Kava liposome extraction method and cosmetic containing kava liposome

Abstract

The application discloses a kava liposome extraction method and a cosmetic containing the kava liposome and belongs to the field of cosmetic raw materials. The extraction steps comprise the following steps: crushing dry kava pepper roots, adding the roots into a broken wall liquid for enzymolysis, then killing the enzyme, filtering out fiber residues to obtain a composite liquid, adding gamma-cyclodextrin and hydroxypropyl methyl cellulose into the composite liquid, and stirring to obtain a mixed liquid containing kava liposomes. The broken wall liquid contains cellulase and pectinase. The adding mass of the gamma-cyclodextrin is 18% to 25% of the mass of the dry kava pepper roots. The application realizes efficient enrichment of kava lactones when the kava lactones are extracted, and is matched with a later encapsulation assembly. By utilizing the hydrophilic and hydrophobic differences of double phospholipid layers and hydrogen bond action, multiple protections of the kava lactones are constructed, the encapsulation rate and anti-interference ability are improved, in specific cosmetic products, a base pre-polymer network and a self-assembly encapsulation body are embedded, the finished product system is stable, and the finished product system has skin feeling and efficacy.

Description

Technical Field

[0001] This invention relates to a method for extracting kava liposomes and cosmetics containing kava liposomes, belonging to the field of cosmetic raw materials. Background Technology

[0002] Kava liposomes are nanoscale vesicle-like raw materials prepared by encapsulating kava lactone extracted from kava pepper root as the core active ingredient. They are used in soothing, anti-allergic, and anti-inflammatory repair cosmetics, addressing the issues of kava lactone's high lipid solubility, poor water solubility, and low transdermal absorption efficiency. Simultaneously, the vesicle structure of the liposomes protects kava lactone from environmental degradation, preserving its biological activity. Kava lactone, as the core lipid-soluble active ingredient of kava pepper, possesses multiple functions including inhibiting TRPV-1 channels, regulating GABA receptors (γ-aminobutyric acid type A receptors), and inhibiting P-glycoprotein efflux. It can achieve skin-soothing, anti-anxiety, anti-inflammatory, and anti-allergic skincare effects, and can also synergistically increase the intracellular concentration of other active ingredients in cosmetics. It is a high-quality raw material that combines emotional and functional skincare. However, kava lactone itself suffers from low extraction efficiency and easy interaction with cosmetic components, leading to inactivation. Even after encapsulation with liposomes, the core defects of traditional preparation processes and application systems remain unresolved.

[0003] First, the extraction rate of kavalactone is low. Traditional extraction methods often use organic solvents to directly extract the lipid-soluble fraction of *Peperomia scabra* root, only dissolving free kavalactone. Second, kavalactone liposomes have low encapsulation efficiency and poor structural stability. Traditional liposomes use only a single phospholipid bilayer as the membrane material, and the binding with kavalactone relies solely on hydrophobic interactions, making it prone to free kavalactone loss. Furthermore, preservatives commonly added in cosmetic systems can easily interact with the phospholipid membrane material through electrostatic or swelling reactions, disrupting the liposome bilayer structure and losing its protective effect on kavalactone activity. These defects arise because impurities in the extraction process directly affect the encapsulation efficiency of liposome preparation, and structurally unstable liposomes are easily inactivated in cosmetics. Ultimately, this results in poor efficacy stability and a poor user experience for kavalactone-based cosmetics, failing to meet the cosmetic industry's demand for highly efficient, stable, and rapidly effective active ingredients.

[0004] Therefore, developing a method for extracting kavalactone efficiently, preparing high-encapsulation-rate anti-interference liposomes, and achieving targeted delivery to inflammatory sites, as well as developing kavalactone extractants and cosmetics, has become a pressing technical problem for the industry. Summary of the Invention

[0005] To overcome the shortcomings of existing technologies, this invention provides a method for extracting kavalactones, which can accurately extract more kavalactones and provide cosmetics containing kavalactones with stronger protection during storage.

[0006] The technical solution adopted by this invention to solve its technical problem is:

[0007] In the first aspect, this application provides a method for extracting kava liposomes, the steps of which include: crushing dried kava pepper roots, adding them to a cell wall breaking solution for enzymatic hydrolysis, then inactivating the enzyme, filtering out the fiber residue to obtain a composite solution, adding γ-cyclodextrin and hydroxypropyl methylcellulose to the composite solution, and stirring to obtain a mixture containing kava liposomes;

[0008] The cell wall disruption liquid contains cellulase and pectinase;

[0009] The mass of the γ-cyclodextrin added is 18% to 25% of the mass of the dried pepper root.

[0010] The liposome extraction method provided in this application can specifically decompose polysaccharide components such as cellulose and pectin, break the cell wall structure of peppercorn root, release calvanolide originally bound to polysaccharides, and increase the content of free calvanolide. The supramolecular host compound (γ-cyclodextrin) can form a stable complex with calvanolide through intermolecular forces, achieving efficient enrichment of calvanolide, while removing impurities from the extract and improving the purity of calvanolide. A slightly excess of γ-cyclodextrin is beneficial for subsequent self-assembly and encapsulation with other components. Furthermore, the enzymatically hydrolyzed polysaccharides of the enzymatic hydrolysis product associate with hydroxypropyl methylcellulose through hydrogen bonding to form complex micelles, which can serve as a stable dispersant for subsequent encapsulation.

[0011] Furthermore, the mass concentration of the hydroxypropyl methylcellulose in the mixture is 1.5% to 2.0%. This helps ensure that the ether groups of HPMC (hydroxypropyl methylcellulose) coordinate with the amino and carboxyl groups of the subsequent encapsulating film material; and the composite micelles formed with the enzymatically hydrolyzed polysaccharide help improve the stability of the subsequent encapsulation structure.

[0012] Further, the mass ratio of the dried kava pepper root to the cell wall-breaking liquid is 1:10-12, the mass concentration of the cellulase in the cell wall-breaking liquid is 1.2%-1.5%, and the mass concentration of the pectinase in the cell wall-breaking liquid is 0.5%-0.7%. Besides centrifuging and eluting the mixture to obtain kava lactone, preferably, in subsequent steps, centrifugation and elution are not performed; the mixture containing kava liposomes is directly used for encapsulation. In this case, obtaining a sufficient concentration of kava lactone for subsequent encapsulation is particularly important. This material-to-liquid ratio and enzyme concentration ensure both the concentration of kava lactone in the enzymatic hydrolysate and provide sufficient space for the interaction of γ-cyclodextrin and HPMC.

[0013] Secondly, a cosmetic containing kava liposomes, comprising the mixture described in the first aspect.

[0014] Furthermore, the cosmetic preparation steps containing kava liposomes include:

[0015] Hydrogenated soybean lecithin, phytosterol palmitate and dioleoylphosphatidylethanolamine are dissolved in an organic solvent to obtain a membrane material solution. Under stirring, the mixture described in the first aspect is added dropwise to the membrane material solution. The organic solvent is removed by vacuum distillation, and after homogenization, a self-assembled encapsulated body is obtained.

[0016] The self-assembled encapsulator, sodium hyaluronate, panthenol, glyceryl polyether-26, and xanthan gum were mixed in water to obtain the cosmetic containing kava liposomes.

[0017] The self-assembled encapsulated body constructs a hierarchical structure in the dispersion system, from the outside to the inside, consisting of "outer aqueous phase - HPMC stabilizing layer - phospholipid bilayer - inner aqueous phase - γ-cyclodextrin - kavalactone". It can stably store kavalactone. The aqueous core (containing kavalactone-cyclodextrin inclusion complex) is located at the center, and the outer encapsulation is composed of a phospholipid bilayer (composed of lecithin, sterols and dioleoylphosphatidylethanolamine, etc.). There is a stereostabilizing layer (complex micelles formed by HPMC and enzymatically hydrolyzed polysaccharides) between the phospholipid bilayer and the outer aqueous phase.

[0018] This cosmetic product is specifically an essence water type. The carboxyl groups of sodium hyaluronate, the hydroxyl groups of panthenol, and xanthan gum form a supramolecular prepolymer network of the base material. The hydroxyl groups of the self-assembled encapsulating outer layer HPMC form hydrogen bonds with the carboxyl and hydroxyl groups of the base material prepolymer network, which allows the inclusion complex (referring to the overall structure of γ-cyclodextrin including kavalactone) to be uniformly embedded in the base material prepolymer network.

[0019] Furthermore, the organic solvent accounts for 80% to 90% of the mass of the membrane material liquid, and the mass ratio of the hydrogenated soybean lecithin, the phytosterol palmitate, and the dioleoylphosphatidylethanolamine in the membrane material liquid is 7:2:1.

[0020] At this dosage ratio, hydrogenated soybean lecithin provides a bilayer membrane structure for the base membrane material. Phytosterol palmitate is inserted into the phospholipid bilayer to regulate the membrane's fluidity and phase transition temperature, preventing gel aggregation of the membrane material due to temperature changes. Dioleoylphosphatidylethanolamine (DOPE) imparts dual active sites of amino and carboxyl groups to the membrane material, which not only improves the dispersibility of the inclusion complex in the aqueous phase but also provides abundant binding sites for subsequent integration with the supramolecular prepolymer network of the base material. Furthermore, the amino groups of DOPE form hydrogen bonds with the phosphate groups of hydrogenated soybean lecithin, reinforcing the phospholipid bilayer structure and improving the compatibility of the membrane material with the inner aqueous phase.

[0021] Furthermore, the mass ratio of the membrane material solution to the mixture is 1:0.8~0.9. This dosage ensures an effective concentration of calvaline while preventing inclusion body aggregation, and allows for supramolecular intercalation between the hydroxyl groups of γ-cyclodextrin, the ether groups of HPMC, and the amino and carboxyl groups of the membrane material. During the previous extraction, a slight excess of γ-cyclodextrin was used, and the remaining hydroxyl groups of γ-cyclodextrin can form hydrogen bonds with the amino groups of the phospholipid bilayer (provided by DOPE), further strengthening the intercalation structure.

[0022] Furthermore, the cosmetic containing kava liposomes comprises, by weight, 8%–11% of the self-assembled encapsulating body, 1.2%–1.8% of the sodium hyaluronate, 0.7%–1% of the panthenol, 6%–9% of the glycerol polyether-26, 0.1%–0.15% of the xanthan gum, with the balance being water. This allows the self-assembled encapsulating body to be evenly distributed when embedded in the supramolecular prepolymer network of the base material, while avoiding excessive network cross-linking and a sticky feel caused by excessive liposomes.

[0023] Furthermore, the sodium hyaluronate comprises a low molecular weight component with a molecular weight below 1000 kDa and a high molecular weight component with a molecular weight above 1000 kDa, wherein the mass ratio of the low molecular weight component to the high molecular weight component is 1:2. Xanthan gum forms hydrogen bonds with glycerol polyether-26, and the low molecular weight component and the high molecular weight component of the sodium hyaluronate are intertwined. At the same time, panthenol forms hydrogen bonds with sodium hyaluronate and xanthan gum respectively, ultimately forming a three-dimensional interwoven prepolymer network with more reactive binding sites.

[0024] Furthermore, before being added to the membrane material solution, the mixture is first mixed with hexanediol, and the amount of hexanediol used is 0.05% to 0.1% of the mass of the mixture. During subsequent encapsulation, the hydroxyl groups of hexanediol can form weak hydrogen bonds with the amino groups of DOPE and the phosphate hydroxyl groups of phospholipids to strengthen the encapsulation structure.

[0025] The beneficial effects of this invention are: This invention achieves efficient enrichment of kavalactone during extraction and adapts it to subsequent encapsulation assembly. By utilizing the differences in hydrophilicity and hydrophobicity of the biphospholipid layer and hydrogen bonding, multiple protections for kavalactone are constructed, improving the encapsulation rate and anti-interference ability. In specific cosmetic products, a base material prepolymer network and self-assembled encapsulation body are constructed, making the finished product system stable and possessing both skin feel and efficacy. Detailed Implementation

[0026] This application provides a method for extracting kava liposomes, comprising the following steps: pulverizing dried kava pepper roots, adding them to a cell wall disruption solution for enzymatic hydrolysis, then inactivating the enzymes, filtering out fibrous residue to obtain a composite solution, adding γ-cyclodextrin and hydroxypropyl methylcellulose to the composite solution, and stirring to obtain a mixture containing kava liposomes. The cell wall disruption solution contains cellulase and pectinase; the mass of γ-cyclodextrin added is 18%~25% of the mass of the dried kava pepper roots.

[0027] Using this mixture, calvaline can then be obtained using conventional separation methods, such as centrifugation and elution. Alternatively, this application can directly encapsulate the mixture to form a protective structure for calvaline, allowing for direct application in cosmetics in one step.

[0028] Such cosmetic preparation steps include:

[0029] Hydrogenated soybean lecithin, phytosterol palmitate and dioleoylphosphatidylethanolamine were dissolved in an organic solvent to obtain a membrane material solution. The mixture was added dropwise to the membrane material solution under stirring. The organic solvent was removed by vacuum distillation. After homogenization, a self-assembled encapsulated body was obtained.

[0030] A cosmetic containing kava liposomes was obtained by mixing a self-assembled encapsulator, sodium hyaluronate, panthenol, glyceryl polyether-26, and xanthan gum in water.

[0031] The specific steps for extraction are as follows:

[0032] Take dried kava pepper roots and grind them to 60-80 mesh. Add an enzymatic hydrolysate (containing 1.2-1.5% cellulase, 0.5-0.7% pectinase, 0.1% Tween-80 phosphate buffer, pH 4.8-5.2) at a material-to-liquid ratio of 1:10-12. Enzymatically hydrolyze in a water bath at 42-45℃ for 3-3.5 hours. After enzymatic hydrolysis, heat to 80-85℃ to inactivate the enzyme for 10 minutes. Filter to remove coarse fiber residue to obtain an enzymatic hydrolysate containing free kava lactone. Simultaneously add 1.5-2.0% hydroxypropyl methylcellulose (HPMC) and 18%-25% γ-cyclodextrin by weight of dried kava pepper root powder to the enzymatic hydrolysate. Incorporate for 2 hours at 40-42℃ and 200-250 r / min to obtain a mixed solution.

[0033] The specific steps for preparing cosmetic products are as follows:

[0034] Hydrogenated soybean lecithin, phytosterol palmitate, and dioleoylphosphatidylethanolamine were weighed at a mass ratio of 7:2:1. These three components were dissolved in anhydrous ethanol-propylene glycol mixture (volume ratio 3:1, with the organic solvent accounting for 80%–90% of the membrane solution mass). The mixture was stirred in a water bath at 52–55°C until completely dissolved to obtain the membrane solution. The above mixed aqueous phase was added dropwise to the membrane solution at a mass ratio of membrane solution:mixture = 1:0.8–0.9 at 1–2 drops / second. The mixture was stirred and emulsified at 52–55°C and a speed of 400–450 r / min for 30 min. The organic solvent was removed by vacuum distillation at 52–55°C (distillation rate 2 mL / min). High-pressure homogenization was continued at 50–55°C (pressure 90–100 MPa, 3–4 cycles). The mixture was then microfiltered through a 0.1 μm polyethersulfone membrane to obtain the self-assembled encapsulated body.

[0035] Weigh the raw materials by mass percentage: 8-11% self-assembled encapsulant, 1.2-1.8% sodium hyaluronate (dual molecular weight, low molecular weight 1000 kDa + high molecular weight 1000 kDa, mass ratio 1:2), 0.7-1.0% panthenol, 6-9% glycerol polyether-26, 0.1-0.15% xanthan gum, and deionized water to 100%. Add glycerol polyether-26 and xanthan gum to deionized water and stir at 65-70℃ until completely dissolved. Cool to 50-55℃, add dual molecular weight sodium hyaluronate and panthenol, and stir for 30 min to obtain the base solution. Cool the base solution to 30-35℃, and add the self-assembled encapsulant dropwise while stirring at 350-400 r / min. After the addition is complete, continue stirring for 25 min. Filter through a 0.22 μm microfiltration membrane to obtain the essence water.

[0036] In the above steps, cellulase and pectinase break the covalent bond network of the cell wall, releasing bound calvanolactone. After filtration, HPMC and γ-cyclodextrin are added simultaneously. γ-cyclodextrin adapts to the molecular structure of calvanolactone and forms a stable supramolecular pre-assembly through hydrophobic interactions and van der Waals forces, converting the lipid-soluble calvanolactone into a water-soluble form and preventing its precipitation in the aqueous phase. HPMC and the enzymatic hydrolysis products form micelles as stabilizers, improving the dispersion stability of the inclusion complex in the aqueous phase and laying the foundation for subsequent self-assembly.

[0037] The self-assembly forms a hierarchical structure of a stable layer, a phospholipid bilayer, an inner aqueous phase, γ-cyclodextrin, and kavalactone. The outer HPMC stabilizing layer can resist the interference of preservatives and surfactants in cosmetics. The phospholipid bilayer forms a physical barrier to protect the core components. The γ-cyclodextrin-kavalactone complex in the inner aqueous phase stably retains the activity of kavalactone, greatly improving the encapsulation efficiency and structural stability.

[0038] In the cosmetic preparation process, xanthan gum forms hydrogen bonds with the ether groups of glycerol polyether-26, the low molecular weight component of sodium hyaluronate and the high molecular weight component are intertwined, and the hydroxyl groups of panthenol form hydrogen bonds with sodium hyaluronate and xanthan gum respectively, ultimately forming a three-dimensional interwoven prepolymer network. The self-assembled encapsulator forms hydrogen bonds with the carboxyl and hydroxyl groups of the base material prepolymer network through the hydroxyl groups of the outer HPMC layer, and is uniformly embedded in the base material network as a functional node, avoiding the problems of delamination and agglomeration.

[0039] The sources of raw materials used in the following specific cases include:

[0040] Cellulase: Solarbio, C8270;

[0041] Pectinase: Solarbio, P8181;

[0042] Hydroxypropyl methylcellulose: Maclean, H811092;

[0043] γ-Cyclodextrin: Maclean, C804509;

[0044] Hydrogenated soybean lecithin: Jixianmei Biotechnology, JXMSW-1031-1;

[0045] Phytosterol palmitate: Guangzhou Jiexin Biotechnology Co., Ltd., β-sitosterol palmitate, JYX-01039;

[0046] Dioleoylphosphatidylethanolamine: Solarbio, SO2-NDO-2K;

[0047] Sodium hyaluronate: low molecular weight component, Maclean, S742253; high molecular weight component, Maclean, 768689;

[0048] Panthenol: Solarb, IP1940;

[0049] Glyceryl polyether-26: Hubei Mingya New Material Technology Co., Ltd., MYEG-26;

[0050] Xanthan gum: Spico, CG-SFT.

[0051] Extraction Example 1

[0052] Take dried kava pepper roots and grind them to 60 mesh. Add an enzymatic hydrolysate (containing 1.3% cellulase, 0.6% pectinase, 0.1% Tween-80 phosphate buffer, pH 5.0) at a material-to-liquid ratio of 1:11. Enzymatically hydrolyze in a 43℃ water bath for 3.2 h. After enzymatic hydrolysis, heat to 82℃ to inactivate the enzyme for 10 min. Filter to remove coarse fiber residue to obtain an enzymatic hydrolysate containing free kava lactone. Simultaneously add 1.8% hydroxypropyl methylcellulose (HPMC) and 20% γ-cyclodextrin by weight of dried kava pepper root powder to the enzymatic hydrolysate. Incorporate for 2 h at 41℃ and 230 r / min to obtain a mixed solution.

[0053] Extraction Example 2

[0054] Dried kava root was pulverized to 70 mesh and added to an enzymatic hydrolysate (containing 1.5% cellulase, 0.7% pectinase, 0.1% Tween-80 phosphate buffer, pH 5.2) at a material-to-liquid ratio of 1:10. The mixture was enzymatically hydrolyzed in a 45℃ water bath for 3 hours, with 80W ultrasound-assisted extraction for 1 minute every 40 minutes during the process. After hydrolysis, the temperature was raised to 85℃ to inactivate the enzyme for 10 minutes. The mixture was then filtered to remove coarse fiber residue, yielding an enzymatic hydrolysate containing free kava lactone. 2.0% HPMC and 22% γ-cyclodextrin (based on the weight of the dried kava root powder) were added to the hydrolysate. The mixture was stirred at 42℃ and 250 r / min for 2 hours to obtain a final mixture.

[0055] Extraction Example 3

[0056] Take dried kava pepper roots and grind them to 60 mesh. Add an enzymatic hydrolysate (containing 1.2% cellulase, 0.5% pectinase, 0.1% Tween-80 phosphate buffer, pH 4.8) at a material-to-liquid ratio of 1:12. Enzymatically hydrolyze in a 42℃ water bath for 3.5 h. After enzymatic hydrolysis, heat to 80℃ for 10 min to inactivate the enzyme. Filter to remove coarse fiber residue to obtain an enzymatic hydrolysate containing free kava lactone. Add 0.6% HPMC and 18% γ-cyclodextrin by weight of dried kava pepper root powder to the enzymatic hydrolysate. Incorporate the mixture for 2 h at 40℃ and 200 r / min to obtain a mixed solution.

[0057] Extraction Example 4

[0058] Take dried kava root and grind it to 80 mesh. Add enzymatic hydrolysate (containing 1.4% cellulase, 0.6% pectinase, 0.1% Tween-80 phosphate buffer, pH 5.1) at a material-to-liquid ratio of 1:18. Enzymatically hydrolyze in a 44℃ water bath for 3.3 h. After enzymatic hydrolysis, heat to 83℃ for 10 min to inactivate the enzyme. Filter to remove coarse fiber residue to obtain enzymatic hydrolysate containing free kava lactone. Add 1.6% HPMC and 25% γ-cyclodextrin by weight of dried kava root powder to the enzymatic hydrolysate. Incorporate for 2 h at 41℃ and 240 r / min to obtain a mixed solution.

[0059] Extraction of Comparative Example 1

[0060] Take dried kava pepper roots and crush them to 60 mesh. Add them to the enzymatic hydrolysate (containing 1.3% cellulase, 0.6% pectinase, 0.1% Tween-80 phosphate buffer, pH 5.0) at a material-to-liquid ratio of 1:11. Enzymatically hydrolyze in a 43℃ water bath for 3.2 h. After enzymatic hydrolysis, heat to 82℃ to inactivate the enzyme for 10 min. Filter to remove coarse fiber residue to obtain an enzymatic hydrolysate containing free kava lactone. Add 1.8% HPMC to the enzymatic hydrolysate and react at 41℃ and 230 r / min for 2 h to obtain a mixed solution.

[0061] Kavalactone extraction rate test: High performance liquid chromatography (HPLC) was used with a C18 column (4.6 mm × 250 mm, 5 μm), a mobile phase of methanol-water (80:20, v / v), a flow rate of 1.0 mL / min, a detection wavelength of 246 nm, and a column temperature of 30 ℃. The ratio of the actual kavalactone content in the extract to the theoretical total kavalactone content in the raw material was calculated.

[0062] Stability test of the mixture: The extracted mixture was left to stand at room temperature for 48 hours, and the stratification was observed to evaluate the dispersion stability.

[0063] The experimental results of each extraction example and extraction comparison example are shown in Table 1.

[0064] Table 1

[0065] Extraction Example 1 88.5 92.3 No layering Extraction Example 2 91.2 94.1 No layering Extraction Example 3 76.3 85.6 Slight stratification Extraction Example 4 72.8 83.2 Clearly layered Extraction of Comparative Example 1 65.7 78.5 Severe stratification

[0066] Compared with Comparative Example 1, Extraction Example 1, due to the addition of γ-cyclodextrin, showed that the extraction rate of kavalactone in Extraction Example 1 was increased by 34.7%, the purity was increased by 17.6%, and the stability of the mixture was better. This proves that γ-cyclodextrin has a significant complexing and enrichment effect on kavalactone, which can improve extraction efficiency and product stability.

[0067] Compared with Example 1, Example 2 incorporated ultrasonic-assisted extraction and adjusted the pulverization mesh size and enzymatic hydrolysis parameters. The extraction rate increased by 3.0% and the purity increased by 2.0% compared with Example 1, indicating that ultrasonic assistance can promote the release of calvalactone, and optimized parameters can further improve the extraction effect.

[0068] Compared with Example 1, Example 3 showed that the amount of HPMC used was reduced to 0.6%, the extraction rate decreased by 13.6% and the purity decreased by 7.3% compared with Example 1, and slight stratification occurred. This confirmed that insufficient HPMC usage would affect the stability of the mixture and the dissolution and retention of kavalactone.

[0069] Compared with Example 1, Example 4 showed that the material-to-liquid ratio was changed to 1:18, resulting in a 17.6% decrease in extraction rate and a 10.9% decrease in purity. The material-to-liquid ratio was also significantly differentiating, indicating that an excessively high material-to-liquid ratio would dilute the concentration of the enzymatic hydrolysate, thereby reducing extraction efficiency and product stability.

[0070] Product Preparation Example 1

[0071] Weigh 14g of hydrogenated soybean lecithin, 4g of phytosterol palmitate, and 2g of dioleoylphosphatidylethanolamine according to a mass ratio of 7:2:1. Dissolve the three in anhydrous ethanol-propylene glycol mixture (volume ratio 3:1, organic solvent mass accounts for 85% of the membrane material solution mass). Stir in a 53℃ water bath until completely dissolved to obtain the membrane material solution. Add the mixture from Example 1 at a mass ratio of membrane material solution: mixture = 1:0.85 at 1.5 drops / second to the membrane material solution. Maintain stirring and emulsification at 53℃ and 420r / min for 30min. Remove the organic solvent by vacuum distillation at 53℃ (distillation rate 2mL / min). Continue high-pressure homogenization at 52℃ (pressure 95MPa, cycle 3 times). Microfilter through a 0.1μm polyethersulfone membrane to obtain the self-assembled encapsulated body.

[0072] Weigh the raw materials according to the following percentages by mass: 9% self-assembled encapsulant, 1.5% sodium hyaluronate (0.5g low molecular weight 1000kDa + 1g high molecular weight 1000kDa), 0.8% panthenol, 7% glycerol polyether-26, 0.12% xanthan gum, and deionized water to 100%. Add glycerol polyether-26 and xanthan gum to deionized water and stir at 68°C until completely dissolved. Cool to 52°C, add sodium hyaluronate and panthenol, and stir for 30 minutes to obtain the base solution. Cool the base solution to 32°C, and add the self-assembled encapsulant dropwise while stirring at 380 rpm. After the addition is complete, continue stirring for 25 minutes. Filter through a 0.22μm microfiltration membrane to obtain the essence water.

[0073] Product Preparation Example 2

[0074] Weigh 14g of hydrogenated soybean lecithin, 4g of phytosterol palmitate, and 2g of dioleoylphosphatidylethanolamine according to a mass ratio of 7:2:1. Dissolve the three in anhydrous ethanol-propylene glycol mixture (volume ratio 3:1, organic solvent mass accounts for 88% of the membrane material solution mass). Stir in a 55℃ water bath until completely dissolved to obtain the membrane material solution. Add the mixture from Example 2 at a mass ratio of membrane material solution: mixture = 1:0.9 at a rate of 2 drops / second to the membrane material solution. Maintain stirring and emulsification at 55℃ and a speed of 450r / min for 30min. Remove the organic solvent by vacuum distillation at 55℃ (distillation rate 2mL / min). Continue high-pressure homogenization at 55℃ (pressure 100MPa, 4 cycles). Microfilter through a 0.1μm polyethersulfone membrane to obtain the self-assembled encapsulated body.

[0075] Weigh the raw materials by mass percentage: 10% self-assembled encapsulant, 1.8% sodium hyaluronate (low molecular weight 1000kDa 0.6g + high molecular weight 1000kDa 1.2g), 1.0% panthenol, 8% glycerol polyether-26, 0.15% xanthan gum, and deionized water to 100%. Add glycerol polyether-26 and xanthan gum to deionized water and stir at 70℃ until completely dissolved. Cool to 55℃, add double molecular weight sodium hyaluronate and panthenol, and stir for 30 min to obtain the base solution. Cool the base solution to 35℃, and add the self-assembled encapsulant dropwise while stirring at 400 rpm. After the addition is complete, continue stirring for 25 min. Filter through a 0.22μm microfiltration membrane to obtain the essence water.

[0076] Product Preparation Example 3

[0077] Weigh 14g of hydrogenated soybean lecithin, 4g of phytosterol palmitate, and 2g of dioleoylphosphatidylethanolamine according to a mass ratio of 7:2:1. Dissolve the three in anhydrous ethanol-propylene glycol mixture (volume ratio 3:1, organic solvent mass accounts for 82% of the membrane material solution mass). Stir in a 52℃ water bath until completely dissolved to obtain the membrane material solution. Add the mixture from Example 3 at a mass ratio of 1:0.8 (membrane material solution: mixture) dropwise to the membrane material solution at 1 drop / second. Maintain stirring and emulsification at 52℃ and 400r / min for 30min. Remove the organic solvent by vacuum distillation at 52℃ (distillation rate 2mL / min). Continue high-pressure homogenization at 50℃ (pressure 90MPa, cycle 3 times). Microfilter through a 0.1μm polyethersulfone membrane to obtain the self-assembled encapsulated body.

[0078] Weigh the raw materials according to the following percentages by mass: 8% self-assembled encapsulant, 1.2% sodium hyaluronate (0.4g low molecular weight 1000kDa + 0.8g high molecular weight 1000kDa), 0.7% panthenol, 6% glycerol polyether-26, 0.1% xanthan gum, and deionized water to 100%. Add glycerol polyether-26 and xanthan gum to deionized water and stir at 65°C until completely dissolved. Cool to 50°C, add sodium hyaluronate and panthenol (dual molecular weight), and stir for 30 minutes to obtain the base solution. Cool the base solution to 30°C, and add the self-assembled encapsulant dropwise while stirring at 350 rpm. Continue stirring for 25 minutes after the addition is complete. Filter through a 0.22μm microfiltration membrane to obtain the essence water.

[0079] Product Preparation Example 4

[0080] Weigh 14g of hydrogenated soybean lecithin, 4g of phytosterol palmitate, and 2g of dioleoylphosphatidylethanolamine according to a mass ratio of 7:2:1. Dissolve the three in anhydrous ethanol-propylene glycol mixture (volume ratio 3:1, organic solvent mass accounts for 86% of the membrane material solution mass). Stir in a 54℃ water bath until completely dissolved to obtain the membrane material solution. Add the mixture from Example 4 at a mass ratio of membrane material solution: mixture = 1:0.88 at a rate of 1.8 drops / second to the membrane material solution. Maintain stirring and emulsification at 54℃ and 430 r / min for 30 min. Remove the organic solvent by vacuum distillation at 54℃ (distillation rate 2 mL / min). Continue high-pressure homogenization at 53℃ (pressure 98 MPa, 4 cycles). Microfilter through a 0.1 μm polyethersulfone membrane to obtain the self-assembled encapsulated body.

[0081] Weigh the raw materials by mass percentage: 11% self-assembled encapsulant, 1.6% sodium hyaluronate (0.5g low molecular weight 1000kDa + 1g high molecular weight 1000kDa), 0.9% panthenol, 9% glycerol polyether-26, 0.13% xanthan gum, and deionized water to 100%. Add glycerol polyether-26 and xanthan gum to deionized water and stir at 69°C until completely dissolved. Cool to 53°C, add sodium hyaluronate and panthenol, and stir for 30 minutes to obtain the base solution. Cool the base solution to 33°C, and add the self-assembled encapsulant dropwise while stirring at 370 rpm. After the addition is complete, continue stirring for 25 minutes. Filter through a 0.22μm microfiltration membrane to obtain the essence water.

[0082] Product Preparation Example 5

[0083] Weigh 14g of hydrogenated soybean lecithin, 4g of phytosterol palmitate, and 2g of dioleoylphosphatidylethanolamine according to a mass ratio of 7:2:1. Dissolve the three in anhydrous ethanol-propylene glycol mixture (volume ratio 3:1, organic solvent mass accounts for 87% of the membrane material solution mass). Stir in a 53℃ water bath until completely dissolved to obtain the membrane material solution. Add the mixture from Example 1 at a mass ratio of membrane material solution: mixture = 1:1.3 at a rate of 1.6 drops / second to the membrane material solution. Maintain stirring and emulsification at 53℃ and 440 r / min for 30 min. Remove the organic solvent by vacuum distillation at 53℃ (distillation rate 2 mL / min). Continue high-pressure homogenization at 52℃ (pressure 96 MPa, 3 cycles). Microfilter through a 0.1 μm polyethersulfone membrane to obtain the self-assembled encapsulated body.

[0084] Weigh the raw materials by mass percentage: 9.5% self-assembled encapsulant, 1.7% sodium hyaluronate (0.5g low molecular weight 1000kDa + 1g high molecular weight 1000kDa), 0.85% panthenol, 7.5% glyceryl polyether-26, 0.14% xanthan gum, and deionized water to 100%. Add glyceryl polyether-26 and xanthan gum to deionized water and stir at 67°C until completely dissolved. Cool to 51°C, add sodium hyaluronate and panthenol (dual molecular weight), and stir for 30 min to obtain the base solution. Cool the base solution to 31°C, and add the self-assembled encapsulant dropwise while stirring at 360 rpm. Continue stirring for 25 min after the addition is complete. Filter through a 0.22μm microfiltration membrane to obtain the essence water.

[0085] Product Preparation Example 6

[0086] Weigh 14g of hydrogenated soybean lecithin, 4g of phytosterol palmitate, and 2g of dioleoylphosphatidylethanolamine according to a mass ratio of 7:2:1. Dissolve the three in anhydrous ethanol-propylene glycol mixture (volume ratio 3:1, organic solvent mass accounts for 84% of the membrane material solution mass). Stir in a 53℃ water bath until completely dissolved to obtain the membrane material solution. Add the mixture from Example 1 at a mass ratio of membrane material solution: mixture = 1:0.86 at 1.4 drops / second to the membrane material solution. Maintain stirring and emulsification at 53℃ and 410 r / min for 30 min. Remove the organic solvent by vacuum distillation at 53℃ (distillation rate 2 mL / min). Continue high-pressure homogenization at 52℃ (pressure 94 MPa, cycle 3 times). Microfilter through a 0.1 μm polyethersulfone membrane to obtain the self-assembled encapsulated body.

[0087] Weigh the raw materials according to the following percentages by mass: 8.5% self-assembled encapsulator, 1.5% sodium hyaluronate (1000 Da molecular weight), 0.8% panthenol, 7% glycerol polyether-26, 0.12% xanthan gum, and deionized water to 100%. Add glycerol polyether-26 and xanthan gum to deionized water and stir at 66°C until completely dissolved. Cool to 52°C, add sodium hyaluronate and panthenol, and stir for 30 minutes to obtain the base solution. Cool the base solution to 32°C, and add the self-assembled encapsulator dropwise while stirring at 380 rpm. After the addition is complete, continue stirring for 25 minutes. Filter through a 0.22 μm microfiltration membrane to obtain the essence water.

[0088] Product Preparation Example 7

[0089] Weigh 14g of hydrogenated soybean lecithin, 4g of phytosterol palmitate, and 2g of dioleoylphosphatidylethanolamine according to a mass ratio of 7:2:1. Dissolve the three in anhydrous ethanol-propylene glycol mixture (volume ratio 3:1, organic solvent mass accounts for 89% of the membrane material solution mass). Stir in a 53℃ water bath until completely dissolved to obtain the membrane material solution. Mix the mixture from Example 1 with 0.05% (mixture mass) of hexanediol. Add the mixture dropwise to the membrane material solution at a mass ratio of 1:0.87 (membrane material solution:mixture solution = 1.7 drops / second. Maintain stirring and emulsification at 53℃ and 420r / min for 30min. Remove the organic solvent by vacuum distillation at 53℃ (distillation rate 2mL / min). Continue high-pressure homogenization at 52℃ (pressure 97MPa, cycle 3 times). Microfilter through a 0.1μm polyethersulfone membrane to obtain the self-assembled encapsulated body.

[0090] Weigh the raw materials by mass percentage: 9.2% self-assembled encapsulant, 1.5% sodium hyaluronate (0.5g low molecular weight 1000kDa + 1g high molecular weight 1000kDa), 0.8% panthenol, 7% glycerol polyether-26, 0.12% xanthan gum, and deionized water to 100%. Add glycerol polyether-26 and xanthan gum to deionized water and stir at 68℃ until completely dissolved. Cool to 52℃, add sodium hyaluronate and panthenol, and stir for 30 min to obtain the base solution. Cool the base solution to 32℃, and add the self-assembled encapsulant dropwise while stirring at 380 rpm. After the addition is complete, continue stirring for 25 min. Filter through a 0.22μm microfiltration membrane to obtain the essence water.

[0091] Product Comparison Example 1

[0092] Weigh the raw materials according to the following percentages by mass: 0.8% pure kavalactone, 1.5% sodium hyaluronate (0.5g low molecular weight 1000kDa + 1g high molecular weight 1000kDa), 0.8% panthenol, 7% glyceryl polyether-26, 0.12% xanthan gum, and deionized water to bring the total to 100%. Mix all raw materials directly, stir at 68℃ and 380r / min for 30min, cool to 32℃, and filter through a 0.22μm microfiltration membrane to obtain the essence water.

[0093] Product Comparison Example 2

[0094] Weigh 14g of hydrogenated soybean lecithin and 4g of phytosterol palmitate at a mass ratio of 7:2. Dissolve them in anhydrous ethanol-propylene glycol mixture (volume ratio 3:1, organic solvent mass accounts for 85% of the membrane material solution mass). Stir in a 53℃ water bath until completely dissolved to obtain the membrane material solution. Add the mixture from Example 1 at a mass ratio of membrane material solution: mixture = 1:0.85 at 1.5 drops / second to the membrane material solution. Maintain stirring and emulsification at 53℃ and 420r / min for 30min. Remove the organic solvent by vacuum distillation at 53℃ (distillation rate 2mL / min). Continue high-pressure homogenization at 52℃ (pressure 95MPa, cycle 3 times). Microfilter through a 0.1μm polyethersulfone membrane to obtain the self-assembled encapsulated body.

[0095] Weigh the raw materials by mass percentage: 9% self-assembled encapsulator, 1.5% sodium hyaluronate (0.5g low molecular weight 1000kDa + 1g high molecular weight 1000kDa), 0.8% panthenol, 7% glyceryl polyether-26, 0.12% xanthan gum, and deionized water to 100%. Subsequent steps are the same as in Product Preparation Example 1 to obtain the essence water.

[0096] Encapsulation efficiency test: The free calvalactone and the encapsulated calvalactone were separated by dialysis combined with HPLC, and the proportion of encapsulated calvalactone to total calvalactone was calculated.

[0097] Transdermal efficiency test: A Franz diffusion cell was used with pigskin as the transdermal barrier and pH 7.4 phosphate buffer as the receiving solution. The mixture was stirred at 37℃ and 500 r / min for 24 h. The calolactone content in the receiving solution was measured, and the transdermal efficiency was calculated (the ratio of calolactone content in the receiving solution to the total calolactone content added is the transdermal efficiency).

[0098] Skin irritation test: In accordance with the "Cosmetic Safety Technical Specifications" (2015 edition), 30 subjects were continuously treated with patches for 24 hours, and their skin reactions were observed.

[0099] The experimental results of each product preparation example and product comparison example are shown in Table 2.

[0100] Table 2

[0101] Product Preparation Example 1 95.2 92.1 42.3 0 Product Preparation Example 2 96.5 93.8 45.6 0 Product Preparation Example 3 82.7 76.5 35.8 0 Product Preparation Example 4 79.3 73.1 33.2 0 Product Preparation Example 5 88.6 83.2 38.5 0 Product Preparation Example 6 92.1 88.4 39.7 0 Product Preparation Example 7 97.3 94.5 46.8 0 Product Comparison Example 1 - - 18.5 2 Product Comparison Example 2 87.5 78.3 37.2 0

[0102] Compared with Comparative Example 1, Product Preparation Example 1, due to its layered coating structure, showed a 128.6% increase in transdermal efficiency and no irritation, demonstrating that the layered coating structure can improve the transdermal effect of calvalactone while reducing irritation.

[0103] Compared with Comparative Example 2, Product Preparation Example 1, containing dioleoylphosphatidylethanolamine, showed an 8.8% increase in encapsulation efficiency compared to Comparative Example 2. After 6 months of storage at room temperature, the encapsulation efficiency increased by 17.6%, demonstrating superior transdermal efficiency. This proves that dioleoylphosphatidylethanolamine can strengthen the phospholipid bilayer structure and improve encapsulation efficiency and stability.

[0104] Compared with Example 1, the encapsulation rate of Example 5 decreased by 6.9% and the transdermal efficiency decreased by 13.7%, confirming that an excessively high proportion of the mixture during encapsulation will affect the encapsulation effect.

[0105] Compared with Example 1, Example 6, which uses single-molecular-weight sodium hyaluronate, showed a 6.1% decrease in transdermal efficiency compared to Example 1, demonstrating that double-molecular-weight sodium hyaluronate is more conducive to synergistic effects of liposomes.

[0106] Compared with Example 1, Example 7 of product preparation added hexanediol pretreatment mixture, and the encapsulation rate was increased by 2.2% and the transdermal efficiency was increased by 10.6% compared with Example 1. This shows that hexanediol can further optimize the compatibility between the mixture and the membrane material and improve product performance.

[0107] In the description of this specification, the references to terms such as "one embodiment," "some embodiments," "illustrative embodiment," "example," "specific example," or "some examples," etc., indicate that a specific feature, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples.

[0108] The above description represents the preferred embodiments of the present invention. It should be noted that those skilled in the art can make various improvements and modifications without departing from the principles of the present invention, and these improvements and modifications are also considered to be within the scope of protection of the present invention.

Claims

1. A method for extracting kava liposomes, characterized in that the steps include... include: The dried kava root was crushed, added to the cell wall breaking liquid for enzymatic hydrolysis, then the enzyme was inactivated, and the fiber residue was filtered off to obtain a composite liquid. γ-cyclodextrin and hydroxypropyl methylcellulose were added to the composite liquid, and after stirring, a mixture containing kava liposomes was obtained. The cell wall disruption liquid contains cellulase and pectinase; The mass of the γ-cyclodextrin added is 18% to 25% of the mass of the dried pepper root.

2. The method for extracting liposomes according to claim 1, characterized in that, The hydroxypropyl methylcellulose has a mass concentration of 1.5% to 2.0% in the mixture.

3. The method for extracting liposomes according to claim 1, characterized in that, The mass ratio of the dried kava pepper root to the cell wall breaking liquid is 1:10~12, the mass concentration of the cellulase in the cell wall breaking liquid is 1.2%~1.5%, and the mass concentration of the pectinase in the cell wall breaking liquid is 0.5%~0.7%.

4. A cosmetic containing kava liposomes, characterized in that, Contains the mixture according to any one of claims 1 to 3.

5. The cosmetic containing kava liposomes according to claim 4, characterized in that, The preparation steps include: Hydrogenated soybean lecithin, phytosterol palmitate and dioleoylphosphatidylethanolamine are dissolved in an organic solvent to obtain a membrane material solution. Under stirring, the mixture according to any one of claims 1 to 3 is added dropwise to the membrane material solution. The organic solvent is removed by vacuum distillation, and after homogenization, a self-assembled encapsulated body is obtained. The self-assembled encapsulator, sodium hyaluronate, panthenol, glyceryl polyether-26, and xanthan gum were mixed in water to obtain the cosmetic containing kava liposomes.

6. The cosmetic containing kava liposomes according to claim 5, characterized in that, The organic solvent accounts for 80% to 90% of the mass of the membrane material solution. In the membrane material solution, the mass ratio of hydrogenated soybean lecithin, phytosterol palmitate, and dioleoylphosphatidylethanolamine is 7:2:

1.

7. The cosmetic containing kava liposomes according to claim 6, characterized in that, The mass ratio of the membrane material liquid to the mixture is 1:0.8~0.

9.

8. The cosmetic containing kava liposomes according to claim 5, characterized in that, By weight, it comprises 8% to 11% of the self-assembled encapsulator, 1.2% to 1.8% of the sodium hyaluronate, 0.7% to 1% of the panthenol, 6% to 9% of the glycerol polyether-26, 0.1% to 0.15% of the xanthan gum, and the balance being water.

9. The cosmetic containing kava liposomes according to claim 5, characterized in that, The sodium hyaluronate comprises a low molecular weight component with a molecular weight of less than 1000 Da and a high molecular weight component with a molecular weight of more than 1000 kDa, wherein the mass ratio of the low molecular weight component to the high molecular weight component is 1:

2.

10. The cosmetic containing kava liposomes according to claim 5, characterized in that, Before being added to the membrane material solution, the mixture is first mixed with hexanediol, and the amount of hexanediol used is 0.05% to 0.1% of the mass of the mixture.