminomethylchalcone manganese chloride (hereinafter referred to as EUK134), etc.

[0011] Furthermore, in the above technical solution, the content of the unstable small molecule active ingredients (the content described in the present invention all refers to the weight content, the same below) is 0.1%-70%, a more suitable content range is 1%-30%, and a more suitable content range is 5%-20%; In the above steady-state delivery system of the composite essence oil efficacy core ball, the biosynthetic active macromolecules are used to construct the framework of the efficacy core ball and improve the mechanical stability of the efficacy core ball.

[0012] Furthermore, in the above technical solution, the biosynthetic active macromolecules include one or more of components such as fermented polysaccharides, fermented proteins, recombinant collagen, recombinant type III collagen, recombinant type XII collagen, recombinant fibronectin, yeast proteins, polyglutamic acid, pullulan, yeast polysaccharides, yeast β-glucan, sodium hyaluronate, xanthan gum, gellan gum, sodium DNA (PDRN polydeoxyribonucleotide), fermented ganoderma lucidum polysaccharides, etc.

[0013] Furthermore, in the above technical solution, the molecular weight range of the biosynthetic active macromolecules is 1000-2000000, a more suitable molecular weight range is 3000-1200000, and a more suitable molecular weight range is 10000-800000.

[0014] In the above steady-state delivery system of the composite essence oil efficacy core ball, the penetration enhancer molecules can further improve the transdermal absorption efficiency of small molecule active ingredients.

[0015] Further, in the above technical solution, the penetration enhancer molecules include one or more of phloretin, menthol, hydroxypropyl-β-cyclodextrin, methyl-β-cyclodextrin, butylene glycol, etc.

[0016] In the above composite essence oil efficacy core ball steady-state delivery system, the functional small molecules can further enrich or improve the skin care efficacy of the core ball.

[0017] Further, in the above technical solution, the functional small molecules include one or more of active ingredients such as asiaticoside, madecassoside, L-theanine, sialic acid, arbutin, niacinamide, tranexamic acid, ectoin, Vc glucoside, catechin, trehalose, nonapeptide-1, snake venom-like peptide, conotoxin-like peptide, acetyl hexapeptide-8, mannitol, etc.

[0018] In the above composite essence oil efficacy core ball steady-state delivery system, dispersing the core ball in the essence oil further improves the stability of the active ingredients, the mechanical strength of the core ball, and the shelf stability.

[0019] Further, in the above technical solution, the essence oil includes one or more of: coco-caprylate / caprate, isocetane, isododecane, jojoba seed oil, squalane, fermented peony seed oil, fermented sacha inchi oil, fermented rice bran oil, fermented grape seed oil, fermented vegetable oil, Shorea obtusa seed fat, corn germ oil, tocopheryl acetate, rapeseed oil, macadamia seed oil, isononyl isononanoate, ethylhexyl palmitate, caprylic / capric triglyceride, Limnanthes alba (meadowfoam) seed oil, sunflower seed oil, Rosa damascena flower oil, hydrogenated polyisobutene, polydimethylsiloxane, lavender essential oil, tea tree essential oil, plant essential oil, essence, etc.

[0020] Further, in the above technical solution, the mass ratio of the unstable small molecule active ingredient, biosynthetic active macromolecule, penetration enhancer molecule to the functional small molecule is 1:0.1-10:0.05-5:0.1-10:1000-10000, and the more suitable ratio range is 1:0.5-5:0.1-1:0.5-5:100-1000.

[0021] Further, in the above technical solution, the composite essence oil efficacy core ball has a particle size range of 0.1-15 mm, and the more suitable range is 0.5-8 mm; the more suitable range is 1-5 mm.

[0022] The present invention also provides a production process for the steady-state delivery system of the composite essence oil efficacy core balls. This process is based on the whole-process low-temperature processing by liquid nitrogen quick-freezing to ensure that the activity of small molecule active ingredients is not affected by the process. The production process of the steady-state delivery system of the composite essence oil efficacy core balls includes the following steps: First, prepare the composite freeze-dried efficacy core balls; then, when dispersing the efficacy core balls in the essence oil, the essence oil quickly fills the pores of the efficacy core balls to obtain the steady-state delivery system of the composite essence oil efficacy core balls.

[0023] The production process of the steady-state delivery system of the composite essence oil efficacy core balls described in the present invention is specifically as follows: A. Mix the unstable small molecule active raw materials and biosynthetic active macromolecules evenly, then add pure water and stir to dissolve to obtain a clear and transparent solution; B. During the stirring process, add the penetration enhancer molecules and functional small molecules to the above solution and stir until all components are completely dissolved to obtain the target solution; C. Drop the target solution into the insulated liquid nitrogen bucket; during the dropping process, it is necessary to introduce nitrogen gas protection into the target solution to avoid the oxidation loss of active ingredients; D. Freeze-dry the small ice balls formed by liquid nitrogen freezing to obtain the composite freeze-dried efficacy core balls.

[0024] E. Disperse the efficacy core balls into the essence oil, and the essence oil quickly fills the pores of the efficacy core balls to obtain the steady-state delivery system of the composite essence oil efficacy core balls.

[0025] Further, in the above technical solution, during the dropping in step C, dropping equipment such as but not limited to peristaltic pumps, syringe pumps, and flow pumps that can control the speed and droplet size is used.

[0026] Further, in the above technical solution, the essence oil described in step E has the following preparation process: Weigh different oil components respectively, put them into a container in sequence, and stir evenly until clear and transparent to obtain the (skin care) essence oil.

[0027] The present invention also provides a preparation method for the efficacy skin care essence liquid, including the following steps: Mix the solvent liquid with the above-mentioned steady-state delivery system of the essence oil efficacy core balls, and gently shake and mix evenly to obtain the freshly prepared efficacy skin care essence liquid.

[0028] Further, in the above technical solution, the solvent liquid described in the present invention includes water, a humectant, and / or an emulsifier. The preparation process of the solvent liquid is briefly as follows: Weigh the humectant component and the emulsifier component respectively, put them into a container in sequence, then add purified water, and stir evenly until clear and transparent to obtain the solvent liquid.

[0029] Further, in the above technical solution, the humectant includes one or more of xylitol glucoside, anhydroxylitol, xylitol, tremella polysaccharide, betaine, sodium hyaluronate, xanthan gum, hydroxyethyl cellulose, butanediol, pentanediol, hexanediol, p-hydroxyacetophenone, glycerol, β-glucan, polyglycerol-10, glycerol polyether-26, chondrus crispus, trehalose glycoside, hydrogenated starch hydrolysate, etc.

[0030] Further, in the above technical solution, the emulsifier includes: Tween-20 (polysorbate-20), Tween 80, laureth-4, PEG-40 hydrogenated castor oil, wild soybean seed extract, coconut glucoside, PEG stearate, etc. Description of the Drawings

[0031] Figure 1 It is the steady-state delivery system diagrams of A1, A2 and A3 ergothioneine composite freeze-dried efficacy core balls and B1, B2 and B3 ergothioneine composite essential oil efficacy core balls. The samples are all from Examples 1-3; Figure 2 It is the steady-state delivery system diagrams of A4, A5 glutathione composite freeze-dried efficacy core balls and B4, B5 glutathione composite essential oil efficacy core balls. The samples are all from Examples 4-5; Figure 3 It is the steady-state delivery system diagrams of A6, A7 anthocyanin-Vc composite freeze-dried efficacy core balls and B6, B7 anthocyanin-Vc composite essential oil efficacy core balls. The samples are all from Examples 6-7; Figure 4 It is the steady-state delivery system diagrams of A8, A9 EUK134 composite freeze-dried efficacy core balls and B8, B9 EUK134 composite essential oil efficacy core balls. The samples are all from Examples 8-9; Figure 5 It is the steady-state delivery system diagrams of A10, A11 copper peptide composite freeze-dried efficacy core balls and B10, B11 copper peptide composite essential oil efficacy core balls. The samples are all from Examples 10 and 11; Figure 6Figure of essence emulsion for the steady - state delivery system of compound essence oil efficacy core balls; among them: C2, essence emulsion II of ergothioneine compound efficacy core ball steady - state delivery system; C3, essence emulsion III of ergothioneine compound efficacy core ball steady - state delivery system; C4, essence emulsion IV of glutathione compound efficacy core ball steady - state delivery system; C5, essence emulsion V of glutathione compound efficacy core ball steady - state delivery system; C6, essence emulsion VI of anthocyanin - Vc compound efficacy core ball steady - state delivery system; C7, essence emulsion VII of anthocyanin - Vc compound efficacy core ball steady - state delivery system; C8, essence emulsion VIII of EUK134 compound efficacy core ball steady - state delivery system; C9, essence emulsion IX of EUK134 compound efficacy core ball steady - state delivery system; C10, essence emulsion X of blue copper peptide compound efficacy core ball steady - state delivery system; C11, essence emulsion XI of blue copper peptide compound efficacy core ball steady - state delivery system; Figure 7 Scanning electron microscope image of the cross - section of the compound freeze - dried efficacy core ball steady - state delivery system: A3, ergothioneine compound freeze - dried efficacy core ball steady - state delivery system; A5, glutathione compound freeze - dried efficacy core ball steady - state delivery system; A7, anthocyanin - Vc compound freeze - dried efficacy core ball steady - state delivery system; A9, EUK134 compound freeze - dried efficacy core ball steady - state delivery system. The samples are from Examples 3, 5, 7, and 9 respectively; Figure 8 Flow chart of the preparation process of the essence emulsion of the active ingredient compound efficacy core ball steady - state delivery system. Detailed implementation methods

[0032] Example 1 Preparation of No.1 of the ergothioneine compound essence oil efficacy core ball steady - state delivery system

[0033] A. Weigh 0.3 g of ergothioneine, 0.6 g of recombinant type III collagen, 0.45 g of pullulan polysaccharide, and 0.75 g of yeast β - glucan respectively, and put them into a beaker and mix evenly; B. Add 27.9 g of pure water, heat and stir until the active ingredients are completely dissolved; C. Use a peristaltic pump to drop the above - mentioned solution into a thermally insulated liquid nitrogen bucket drop by drop. The droplet size is about 50 mg, and it is rapidly frozen to obtain small ice balls. When dropping, nitrogen needs to be introduced into the target solution for protection to avoid the loss of active ingredients due to oxidation; D. Transfer the small ice balls formed by liquid nitrogen freezing to a freeze - dryer and conduct freeze - drying for 40 h. The cold trap temperature of the freeze - dryer is controlled at about - 70 °C (about means a deviation of 3 °C up and down, the same below), and the final temperature of the drying chamber is controlled at about 30 °C, then the ergothioneine compound freeze - dried efficacy core ball steady - state delivery system can be obtained, denoted as A1; E. Weigh 39.5 g of hydrogenated polyisobutene, 35 g of coco-caprylate / caprate, 7.0 g of fermented peony seed oil, 9.0 g of isocetane, 5.0 g of squalane, 3.0 g of corn germ oil, 1.0 g of acrylate copolymer and 0.5 g of Rosa damascena flower oil respectively, put them into a beaker, and then stir and mix evenly to obtain the essence oil; F. Take a certain amount of freeze-dried efficacy core balls, put them into a container, such as a vial, a glass bottle, a plastic bottle, etc., and then add a certain amount of essence oil to obtain the composite essence oil efficacy core ball steady-state delivery system No. I, denoted as B1.

[0034] Example 2 Preparation of the ergothioneine composite essence oil efficacy core ball steady-state delivery system No. II

[0035] A. Weigh 0.3 g of ergothioneine, 0.48 g of recombinant type III collagen, 0.45 g of pullulan polysaccharide, 0.54 g of yeast β-glucan, 0.3 g of trehalose and 0.06 g of ectoine respectively, put them into a beaker and mix evenly; B. Add 27.87 g of purified water, heat and stir until the active ingredients are completely dissolved; C. Use a peristaltic pump to drop the above solution into a thermally insulated liquid nitrogen bucket drop by drop, with the droplet size of about 50 mg, and quickly freeze to obtain small ice balls; when dropping, nitrogen needs to be introduced into the target solution for protection to avoid oxidation loss of the active ingredients; D. Transfer the small ice balls formed by liquid nitrogen freezing to a freeze dryer, and carry out freeze drying for 40 h. The cold trap temperature of the freeze dryer is controlled at about -70 °C, and the final temperature of the drying chamber is controlled at about 30 °C to obtain the ergothioneine composite freeze-dried efficacy core ball steady-state delivery system, denoted as A2; E. Weigh 39.5 g of hydrogenated polyisobutene, 35 g of coco-caprylate / caprate, 7.0 g of fermented peony seed oil, 9.0 g of isocetane, 5.0 g of squalane, 3.0 g of corn germ oil, 1.0 g of acrylate copolymer and 0.5 g of Rosa damascena flower oil respectively, put them into a beaker, and then stir and mix evenly to obtain the essence oil; F. Take a certain amount of freeze-dried efficacy core balls, put them into a container, such as a vial, a glass bottle, a plastic bottle, etc., and then add a certain amount of essence oil to obtain the composite essence oil efficacy core ball steady-state delivery system No. II, denoted as B2.

[0036] Example 3 Preparation of the ergothioneine composite essence oil efficacy core ball steady-state delivery system No. III

[0037] A. Weigh 0.3 g of ergothioneine, 0.48 g of recombinant type III collagen, 0.45 g of pullulan, 0.54 g of yeast β-glucan, 0.3 g of trehalose, 0.03 g of heptapeptide-1, 0.06 g of ectoin, 0.03 g of phloretin and 0.18 g of methyl-β-cyclodextrin respectively, and put them into a beaker and mix well; B. Add 27.66 g of purified water, heat and stir until the active ingredients are completely dissolved; C. Use a peristaltic pump to drop the above solution drop by drop into a thermally insulated liquid nitrogen bucket. The size of the liquid droplets is about 50 mg, and rapid freezing is carried out to obtain small ice balls; when dropping, it is necessary to introduce nitrogen gas into the target solution for protection to avoid oxidation loss of the active ingredients; D. Transfer the small ice balls formed by liquid nitrogen freezing to a freeze dryer and carry out freeze drying for 40 h. The cold trap temperature of the freeze dryer is controlled at about -70 °C, and the final temperature of the drying chamber is controlled at about 30 °C, then the ergothioneine composite freeze-dried efficacy core ball steady-state delivery system can be obtained, denoted as A3; E. Weigh 39.5 g of hydrogenated polyisobutene, 35 g of coco-caprylate / caprate, 7.0 g of fermented peony seed oil, 9.0 g of isocetane, 5.0 g of squalane, 3.0 g of corn germ oil, 1.0 g of acrylate copolymer and 0.5 g of Rosa damascena flower oil respectively, put them into a beaker, and then stir and mix well to obtain the essence oil; F. Take a certain amount of freeze-dried efficacy core balls, put them into a container, such as a vial, a glass bottle, a plastic bottle, etc., and then add a certain amount of essence oil to obtain the composite essence oil efficacy core ball steady-state delivery system No. III, denoted as B3.

[0038] Example 4 Preparation of glutathione composite essence oil efficacy core ball steady-state delivery system No. IV

[0039] A. Weigh 0.24 g of glutathione, 0.36 g of recombinant type XVII collagen, 0.48 g of yeast polysaccharide, 0.36 g of sodium hyaluronate, 0.3 g of asiaticoside, 0.06 g of acetyl hexapeptide-8, 0.12 g of sodium DNA, 0.18 g of mannitol respectively, and put them into a beaker and mix well; B. Add 27.96 g of purified water and stir until the active ingredients are completely dissolved; C. Use a peristaltic pump to drop the above solution drop by drop into a thermally insulated liquid nitrogen bucket. The size of the liquid droplets is about 40 mg, and rapid freezing is carried out to obtain small ice balls; when dropping, it is necessary to introduce nitrogen gas into the target solution for protection to avoid oxidation loss of the active ingredients; D. Transfer the small ice balls formed by liquid nitrogen freezing to a freeze dryer and conduct freeze drying for 40 h. Control the cold trap temperature of the freeze dryer at about -70 °C and the final temperature of the drying chamber at about 30 °C to obtain the ergothioneine composite freeze-dried efficacy core ball steady-state delivery system, denoted as A4; E. Weigh 41 g of jojoba seed oil, 22 g of isododecane, 9 g of fermented Sacha inchi oil, 8 g of fermented rice bran oil, 8 g of tocopheryl acetate, 11 g of sunflower seed oil, and 1.0 g of tea tree essential oil respectively, put them into a beaker, and then stir and mix evenly to obtain the essential oil; F. Take a certain amount of freeze-dried efficacy core balls, put them into a container, such as a vial, a glass bottle, a plastic bottle, etc., and then add a certain amount of the essential oil to obtain the composite essential oil efficacy core ball steady-state delivery system No. IV, denoted as B4.

[0040] Example 5 Preparation of glutathione composite essential oil efficacy core ball steady-state delivery system No. V

[0041] A. Weigh 0.24 g of glutathione, 0.36 g of recombinant type XVII collagen, 0.48 g of yeast polysaccharide, 0.36 g of sodium hyaluronate, 0.3 g of asiaticoside, 0.01 g of conopeptide, 0.12 g of sodium DNA, 0.18 g of mannitol, 0.06 g of menthol, and 0.15 g of hydroxypropyl-β-cyclodextrin respectively, put them into a beaker and mix evenly; B. Add 27.75 g of purified water and stir until the active ingredients are completely dissolved; C. Use a peristaltic pump to drop the above solution into a thermally insulated liquid nitrogen bucket drop by drop. The droplet size is about 40 mg, and rapid freezing is carried out to obtain small ice balls; when dropping, it is necessary to introduce nitrogen protection into the target solution to avoid oxidation loss of the active ingredients; D. Transfer the small ice balls formed by liquid nitrogen freezing to a freeze dryer and conduct freeze drying for 40 h. Control the cold trap temperature of the freeze dryer at about -70 °C and the final temperature of the drying chamber at about 30 °C to obtain the ergothioneine composite freeze-dried efficacy core ball steady-state delivery system, denoted as A5; E. Weigh 41 g of jojoba seed oil, 22 g of isododecane, 9 g of fermented Sacha inchi oil, 8 g of fermented rice bran oil, 8 g of tocopheryl acetate, 11 g of sunflower seed oil, and 1.0 g of tea tree essential oil respectively, put them into a beaker, and then stir and mix evenly to obtain the essential oil; F. Take a certain amount of freeze-dried efficacy core balls, put them into a container, such as a vial, a glass bottle, a plastic bottle, etc., and then add a certain amount of the essential oil to obtain the composite essential oil efficacy core ball No. V, denoted as B5.

[0042] Example 6 Preparation of anthocyanin-Vc composite essential oil efficacy core ball steady-state delivery system No. VI

[0043] A. Weigh 0.09 g of anthocyanin, 0.54 g of recombinant fibronectin, 0.15 g of xanthan gum, 0.45 g of polyglutamic acid, 0.3 g of asiaticoside, 0.42 g of vitamin C (Vc), 0.15 g of Vc glucoside, and 0.3 g of theanine separately, and put them into a beaker and mix evenly; B. Add 27.75 g of pure water and stir until the active ingredients are completely dissolved; C. Use a peristaltic pump to drop the above solution into a thermally insulated liquid nitrogen bucket drop by drop. The size of the liquid droplets is about 40 mg, and rapid freezing is carried out to obtain small ice balls. When dropping, nitrogen needs to be introduced into the target solution for protection to avoid the oxidation loss of the active ingredients; D. Transfer the small ice balls formed by liquid nitrogen freezing to a freeze dryer and carry out freeze drying for 40 h. The cold trap temperature of the freeze dryer is controlled at about -70 °C, and the final temperature of the drying chamber is controlled at about 30 °C, then the ergothioneine composite freeze-dried efficacy core ball steady-state delivery system can be obtained, denoted as A6; E. Weigh 33 g of fermented grape seed oil, 32 g of ethylhexyl palmitate, 8 g of shorea obtusa seed fat, 9 g of rapeseed oil, 12 g of macadamia nut oil, 5 g of squalane, and 1.0 g of essence separately, put them into a beaker, and then stir and mix evenly to obtain the essence oil; F. Take a certain amount of freeze-dried efficacy core balls and put them into a container, such as a vial, a glass bottle, a plastic bottle, etc., and then add a certain amount of essence oil to obtain the composite essence oil efficacy core ball steady-state delivery system No. VI, denoted as B6.

[0044] Example 7 Preparation of Anthocyanin-Vc Composite Essence Oil Efficacy Core Ball Steady-State Delivery System No. VII

[0045] A. Weigh 0.09 g of anthocyanin, 0.54 g of recombinant fibronectin, 0.15 g of xanthan gum, 0.45 g of polyglutamic acid, 0.3 g of asiaticoside, 0.42 g of vitamin C, 0.15 g of Vc glucoside, 0.3 g of theanine, 0.03 g of butanediol, and 0.03 g of phloretin separately, and put them into a beaker and mix evenly; B. Add 27.69 g of pure water and stir until the active ingredients are completely dissolved; C. Use a peristaltic pump to drop the above solution into a thermally insulated liquid nitrogen bucket drop by drop. The size of the liquid droplets is about 40 mg, and rapid freezing is carried out to obtain small ice balls. When dropping, nitrogen needs to be introduced into the target solution for protection to avoid the oxidation loss of the active ingredients; D. Transfer the small ice balls formed by liquid nitrogen freezing to a freeze dryer and carry out freeze drying for 40 h. The cold trap temperature of the freeze dryer is controlled at about -70 °C, and the final temperature of the drying chamber is controlled at about 30 °C, then the ergothioneine composite freeze-dried efficacy core ball steady-state delivery system can be obtained, denoted as A7; E. Weigh 33 g of fermented grape seed oil, 32 g of ethylhexyl palmitate, 8 g of Shorea obtusa seed fat, 9 g of rapeseed oil, 12 g of macadamia nut oil, 5 g of squalane, and 1.0 g of essence respectively, put them into a beaker, and then stir and mix evenly to obtain the essence oil. F. Take a certain amount of freeze-dried efficacy core balls, put them into a container, such as a vial, a glass bottle, a plastic bottle, etc., and then add a certain amount of essence oil to obtain the composite essence oil efficacy core ball steady-state delivery system VII, denoted as B7.

[0046] Example 8 Preparation of EUK134 Composite Essence Oil Efficacy Core Ball Steady-State Delivery System VIII

[0047] A. Weigh 0.09 g of EUK134, 0.48 g of yeast protein, 0.3 g of recombinant collagen, 0.24 g of gellan gum, 0.18 g of fermented ganoderma lucidum polysaccharide, 0.45 g of neuraminic acid, 0.09 g of snake venom-like peptide, and 0.12 g of arbutin respectively, and put them into a beaker and mix evenly. B. Add 28.14 g of purified water and stir until the active ingredients are completely dissolved. C. Use a peristaltic pump to drop the above solution into a thermally insulated liquid nitrogen bucket drop by drop. The droplet size is about 40 mg, and it is rapidly frozen to obtain small ice balls. When dropping, nitrogen needs to be introduced into the target solution for protection to avoid oxidation loss of the active ingredients. D. Transfer the small ice balls formed by liquid nitrogen freezing to a freeze dryer and conduct freeze drying for 40 h. The cold trap temperature of the freeze dryer is controlled at about -70 °C, and the final temperature of the drying chamber is controlled at about 30 °C to obtain the ergothioneine composite freeze-dried efficacy core ball steady-state delivery system, denoted as A8. E. Weigh 22 g of isononyl isononanoate, 37 g of caprylic / capric triglyceride, 5 g of Shorea obtusa seed fat, 20 g of Limnanthes alba seed oil, 5 g of polydimethylsiloxane, 10 g of fermented grape seed oil, and 1.0 g of lavender essential oil respectively, put them into a beaker, and then stir and mix evenly to obtain the essence oil. F. Take a certain amount of freeze-dried efficacy core balls, put them into a container, such as a vial, a glass bottle, a plastic bottle, etc., and then add a certain amount of essence oil to obtain the composite essence oil efficacy core ball steady-state delivery system VIII, denoted as B8.

[0048] Example 9 Preparation of EUK134 Composite Essence Oil Efficacy Core Ball Steady-State Delivery System IX

[0049] A. Weigh 0.09 g of EUK134, 0.48 g of yeast protein, 0.3 g of recombinant collagen, 0.24 g of gellan gum, 0.18 g of fermented ganoderma lucidum polysaccharide, 0.45 g of neuraminic acid, 0.12 g of arbutin, 0.03 g of phloretin, 0.18 g of hydroxypropyl-β-cyclodextrin and 0.03 g of butanediol respectively, and put them into a beaker and mix evenly; B. Add 27.9 g of purified water and stir until the active ingredients are completely dissolved; C. Use a peristaltic pump to drop the above solution drop by drop into a thermally insulated liquid nitrogen bucket. The size of the liquid droplets is about 40 mg, and rapid freezing is carried out to obtain small ice balls; when dropping, nitrogen needs to be introduced into the target solution for protection to avoid oxidation loss of the active ingredients; D. Transfer the small ice balls formed by liquid nitrogen freezing to a freeze dryer and carry out freeze drying for 40 h. The cold trap temperature of the freeze dryer is controlled at about -70 °C, and the final temperature of the drying chamber is controlled at about 30 °C, then the ergothioneine composite freeze-dried efficacy core ball steady-state delivery system can be obtained, denoted as A9; E. Weigh 22 g of isononyl isononanoate, 37 g of caprylic / capric triglyceride, 5 g of shorea robusta seed fat, 20 g of limnanthes alba seed oil, 5 g of polydimethylsiloxane, 10 g of fermented grape seed oil and 1.0 g of lavender essential oil respectively, put them into a beaker, and then stir and mix evenly to obtain the essence oil; F. Take a certain amount of freeze-dried efficacy core balls, put them into a container, such as a vial, a glass bottle, a plastic bottle, etc., and then add a certain amount of essence oil, then the composite essence oil efficacy core ball steady-state delivery system No. IX can be obtained, denoted as B9.

[0050] Example 10 Preparation of the copper peptide complex essence oil efficacy core ball steady-state delivery system No. X

[0051] A. Weigh 0.24 g of copper peptide, 0.36 g of recombinant type III collagen, 0.6 g of yeast β-glucan, 0.45 g of sodium hyaluronate, 0.18 g of nicotinamide, 0.09 g of ectoin, 0.09 g of Vc ethyl ether, 0.45 g of hydroxypropyl-β-cyclodextrin and 0.06 g of phloretin respectively, and put them into a beaker and mix evenly; B. Add 27.48 g of purified water and stir until the active ingredients are completely dissolved; C. Use a peristaltic pump to drop the above solution drop by drop into a thermally insulated liquid nitrogen bucket. The size of the liquid droplets is about 40 mg, and rapid freezing is carried out to obtain small ice balls; when dropping, nitrogen needs to be introduced into the target solution for protection to avoid oxidation loss of the active ingredients; D. Transfer the small ice balls formed by liquid nitrogen freezing to a freeze dryer and carry out freeze drying for 40 h. The cold trap temperature of the freeze dryer is controlled at about -70 °C, and the final temperature of the drying chamber is controlled at about 30 °C, then the ergothioneine composite freeze-dried efficacy core ball steady-state delivery system can be obtained, denoted as A10; E. Weigh 22 g of isononyl isononanoate, 37 g of glyceryl caprylate / caprate, 5 g of shorea robusta seed fat, 20 g of limnanthes alba seed oil, 5 g of polydimethylsiloxane, 10 g of fermented grape seed oil, and 1.0 g of lavender essential oil, put them into a beaker, and then stir and mix evenly to obtain the essence oil; F. Take a certain amount of freeze-dried functional core balls, put them into a container, such as a vial, a glass bottle, a plastic bottle, etc., and then add a certain amount of essence oil to obtain the composite essence oil functional core ball steady-state delivery system No. X, denoted as B10.

[0052] Example 11 Preparation of the composite essence oil functional core ball steady-state delivery system No. XI containing copper tripeptide

[0053] A. Weigh 0.15 g of copper tripeptide, 0.06 g of niacinamide, 0.3 g of recombinant fibronectin, 0.36 g of pullulan, 0.3 g of sodium hyaluronate, 0.27 g of L-theanine, 0.15 g of trehalose, and 0.03 g of butanediol, put them into a beaker and mix evenly; B. Add 27.69 g of purified water and stir until the active ingredients are completely dissolved; C. Use a peristaltic pump to drop the above solution into a thermally insulated liquid nitrogen bucket drop by drop. The droplet size is about 40 mg, and quickly freeze to obtain small ice balls; when dropping, nitrogen needs to be introduced into the target solution for protection to avoid oxidation loss of the active ingredients; D. Transfer the small ice balls formed by liquid nitrogen freezing to a freeze dryer and perform freeze drying for 40 h. The cold trap temperature of the freeze dryer is controlled at about -70 °C, and the final temperature of the drying chamber is controlled at about 30 °C to obtain the ergothioneine composite freeze-dried functional core balls, denoted as A11; E. Weigh 22 g of isononyl isononanoate, 37 g of glyceryl caprylate / caprate, 5 g of shorea robusta seed fat, 20 g of limnanthes alba seed oil, 5 g of polydimethylsiloxane, 10 g of fermented grape seed oil, and 1.0 g of lavender essential oil, put them into a beaker, and then stir and mix evenly to obtain the essence oil; F. Take a certain amount of freeze-dried functional core balls, put them into a container, such as a vial, a glass bottle, a plastic bottle, etc., and then add a certain amount of essence oil to obtain the composite essence oil functional core ball steady-state delivery system No. XI, denoted as B11.

[0054] Detection Example 1 Appearance of the composite freeze-dried functional core ball steady-state delivery system and the composite essence oil functional core ball steady-state delivery system

[0055] Take pictures with a camera to characterize the appearance morphology diagrams of the composite freeze-dried functional core ball steady-state delivery system and the composite essence oil functional core ball steady-state delivery system, and conduct comparative analysis.

[0056] 1) Ergothioneine complex essence oil efficacy core sphere steady delivery system series: Figure 1 As can be seen from A1, A2, and A3 in the figure, after freeze-drying, white ergothioneine complex freeze-dried efficacy core sphere steady delivery systems, namely beauty core spheres, can be obtained in Examples 1-3. Most of the small spheres are in good spherical shape and the surface is relatively smooth. There are a few cracks on the surface of the small spheres, which are mainly caused by uneven internal stress during freezing and do not affect subsequent use. From the appearance of the samples, there is no obvious difference among the three samples. After adding the essence oil, the essence oil quickly fills the pores of the freeze-dried core spheres, obtaining the complex essence oil efficacy core sphere steady delivery systems B1, B2, and B3. The perfect spherical structure appearance remains intact, and the structural stability of the efficacy core spheres and the shelf-life stability of the active substances have also been significantly improved.

[0057] 2) Glutathione complex essence oil efficacy core sphere steady delivery system series: Figure 2 A4 and A5 in the figure are glutathione complex freeze-dried efficacy core sphere steady delivery systems from Examples 4 and 5. In samples A4 and A5, most of the white small spheres are in good spherical shape and the surface is relatively smooth. There are a few cracks on the surface of the small spheres, which are mainly caused by uneven internal stress during freezing and do not affect subsequent use. After adding the essence oil, the complex essence oil efficacy core spheres B4 and B5 are obtained. The perfect spherical structure appearance remains intact, and the structural stability of the efficacy core spheres and the shelf-life stability of the active substances have also been significantly improved.

[0058] 3) Anthocyanin-Vc complex essence oil efficacy core sphere steady delivery system: Figure 3 It is an anthocyanin-Vc complex freeze-dried efficacy core sphere steady delivery system from Examples 6 and 7. In samples A6 and A7, most of the rose-colored small spheres are in good spherical shape and the surface is relatively smooth. There are a few cracks on the surface of the small spheres, which are mainly caused by uneven internal stress during freezing and do not affect subsequent use. After adding the essence oil, the complex essence oil efficacy core spheres B6 and B7 are obtained. The color of the core spheres becomes brighter, the perfect spherical structure appearance remains intact, and the structural stability of the efficacy core spheres and the shelf-life stability of the active substances have also been significantly improved.

[0059] 4) EUK134 complex essence oil efficacy core sphere steady delivery system: Figure 4 It is an EUK134 complex freeze-dried efficacy core sphere steady delivery system from Examples 8 and 9. In samples A8 and A9, most of the yellow small spheres are in good spherical shape and the surface is relatively smooth. There are a few cracks on the surface of the small spheres, which are mainly caused by uneven internal stress during freezing and do not affect subsequent use. After adding the essence oil, the complex essence oil efficacy core spheres B8 and B9 are obtained. The color of the core spheres becomes brighter, the perfect spherical structure appearance remains intact, and the structural stability of the efficacy core spheres and the shelf-life stability of the active substances have also been significantly improved.

[0060] 5) Blue Copper Peptide Complex Essence Oil Efficacy Core Sphere Steady Delivery System: Figure 5 It is a blue copper peptide complex freeze-dried efficacy core sphere steady delivery system, from Examples 10 and 11. In samples A10 and A11, most of the blue spheres have a good spherical shape and a relatively smooth surface. There are a few cracks on the surface of the spheres, which are mainly caused by uneven internal stress during freezing and do not affect subsequent use. After adding the essence oil, the composite essence oil efficacy core sphere steady delivery systems B10 and B11 are obtained. The color of the core spheres becomes brighter, and the perfect spherical structure appearance remains intact. The structural stability of the efficacy core spheres and the shelf-life stability of the active substances have also been significantly improved.

[0061] Test Example 2 Appearance of the Essence Emulsion of the Composite Essence Oil Efficacy Core Sphere Steady Delivery System

[0062] Based on the composite essence oil efficacy core spheres, fresh essence emulsions can be prepared, namely the composite efficacy core sphere steady delivery system essence emulsions. See the application cases for details. Take pictures with a camera to characterize the essence emulsion based on the composite efficacy core spheres and conduct comparative analysis ( Figure 6 ).

[0063] From Figure 6 it can be seen that C2, C3, C4, C5, C6, and C7 are milk cap-type essence emulsions. This is mainly because emulsifier components such as Tween 20, laureth-4, and PEG-40 hydrogenated castor oil are added to the solvent solution. When shaking to prepare the essence emulsion, the efficacy core sphere steady delivery system dissolves in the solvent solution, and at the same time, the essence oil is emulsified to form fine droplets. After standing for a period of time, the droplets float up, and the milk cap-type efficacy core sphere essence emulsion can be obtained. In contrast, C8, C9, C10, and C11 are double-layer transparent essence liquids. This is mainly because no emulsifier is added to the solvent solution. Although the essence oil liquid will become fine droplets when shaking to prepare the essence emulsion, without an emulsifier, a stable emulsion cannot be formed. After standing for a period of time, the oil and water phases separate to obtain a double-layer transparent essence liquid. The double-layer transparent essence liquid does not affect consumers' use. Instead, when applied, it is easier to form a protective layer on the skin surface.

[0064] Test Example 3 Scanning Electron Microscope Images

[0065] Figure 7Scanning electron micrographs of four samples, namely A3, A5, A7, and A9. The steady-state delivery system of the efficacy core spheres was gently broken apart and then observed using a scanning electron microscope. As can be seen from the figure, the interior of the small spheres is a uniform layered structure, and there are uniformly distributed micron-scale channels between the layers. When rapidly frozen in liquid nitrogen, the active substances dissolved in water quickly precipitate to form extremely small crystals. Then, during freeze-drying, as the ice crystals sublime, water vapor forms micron-scale water vapor channels, and at the same time, the tiny active substance crystals are connected into a continuous sheet to form a layered structure. Due to the very rapid liquid nitrogen freezing, the microstructure of the entire small sphere is very uniform. The active substance layer is very thin, basically less than 1 micron, which ensures that the active substances can dissolve extremely rapidly when rehydrated.

[0066] Detection Example 4 Stability

[0067] Active ingredients such as ergothioneine, glutathione, anthocyanins, copper peptides, vitamin C, and EUK134 have poor stability, especially in aqueous formulation systems, where they are extremely prone to oxidation, complexation, or decomposition, resulting in the loss of biological activity.

[0068] Referring to the evaluation of the stability of cosmetics, through a 45°C accelerated experiment, the stability of the above-mentioned composite freeze-dried efficacy core sphere steady-state delivery system and the composite essential oil efficacy core sphere steady-state delivery system was evaluated and compared with their control essence solutions. For the composite freeze-dried efficacy core sphere steady-state delivery system and the composite essential oil efficacy core sphere steady-state delivery system, an accelerated experiment was first carried out, and then a solution with a certain concentration prepared from them was subjected to detection and analysis. Taking the initial concentration of the target active ingredient as 100%, the percentage of the retained concentration of the target active ingredient in the initial concentration was measured at different aging times. The results are shown in the following table.

[0069] A. Series of samples of the ergothioneine composite efficacy core sphere steady-state delivery system

[0070] As can be seen from Table 1, after 28 days of accelerated experiment, the content or concentration of ergothioneine in the ergothioneine essence solution decreased by approximately 10%. The change in ergothioneine in the three ergothioneine composite freeze-dried efficacy core spheres was very small, decreasing by less than 1% (about 0.8%). This shows that the stability of ergothioneine is greatly improved in the composite freeze-dried efficacy core spheres. In the ergothioneine composite essential oil efficacy core sphere steady-state delivery system, the content of ergothioneine hardly changed, decreasing by about 0.1%, which is approximately one-eighth of the decrease in the freeze-dried efficacy core spheres. This indicates that adding essential oil to the freeze-dried efficacy core spheres can further block the influence of oxygen and even light on ergothioneine, further improving the stability of ergothioneine.

[0071] Table 1. Stability of the series of products of the ergothioneine composite efficacy core sphere steady-state delivery system

[0072] B. Series samples of glutathione composite efficacy core ball steady delivery system

[0073] As can be seen from Table 2, the stability of glutathione is relatively poor. After 1-day accelerated experiment, about 99% of the glutathione in the control essence has been oxidized and degraded, and the content is only about 0.3% of the original content. After 7 days, it cannot be detected at all. The change of glutathione in the two glutathione composite freeze-dried efficacy core ball steady delivery systems is very small. After 28 days, the decrease is less than 2% (about 1.9%). This shows that the stability of glutathione is greatly improved in the composite freeze-dried efficacy core ball steady delivery system. In the glutathione composite essence oil efficacy core ball steady delivery system, the change of glutathione content is even smaller, decreasing by about 0.9% or so, less than half of the decrease amount of the freeze-dried efficacy core ball. This indicates that adding essence oil to the freeze-dried efficacy core ball steady delivery system can further block the influence of oxygen and even light on glutathione, and further improve its stability.

[0074] Table 2. Stability of glutathione composite efficacy core ball series products

[0075] C. Series samples of anthocyanin-Vc composite efficacy core ball steady delivery system

[0076] As can be seen from Table 3, the stability of anthocyanin is relatively poor. After 1-day accelerated experiment, about 99% of the glutathione in the control essence has been oxidized and degraded, and the content is only about 1% of the original content. After 7 days, it cannot be detected at all. The change of anthocyanin in the two anthocyanin-Vc composite freeze-dried efficacy core ball steady delivery systems is very small. After 28 days, the decrease is less than 2% (about 1.7%). This shows that the stability of anthocyanin is greatly improved in the composite freeze-dried efficacy core ball steady delivery system. In the anthocyanin-Vc composite essence oil efficacy core ball steady delivery system, the change of anthocyanin content is even smaller, decreasing by about 0.7% or so, less than half of the decrease amount of the freeze-dried efficacy core ball steady delivery system. This indicates that adding essence oil to the freeze-dried efficacy core ball steady delivery system can further block the influence of oxygen and even light on anthocyanin, and further improve its stability.

[0077] Table 3. Stability of anthocyanin in anthocyanin-Vc composite efficacy core ball steady delivery system series products

[0078] Similarly, as can be seen from Table 4, after 1-day accelerated experiment, more than 99% of vitamin C in the control essence has been oxidized and degraded, and the content is only about 1% of the original content. After 7 days, it cannot be detected at all. The change of Vc in the two anthocyanin-Vc composite freeze-dried efficacy core sphere steady-state delivery systems is very small. After 28 days, the decrease is less than 2% (about 1.9%). This indicates that in the composite freeze-dried efficacy core sphere steady-state delivery system, the stability of Vc is greatly improved. In the anthocyanin-Vc composite essence oil efficacy core sphere, the change of Vc content is even smaller, with a decrease of about 0.65%, which is about one-third of the decrease in the freeze-dried efficacy core sphere steady-state delivery system. This shows that adding essence oil to the freeze-dried efficacy core sphere steady-state delivery system can further block the influence of oxygen and even light on Vc, and further improve its stability.

[0079] Table 4. Vc Stability in Anthocyanin-Vc Composite Efficacy Core Sphere Steady-State Delivery System Series Products

[0080] D, EUK134 Composite Efficacy Core Sphere Steady-State Delivery System Series Samples

[0081] As can be seen from Table 5, after 28-day accelerated experiment, the content or concentration of EUK134 in the EUK134 essence has decreased by about 13%. The change of EUK134 in the two EUK134 composite freeze-dried efficacy core sphere steady-state delivery systems is very small, with a decrease of about 1%. This indicates that in the composite freeze-dried efficacy core sphere steady-state delivery system, the stability of EUK134 is greatly improved. In the EUK134 composite essence oil efficacy core sphere steady-state delivery system, the content of EUK134 hardly changes, with a decrease of about 0.3%, which is about one-third of the decrease in the freeze-dried efficacy core sphere steady-state delivery system. This shows that adding essence oil to the freeze-dried efficacy core sphere steady-state delivery system can further block the influence of oxygen and even light on EUK134, and further improve its storage stability.

[0082] Table 5. Stability of EUK134 Composite Efficacy Core Sphere Steady-State Delivery System Series Products

[0083] F, Copper Peptide Composite Efficacy Core Sphere Steady-State Delivery System Series Samples

[0084] As can be seen from Table 6, after 28 days of accelerated testing, the content or concentration of copper tripeptide in the copper tripeptide essence decreased by about 17%. The change in copper tripeptide in the two copper tripeptide composite freeze-dried efficacy core sphere steady-state delivery systems was very small, decreasing by about 0.9%. This indicates that the stability of copper tripeptide was greatly improved in the composite freeze-dried efficacy core sphere steady-state delivery system. In the EUK134 composite essence oil efficacy core sphere steady-state delivery system, the content of EUK134 hardly changed, decreasing by about 0.2%, which was about one-fourth of the decrease in the freeze-dried efficacy core sphere steady-state delivery system. This shows that adding essence oil to the freeze-dried efficacy core sphere steady-state delivery system can further block the effects of oxygen and light on copper tripeptide and further improve its storage stability.

[0085] Table 6. Stability of Copper Tripeptide Composite Efficacy Core Sphere Steady-State Delivery System Series Products

[0086] Detection Example 5 Transdermal Absorption

[0087] For the application cases of different active ingredient composite essence oil efficacy core sphere steady-state delivery systems, corresponding control essence solutions were selected, and systematic transdermal experimental efficacy evaluations were conducted. The evaluation method referred to the "In Vitro Test Method for Skin Absorption of Chemicals", and the evaluation results are as follows: Table 7. Transdermal Experimental Evaluation Data of Active Ingredient Composite Essence Oil Efficacy Core Spheres and Their Control Essence Solutions

[0088]

[0089]

[0090]

[0091] For the ergothioneine series of Application Examples 1 - 3, as can be seen from Table 7, the transdermal effect of the ergothioneine composite efficacy core sphere steady-state delivery system essence emulsion II was significantly better than that of the ergothioneine control essence solution, and the 24-hour transdermal amount was nearly 3 times that of the control essence solution. The transdermal effect of the ergothioneine composite efficacy core sphere steady-state delivery system essence emulsion III with a penetration enhancer was even better, and the 24-hour transdermal amount was more than 4 times that of the control essence solution.

[0092] For the glutathione series of Application Examples 4 - 6, only the 1-hour and 4-hour transdermal effects were detected because glutathione is very unstable and easily oxidized and deteriorated. As can be seen from Table 7, the transdermal effect of the glutathione composite efficacy core sphere steady-state delivery system essence emulsion IV was significantly better than that of the glutathione control essence solution, and the 4-hour transdermal amount was about 2 times that of the control essence solution. The transdermal effect of the glutathione composite efficacy core sphere steady-state delivery system essence emulsion V with a penetration enhancer was even better, and the 4-hour transdermal amount was about 3 times that of the control essence solution.

[0093] For anthocyanin-Vc series application examples 7-9, due to the poor stability of anthocyanin and Vc, only the 1h and 4h transdermal effects were tested. As can be seen from Table 7, the transdermal effect of anthocyanin-Vc composite core ball steady-state delivery system essence lotion VI is significantly better than the anthocyanin-Vc control essence. The 4h transdermal amount of anthocyanin is about 2.5 times that of the control essence, and the 4h transdermal amount of Vc is about 2 times that of the control essence. The composite functional core ball steady-state delivery system essence lotion VII, which has a penetration enhancer, has an even better transdermal effect. The 4h transdermal amount of anthocyanin is about 4 times that of the control essence, and the 4h transdermal amount of Vc is about 3 times that of the control essence.

[0094] For EUK134 series application examples 10-12, as shown in Table 7, the transdermal performance of EUK134 Complex Functional Core-Sphere Steady-State Delivery System Essence Emulsion VIII was significantly better than that of the EUK134 control essence, with a 24-hour transdermal volume nearly double that of the control essence. EUK134 Complex Functional Core-Sphere Steady-State Delivery System Essence Emulsion IX, which added a penetration enhancer, achieved even better transdermal performance, with a 24-hour transdermal volume approximately three times that of the control essence.

[0095] For the Copper Peptide Series Application Examples 13-15, both Copper Peptide Complex Functional Core-Ball Steady-State Delivery Systems incorporate a penetration enhancer active ingredient. As shown in Table 7, the transdermal efficacy of Copper Peptide Complex Functional Core-Ball Steady-State Delivery System Essence Emulsions X and XI significantly outperformed the Copper Peptide Control Essence, with 24-hour transdermal penetration rates approximately four times that of the Control Essence.

[0096] Application Example 1 Ergothioneine Control Essence

[0097] (1) Weigh 86.6 g of purified water, 5.0 g of butylene glycol, 0.80 g of Chondrus crispus, and 0.40 g of raspberry ketone in sequence, place them in a container, and heat at 40°C with stirring until they are evenly dissolved; (2) After stirring and cooling, add 5.0g of Rosa damascena flower water, 2.0g of 1,2-pentanediol and 0.20g of ergothioneine in sequence, stir evenly, and then discharge the material to obtain the ergothioneine control essence solution for subsequent evaluation.

[0098] Application Example 2 Ergothioneine Complex Efficacy Core Ball Steady-state Delivery System Essence Emulsion II

[0099] (1) Weigh 1.0 g of ergothioneine compound essential oil functional core ball steady-state delivery system B2 (including 0.95 g of essential oil and 0.05 g of A2 functional core ball) and place it into a vial; (2) Meixin ball solvent configuration: Weigh 91.5 g of pure water, 2.0 g of butylene glycol, 0.5 g of tremella polysaccharide, 0.2 g of glucosylglycerol, 0.2 g of chondrus crispus, 0.5 g of PEG-40 hydrogenated castor oil, 1.0 g of Tween-20, 0.5 g of hydroxyacetophenone, 1.0 g of 1,2-hexanediol, 0.5 g of 1,2-pentanediol and 2.1 g of rosa damascena flower water in sequence, and put them into a container; heat and stir at 40 °C until dissolved uniformly, and then discharge after cooling with stirring to obtain the Meixinqiu solvent solution.

[0100] (3)Use a pipette to add 3 mL of the Meixinqiu solvent solution to a vial containing 1.0 g of the composite essence oil efficacy core ball steady-state delivery system B2. (4)Gently shake, the composite freeze-dried efficacy core ball steady-state delivery system will dissolve in the solvent solution, and at the same time the solvent solution will emulsify the essence oil to obtain an essence emulsion. After standing for 5 min, part of the essence emulsion floats up, and the milk cap type ergothioneine composite efficacy core ball steady-state delivery system essence emulsion II can be obtained (see Figure 6 Essence emulsion, C2); for subsequent evaluation.

[0101] Application Example 3 Ergothioneine Composite Efficacy Core Ball Steady-State Delivery System Essence Emulsion III

[0102] (1)Weigh 1.0 g of the ergothioneine composite essence oil efficacy core ball steady-state delivery system B3 (where: 0.95 g of essence oil, 0.05 g of A3 efficacy core ball) and put it into a vial. (2)Configuration of the Meixinqiu solvent solution: Weigh 91.5 g of pure water, 2.0 g of butylene glycol, 0.5 g of tremella polysaccharide, 0.2 g of glucosylglycerol, 0.2 g of chondrus crispus, 0.5 g of PEG-40 hydrogenated castor oil, 1.0 g of Tween-20, 0.5 g of hydroxyacetophenone, 1.0 g of 1,2-hexanediol, 0.5 g of 1,2-pentanediol and 2.1 g of rosa damascena flower water in sequence, and put them into a container; heat and stir at 40 °C until dissolved uniformly, and then discharge after cooling with stirring to obtain the Meixinqiu solvent solution.

[0103] (3)Use a pipette to add 3 mL of the Meixinqiu solvent solution to a vial containing 1.0 g of the composite essence oil efficacy core ball steady-state delivery system B3. (4)Gently shake, the composite freeze-dried efficacy core ball steady-state delivery system will dissolve in the solvent solution, and at the same time the solvent solution will emulsify the essence oil to obtain an essence emulsion. After standing for 5 min, part of the essence emulsion floats up, and the milk cap type ergothioneine composite efficacy core ball steady-state delivery system essence emulsion III can be obtained (see Figure 6 Essence emulsion, C3); for subsequent evaluation.

[0104] Application Example 4 Glutathione Control Essence Liquid

[0105] (1)Weigh 86.6 g of pure water, 5.0 g of butylene glycol, 0.80 g of Chondrus crispus, and 0.40 g of raspberry ketone in sequence, put them into a container, and heat and stir at 40 °C until dissolved evenly; (2)After stirring and cooling, add 5.0 g of Rosa damascena flower water, 2.0 g of 1,2-pentanediol, and 0.20 g of glutathione in sequence, stir for about 10 minutes to obtain a uniform solution, then discharge to obtain glutathione control essence; for subsequent evaluation.

[0106] Application Example 5 Glutathione Composite Efficacy Core Sphere Steady Delivery System Essence Emulsion IV

[0107] (1)Weigh 1.0 g of glutathione composite essence oil efficacy core sphere steady delivery system B4 (wherein, 0.95 g of essence oil and 0.05 g of A4 efficacy core sphere) and put it into a vial; (2)Preparation of the core sphere solvent solution: Weigh 94.5 g of pure water, 1.8 g of butylene glycol, 0.5 g of Glycine max (L.) Merr. seed extract, 0.5 g of cocoyl glucoside, 0.8 g of PEG stearate, 0.3 g of hydroxyethyl cellulose, 0.1 g of hydrogenated starch hydrolysate, 0.5 g of p-hydroxyacetophenone, and 1.0 g of 1,2-pentanediol in sequence, put them into a container; heat and stir at 40 °C until dissolved evenly, and after stirring and cooling, discharge to obtain the core sphere solvent solution.

[0108] (3)Use a pipette to add 3 mL of the core sphere solvent solution to the vial containing 1.0 g of the composite essence oil efficacy core sphere steady delivery system B4; (4)Gently shake, the composite freeze-dried efficacy core sphere steady delivery system will dissolve in the solvent solution, and at the same time the solvent solution will emulsify the essence oil to obtain an essence emulsion. After standing for 5 min, part of the essence emulsion floats up, and the milk cap type glutathione composite efficacy core sphere essence emulsion IV (see Figure 6 Essence emulsion, C4) can be obtained; for subsequent evaluation.

[0109] Application Example 6 Glutathione Composite Efficacy Core Sphere Steady Delivery System Essence Emulsion V

[0110] (1)Weigh 1.0 g of glutathione composite essence oil efficacy core sphere steady delivery system B5 (wherein: 0.95 g of essence oil and 0.05 g of A5 efficacy core sphere) and put it into a vial; (2)Preparation of the core sphere solvent solution: Weigh 94.5 g of purified water, 1.8 g of butylene glycol, 0.5 g of wild soybean seed extract, 0.5 g of cocoyl glucoside, 0.8 g of PEG stearate, 0.3 g of hydroxyethyl cellulose, 0.1 g of hydrogenated starch hydrolysate, 0.5 g of p-hydroxyacetophenone, and 1.0 g of 1,2-pentanediol in sequence and put them into a container; heat and stir at 40°C to dissolve evenly, stir and cool, then discharge the material to obtain the Meixinqiu solvent solution.

[0111] (3) Use a pipette to add 3 mL of the Meixinqiu solvent solution into the vial containing 1.0 g of the compound essential oil efficacy core ball steady-state delivery system B5; (4) Gently shake the compound freeze-dried functional core ball steady-state delivery system to dissolve in the solvent liquid, and the solvent liquid emulsifies the essential oil to obtain the essence emulsion. After standing for 5 minutes, the essence emulsion partially floats up to obtain the milk cap type glutathione compound functional core ball steady-state delivery system essence emulsion V (see Figure 6 Essence lotion, C5); for subsequent evaluation.

[0112] Application Example 7 Anthocyanin-Vc Control Essence

[0113] (1) Weigh 86.4 g of purified water, 5.0 g of butylene glycol, 0.80 g of Chondrus crispus, and 0.40 g of raspberry ketone in sequence, place them in a container, heat at 40°C, and stir until dissolved evenly; (2) After stirring and cooling, add 5.0 g of Rosa damascena flower water, 2.0 g of 1,2-pentanediol, 0.10 g of anthocyanin and 0.30 g of vitamin C in sequence and stir for about 10 minutes to obtain a uniform solution. The material can be discharged for subsequent evaluation.

[0114] Application Example 8 Anthocyanin-Vc Composite Efficacy Core Ball Steady-State Delivery System Essence Emulsion VI

[0115] (1) Weigh 1.0 g of anthocyanin-Vc composite essential oil functional core ball steady-state delivery system B6 (including 0.95 g of essential oil and 0.05 g of A6 functional core ball) and place it into a vial; (2) Meixin ball solvent configuration: 93.0 g of purified water, 1.5 g of Tween 80, 0.7 g of laureth-4, 0.5 g of xylitol glucoside, 0.6 g of anhydroxylitol, 0.5 g of sodium hyaluronate, 1.6 g of polyglycerol-10, 0.8 g of p-hydroxyacetophenone, and 0.8 g of hexylene glycol were weighed in sequence and placed in a container; heated and stirred at 40° C. until uniformly dissolved, stirred and cooled, and then discharged to obtain a Meixin ball solvent solution.

[0116] (3) Use a pipette to add 3 mL of the Meixinqiu solvent solution into the vial containing 1.0 g of the compound essential oil efficacy core ball steady-state delivery system B6; (4) Gently shake, and the composite freeze-dried efficacy core sphere steady-state delivery system will dissolve in the solvent solution. Meanwhile, the solvent solution emulsifies the essential oil to obtain an essential emulsion. After standing for 5 min, part of the essential emulsion floats up, and the milk cap type anthocyanin-Vc composite efficacy core sphere steady-state delivery system essential emulsion VI can be obtained (see Figure 6 essential emulsion, C6); for subsequent evaluation.

[0117] Application Example 9 Anthocyanin-Vc Composite Efficacy Core Sphere Steady-State Delivery System Essential Emulsion VII

[0118] (1) Weigh 1.0 g of the anthocyanin-Vc composite essential oil efficacy core sphere steady-state delivery system B7 (where: 0.95 g of essential oil and 0.05 g of A7 efficacy core sphere) and put it into a vial; (2) Preparation of the core sphere solvent solution: Weigh 93.0 g of purified water, 1.5 g of Tween 80, 0.7 g of laureth-4, 0.5 g of xylitol glucoside, 0.6 g of anhydroxylitol, 0.5 g of sodium hyaluronate, 1.6 g of polyglycerol-10, 0.8 g of p-hydroxyacetophenone, and 0.8 g of hexylene glycol in sequence and put them into a container; heat and stir at 40 °C until dissolved evenly. After stirring and cooling, discharge the solution to obtain the core sphere solvent solution.

[0119] (3) Use a pipette to add 3 mL of the core sphere solvent solution to the vial containing 1.0 g of the composite essential oil efficacy core sphere steady-state delivery system B7; (4) Gently shake, and the composite freeze-dried efficacy core sphere steady-state delivery system will dissolve in the solvent solution. Meanwhile, the solvent solution emulsifies the essential oil to obtain an essential emulsion. After standing for 5 min, part of the essential emulsion floats up, and the milk cap type anthocyanin-Vc composite efficacy core sphere steady-state delivery system essential emulsion VII can be obtained (see Figure 6 essential emulsion, C7); for subsequent evaluation.

[0120] Application Example 10 EUK134 Control Serum

[0121] (1) Weigh 86.7 g of purified water, 5.0 g of butanediol, 0.80 g of Chondrus crispus, and 0.40 g of raspberry ketone in sequence and put them into a container, heat and stir at 40 °C until dissolved evenly; (2) After stirring and cooling, add 5.0 g of Rosa damascena flower water, 2.0 g of 1,2-pentanediol, and 0.10 g of EUK134 in sequence, and stir for about 20 minutes to obtain a uniform solution, then discharge the solution; for subsequent evaluation.

[0122] Application Example 11 EUK134 Composite Efficacy Core Sphere Steady-State Delivery System Essential Emulsion VIII

[0123] (1) Weigh 1.0 g of the EUK134 composite essence oil efficacy core ball steady delivery system B8 (wherein: 0.95 g of essence oil and 0.05 g of A8 efficacy core ball) and put it into a vial; (2) Preparation of the core ball solvent solution: Weigh 94.5 g of purified water, 2.0 g of butylene glycol, 1.5 g of xylitol, 0.6 g of betaine, 0.5 g of xanthan gum, 0.4 g of glycerol polyether-26, 2.0 g of β-glucan, 0.3 g of trehalose glycoside, 0.6 g of p-hydroxyacetophenone, and 1.0 g of hexylene glycol in sequence and put them into a container; Heat and stir at 40 °C until dissolved uniformly, and then discharge after stirring and cooling to obtain the core ball solvent solution.

[0124] (3) Use a pipette to add 3 mL of the core ball solvent solution to the vial containing 1.0 g of the composite essence oil efficacy core ball steady delivery system B8; (4) Gently shake. The composite freeze-dried efficacy core ball steady delivery system will dissolve in the solvent solution, and at the same time, the solvent solution will emulsify the essence oil to obtain an essence emulsion. After standing for 5 min, part of the essence emulsion floats up, and the double-layer transparent EUK134 composite efficacy core ball steady delivery system essence emulsion VIII can be obtained (see Figure 6 Essence emulsion, C8); for subsequent evaluation.

[0125] Application Example 12 EUK134 Composite Efficacy Core Ball Steady Delivery System Essence Emulsion IX

[0126] (1) Weigh 1.0 g of the EUK134 composite essence oil efficacy core ball steady delivery system B9 (wherein: 0.95 g of essence oil and 0.05 g of A9 efficacy core ball) and put it into a vial; (2) Preparation of the core ball solvent solution: Weigh 94.5 g of purified water, 2.0 g of butylene glycol, 1.5 g of xylitol, 0.6 g of betaine, 0.5 g of xanthan gum, 0.4 g of glycerol polyether-26, 2.0 g of β-glucan, 0.3 g of trehalose glycoside, 0.6 g of p-hydroxyacetophenone, and 1.0 g of hexylene glycol in sequence and put them into a container; Heat and stir at 40 °C until dissolved uniformly, and then discharge after stirring and cooling to obtain the core ball solvent solution.

[0127] (3) Use a pipette to add 3 mL of the core ball solvent solution to the vial containing 1.0 g of the composite essence oil efficacy core ball steady delivery system B9; (4) Gently shake. The composite freeze-dried efficacy core ball steady delivery system will dissolve in the solvent solution, and at the same time, the solvent solution will emulsify the essence oil to obtain an essence emulsion. After standing for 5 min, part of the essence emulsion floats up, and the double-layer transparent EUK134 composite efficacy core ball steady delivery system essence emulsion IX can be obtained (see Figure 6Essence Lotion, C9); for subsequent evaluation.

[0128] Application Example 13 Copper Peptide Control Essence

[0129] (1) Weigh 86.6 g of purified water, 5.0 g of butylene glycol, 0.80 g of Chondrus crispus, and 0.40 g of raspberry ketone in sequence, put them into a container, and heat and stir at 40 °C until dissolved evenly; After stirring and cooling, add 5.0 g of Rosa damascena flower water, 2.0 g of 1,2-pentanediol, and 0.20 g of copper peptide in sequence, stir for about 10 minutes to obtain a homogeneous solution, and then discharge; for subsequent evaluation.

[0130] Application Example 14 Copper Peptide Composite Efficacy Core Sphere Steady Delivery System Essence Lotion X

[0131] (1) Weigh 1.0 g of copper peptide composite essence oil efficacy core sphere steady delivery system B10 (where: essence oil 0.95 g, A10 efficacy core sphere 0.05 g) and put it into a vial; (2) Preparation of the core sphere solvent solution: Weigh 91.1 g of purified water, 2.0 g of butylene glycol, 1.2 g of xylitol, 2.0 g of glycerol, 0.5 g of sodium hyaluronate, 1.0 g of β-glucan, 0.5 g of trehalose glycoside, 0.7 g of p-hydroxyacetophenone, and 1.0 g of pentanediol in sequence, put them into a container; heat and stir at 40 °C until dissolved evenly, and then discharge after stirring and cooling to obtain the core sphere solvent solution.

[0132] (3) Use a pipette to add 3 mL of the core sphere solvent solution to the vial containing 1.0 g of the composite essence oil efficacy core sphere steady delivery system B10; (4) Gently shake, the composite freeze-dried efficacy core sphere steady delivery system will dissolve in the solvent solution, and at the same time the solvent solution will emulsify the essence oil to obtain the essence lotion. After standing for 5 min, part of the essence lotion floats up, and the double-layer transparent copper peptide composite efficacy core sphere steady delivery system essence lotion X can be obtained (see Figure 6 Essence Lotion, C10); for subsequent evaluation.

[0133] Application Example 15 Copper Peptide Composite Efficacy Core Sphere Steady Delivery System Essence Lotion XI

[0134] (1) Weigh 1.0 g of copper peptide composite essence oil efficacy core sphere steady delivery system B11 (where: essence oil 0.95 g, A11 efficacy core sphere 0.05 g) and put it into a vial; (2) Preparation of the core sphere solvent solution: Weigh 91.1 g of pure water, 2.0 g of butanediol, 1.2 g of xylitol, 2.0 g of glycerol, 0.5 g of sodium hyaluronate, 1.0 g of β-glucan, 0.5 g of trehalose glycoside, 0.7 g of p-hydroxyacetophenone, and 1.0 g of pentylene glycol in sequence, and put them into a container; heat and stir at 40 °C until dissolved evenly, and after stirring and cooling, the material can be discharged to obtain the Meixinqiu solvent solution.

[0135] (3) Use a pipette to add 3 mL of the Meixinqiu solvent solution to a vial containing 1.0 g of the composite essence oil efficacy core ball steady delivery system B11; (4) Gently shake, and the composite freeze-dried efficacy core ball steady delivery system will dissolve in the solvent solution. At the same time, the solvent solution will emulsify the essence oil to obtain an essence emulsion. After standing for 5 minutes, part of the essence emulsion floats up, and the double-layer transparent blue copper peptide composite efficacy core ball steady delivery system essence emulsion XI (see Figure 6 Essence emulsion, C11) can be obtained; for subsequent evaluation.

[0136] The above embodiments describe the basic principles, main features, and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited by the above embodiments. The content described in the above embodiments and the specification only illustrates the principle of the present invention. Without departing from the principle of the present invention, the present invention will have various changes and improvements, and these changes and improvements all fall within the protection scope of the present invention.

Claims

1. Composite essence oil efficacy core ball steady delivery system, characterized in that, It includes: Unstable small molecule active ingredients, biosynthetic active macromolecules, penetration enhancer molecules, functional small molecules and essence oil; the unstable small molecule active ingredients are selected from one or more of ergothioneine, glutathione, anthocyanin, copper peptide, vitamin C, ethyl bisiminomethylguaiacol manganese chloride active ingredients; the penetration enhancer molecules are selected from one or more of phloretin, menthol, hydroxypropyl-β-cyclodextrin, methyl-β-cyclodextrin, butylene glycol; the mass ratio of the unstable small molecule active ingredients, biosynthetic active macromolecules, penetration enhancer molecules to functional small molecules is 1:0.1-10:0.05-5:0.1-10:1000-10000; the composite essence oil efficacy core ball has a particle size range of 0.1-15mm.

2. The steady-state delivery system of the composite essence oil efficacy core ball according to claim 1, wherein: The biosynthetic active macromolecules are selected from one or more of fermented polysaccharides, fermented proteins, recombinant collagen, recombinant type III collagen, recombinant type XII collagen, recombinant fibronectin, yeast proteins, polyglutamic acid, pullulan, yeast polysaccharides, yeast β-glucan, sodium hyaluronate, xanthan gum, gellan gum, sodium DNA, fermented ganoderma lucidum polysaccharide components.

3. The steady-state delivery system of the composite essence oil efficacy core ball according to claim 1, characterized in that: The functional small molecules are selected from one or more of asiaticoside, madecassoside, L-theanine, sialic acid, arbutin, niacinamide, tranexamic acid, ectoin, Vc glucoside, catechins, trehalose, nonapeptide-1, snake venom-like peptide, conotoxin-like peptide, acetyl hexapeptide-8, mannitol active ingredients.

4. The steady-state delivery system of the composite essence oil efficacy core ball according to claim 1, characterized in that: The essence oil is selected from one or more of cetearyl octanoate / decanoate, isocetane, isododecane, jojoba seed oil, squalane, fermented peony seed oil, fermented sacha inchi oil, fermented rice bran oil, fermented grape seed oil, fermented vegetable oil, shorea robusta seed fat, corn germ oil, tocopheryl acetate, rapeseed oil, macadamia seed oil, isononyl isononanoate, ethylhexyl palmitate, caprylic / capric triglyceride, Limnanthes alba (meadowfoam) seed oil, sunflower seed oil, Rosa damascena flower oil, hydrogenated polyisobutene, dimethicone, lavender essential oil, tea tree essential oil, plant essential oil, essence.

5. The production process of the steady-state delivery system of the composite essence oil efficacy core ball according to any one of claims 1-4, characterized in that, It includes the following steps: First, prepare a composite freeze-dried efficacy core ball; then, when dispersing the efficacy core ball in the essence oil, the essence oil quickly fills the pores of the efficacy core ball to obtain a composite essence oil efficacy core ball.

6. The production process of the steady-state delivery system of the composite essence oil efficacy core ball according to claim 5, characterized in that, The specific steps are as follows: A. Mix the unstable small molecule active raw materials and biosynthetic active macromolecules evenly, then add purified water and stir to dissolve to obtain a clear and transparent solution. B. During the stirring process, add the penetration enhancer molecules and functional small molecules to the above solution and stir until all components are completely dissolved to obtain a target solution. C. Drop the target solution into a thermally insulated liquid nitrogen bucket; when dropping, it is necessary to introduce nitrogen protection into the target solution to avoid oxidation loss of the active ingredients. D. Freeze-dry the small ice balls formed by liquid nitrogen freezing to obtain a composite freeze-dried efficacy core ball. E. Disperse the efficacy core ball into the essence oil, and the essence oil quickly fills the pores of the efficacy core ball to obtain a composite essence oil efficacy core ball.

7. A preparation method of an efficacy skin care essence, characterized in that It includes the following steps: Mix the solvent solution with the essence oil efficacy core ball steady-state delivery system according to any one of claims 1-4, and gently shake to mix evenly to obtain a freshly prepared efficacy skin care essence; the solvent solution includes water, a moisturizing agent, and / or an emulsifier.

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