An anti-aging skin care product composition containing a fermented extract of polygonatum

Abstract

The application relates to the cosmetic technical field and particularly relates to an anti-aging skin care product composition containing a fermented extract of rhizoma polygonati, which comprises the following components in percentage by mass: 2-5% of selenium-phosphorylated composite modified rhizoma polygonati polysaccharide, 1-2% of ferulic acid-alpha-tocopherol-1,3-diglyceride, 1-3% of carboxymethylized pachyman-nervonyl ceramide 3 compound, 5-20% of a moisturizing agent, 0.1-0.5% of a thickening agent, 0.2-1.0% of a preservative, a proper amount of a pH regulator, and the rest is deionized water, wherein the selenium-phosphorylated composite modified rhizoma polygonati polysaccharide is prepared by taking nine times of steaming and nine times of drying rhizoma polygonati as raw material, extracting rhizoma polygonati fermented crude polysaccharide through fermentation of lactobacillus plantarum, and then sequentially performing phosphorylation modification and selenium modification, the composition has multiple anti-aging effects such as antioxidation, promotion of collagen synthesis and repair of skin barrier, and has high transdermal absorption rate, good stability and high safety.

Description

Technical Field

[0001] This invention relates to the field of cosmetic technology, specifically to an anti-aging skincare composition containing Polygonatum odoratum fermentation extract. Background Technology

[0002] Skin aging is a complex biological process, mainly manifested as dry and loose skin, wrinkle formation, pigmentation, and decreased barrier function. Oxidative stress, collagen loss, inflammatory responses, and skin barrier damage are the main mechanisms leading to skin aging. Currently, most anti-aging skincare products on the market rely on single active ingredients, which suffer from low transdermal absorption rates, poor stability, and limited efficacy, making it difficult to achieve comprehensive and effective anti-aging results.

[0003] Polygonatum rhizome, the dried rhizome of a plant in the genus Polygonatum of the Liliaceae family, possesses the effects of tonifying qi and nourishing yin, strengthening the spleen and moistening the lungs. Modern research shows that Polygonatum polysaccharides have strong antioxidant activity, but the large molecular weight and low transdermal absorption rate of natural Polygonatum polysaccharides limit their application in skincare products. Furthermore, raw Polygonatum has a certain degree of irritation and must be processed before use. Therefore, modifying the active ingredients of Polygonatum to improve its transdermal absorption rate and efficacy stability, and synergistically combining it with other active ingredients, is key to developing highly effective anti-aging skincare products. Summary of the Invention

[0004] To address the existing problems, this invention provides an anti-aging skincare composition containing Polygonatum odoratum fermentation extract. This composition has multiple anti-aging effects, including anti-oxidation, promoting collagen synthesis, and repairing the skin barrier. It also has high transdermal absorption rate, good stability, and high safety.

[0005] In a first aspect, the present invention provides an anti-aging skin care product composition containing Polygonatum odoratum fermentation extract, comprising the following components in the indicated weight percentages: 2%-5% selenized-phosphorylated modified Polygonatum odoratum polysaccharide, 1%-2% ferulic acid-α-tocopherol-1,3-diglyceride, 1%-3% carboxymethylated Poria cocos polysaccharide-ceramide 3 complex, 5%-20% moisturizer, 0.1%-0.5% thickener, 0.2%-1.0% preservative, appropriate amount of pH adjuster, and the balance being deionized water.

[0006] The selenized-phosphorylated composite modified Polygonatum polysaccharide is prepared by using Polygonatum that has been processed through nine steaming and nine sun-drying as raw material, extracting crude polysaccharide from Polygonatum through fermentation with Lactobacillus plantarum, and then successively modifying it through phosphorylation and selenization.

[0007] This invention reduces the irritation of Polygonatum sibiricum and enhances its antioxidant activity through a nine-steaming and nine-drying process. It moderately degrades the macromolecular polysaccharides through fermentation with Lactobacillus plantarum, and further improves transdermal absorption through phosphorylation modification and imparts additional antioxidant activity through selenization modification, achieving multi-level modification of Polygonatum sibiricum polysaccharides. Simultaneously, the composite modified Polygonatum sibiricum polysaccharides are combined with ferulic acid-α-tocopherol-1,3-diglyceride and carboxymethylated Poria cocos polysaccharide-ceramide 3 complex. These three components, in a specific ratio, self-assemble to form a stable nanocomplex, achieving a multi-target synergistic anti-aging effect including antioxidant, anti-inflammatory, collagen synthesis promotion, skin barrier repair, and mitochondrial function enhancement.

[0008] Preferably, the phosphorylated Polygonatum polysaccharide has a degree of phosphorylation substitution of 0.12-0.15, within which its antioxidant activity and transdermal absorption rate are optimal. The selenized-phosphorylated composite modified Polygonatum polysaccharide contains 120-150 μg / g of selenium, which is entirely in the form of organic selenium and is safe and non-cytotoxic.

[0009] The ferulic acid-α-tocopherol-1,3-diglyceride is prepared by esterification of ferulic acid, glycerol and α-tocopherol. It combines the antioxidant and anti-inflammatory activities of ferulic acid with the lipid-soluble antioxidant and moisturizing properties of α-tocopherol, and has good water solubility.

[0010] The grafting rate of ceramide 3 in the carboxymethylated Poria cocos polysaccharide-ceramide 3 complex is 15%-20%, and within this range, the complex exhibits the best water solubility and skin barrier repair effect.

[0011] Preferably, the humectant is selected from at least one of glycerin, propylene glycol, and sodium hyaluronate; the thickener is selected from carbomer and / or xanthan gum; the preservative is a compound of phenoxyethanol and ethylhexylglycerin; and the pH adjuster is triethanolamine.

[0012] The components in the composition self-assemble to form a nanocomposite with an average particle size of 60-70 nm and a zeta potential of -23 to -26 mV, which significantly improves the transdermal absorption rate and storage stability of the active ingredients.

[0013] Secondly, the present invention provides a method for preparing the above-mentioned composition, comprising the following steps: S1. Disperse the thickener in deionized water and allow it to swell to obtain an aqueous phase; S2. Add the humectant to the aqueous phase and stir to dissolve; S3. Add the three active ingredients in sequence and stir at 30-50℃ for 1-3 hours to form a nanocomposite. S4. Add preservative and stir well; S5. Adjust the pH to 5.5-6.5 using a pH adjuster.

[0014] Preferably, the stirring temperature in step S3 is 40°C and the stirring time is 2 hours.

[0015] Thirdly, the present invention provides the application of the above composition in the preparation of skin care products with antioxidant, collagen synthesis promoting, and skin barrier repair effects.

[0016] In summary, this application has the following beneficial effects: 1. The composition of the present invention simultaneously covers five core aging targets: anti-oxidation, anti-inflammation, promoting collagen synthesis, repairing the skin barrier, and enhancing mitochondrial function, thereby achieving multi-dimensional anti-aging.

[0017] 2. The antioxidant and collagen synthesis capabilities of selenized-phosphorylated polysaccharides are significantly higher than those of simple superposition of single modifications, achieving a synergistic effect of "1+1>2"; the three active ingredients form a nanocomposite through self-assembly, further improving the transdermal absorption rate and stability, achieving an overall synergistic effect of "1+1+1>3".

[0018] 3. The nine-steaming and nine-drying process effectively eliminates the irritation of raw Polygonatum sibiricum; the selenium in the compound modified Polygonatum sibiricum polysaccharide exists entirely in the form of organic selenium, and the total selenium content of the final product is far below the safety limit; cytotoxicity and skin irritation tests prove that the composition is safe and non-irritating.

[0019] 4. The preparation process uses conventional equipment in the cosmetics industry, the conditions are mild, it is easy to scale up production, and it has good industrial applicability. Detailed Implementation

[0020] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail below with reference to specific embodiments, comparative examples, and test data. The specific embodiments described herein are only used to explain the invention and are not intended to limit the invention.

[0021] Unless otherwise specified, all raw materials and components used in this application are commercially available. All raw materials comply with the requirements of the "Cosmetic Safety Technical Specifications," the "Chinese Pharmacopoeia," and relevant industry standards, and contain no highly allergenic or strongly irritating ingredients. All chemically modified products have undergone rigorous purification processes, and the residual amount of unreacted raw materials in the final product is below the detection limit, meeting cosmetic safety requirements.

[0022] raw material 1. Polygonatum sibiricum medicinal material (purchased from Bozhou Boyuantong Traditional Chinese Medicine Planting Co., Ltd.) 2. Lactobacillus plantarum (purchased from Zhengzhou Yukong Biotechnology Co., Ltd.) 3. Chemical reagents (all analytical grade, purchased from Sinopharm Chemical Reagent Co., Ltd., including: sodium tripolyphosphate, sodium hydroxide, triethanolamine, toluene, p-toluenesulfonic acid, sodium trimetaphosphate, sodium selenite, glacial acetic acid, chloroacetic acid, EDC, NHS, glycerol, propylene glycol) 4. Poria cocos crude polysaccharide (polysaccharide content ≥80%, purchased from Xi'an Yunuo Bioengineering Co., Ltd.) 5. Ceramide 3 (purity ≥98%, purchased from Xi'an Jincuifang Plant Technology Development Co., Ltd.) 6. Ferulic acid (analytical grade, purchased from Shanghai Yuanye Biotechnology Co., Ltd.) 7. α-Tocopherol (analytical grade, purchased from Wuhan Fengtai Weiyuan Technology Co., Ltd.) 8. Sodium hyaluronate (cosmetic grade, mixed molecular weight, purchased from Shanghai Oule Chemical Co., Ltd.) 9. Carbomer (cosmetic grade, purchased from Qingdao Yufengda Fine Chemical Co., Ltd.) 10. Compound preservative (cosmetic grade, a compound of phenoxyethanol and ethylhexylglycerin in a mass ratio of 9:1, purchased from Shanghai Shifeng Biotechnology Co., Ltd.) 11. Deionized water (purchased from Guangdong Shengke Biochemical Technology Co., Ltd.)

[0023] Unless otherwise specified, all raw materials used in the examples and comparative examples are conventional products that can be purchased from the market.

[0024] I. Preparation Example Preparation Example 1: Preparation of Phosphorylated Polysaccharide from Polygonatum odoratum Terminology Explanation: The "nine-steaming and nine-drying" process described in this invention refers to placing the Polygonatum rhizome in a steaming container and steaming it at normal pressure for 2-3 hours until it is thoroughly steamed (easily pierced with a bamboo skewer without any white core). After removal, it is spread out in a well-ventilated and sunny place to dry until the moisture content reaches 10%-15% (measured using the drying method; calculation formula: moisture content = (mass before drying - mass after drying) / mass before drying × 100%). This steaming and drying process is repeated a total of 9 times, ultimately yielding a processed Polygonatum rhizome that is black and oily inside and out, soft in texture, and has a sweet and slightly bitter taste. This process is a traditional processing method for Polygonatum rhizome included in Part I of the 2025 edition of the Chinese Pharmacopoeia. It can convert bound polyphenols in Polygonatum rhizome into free polyphenols, partially hydrolyze polysaccharides into oligosaccharides and monosaccharides, maintain a relatively stable total saponin content, and increase the overall antioxidant activity by more than 25%, while eliminating the numbing sensation and irritation of raw Polygonatum rhizome.

[0025] 1. Formula: 100g of nine-steamed and nine-dried Polygonatum sibiricum, 10mL of Lactobacillus plantarum seed liquid, 1000mL of deionized water, and chemical reagents (15g of sodium tripolyphosphate and 5g of sodium tripolyphosphate).

[0026] 2. Preparation steps: s1. The nine-steamed and nine-dried Polygonatum sibiricum was pulverized to 80 mesh, deionized water was added, and it was extracted at 90℃ for 2 hours. After filtration, the filtrate was concentrated to a relative density of 1.10 (25℃) to obtain the water extract of Polygonatum sibiricum. s2. Inoculate the aqueous extract of Polygonatum odoratum with Lactobacillus plantarum seed liquid and ferment at 37℃ and 150 rpm for 72 h. After fermentation, sterilize at 100℃ for 10 min, centrifuge and collect the supernatant, add 3 times the volume of anhydrous ethanol, let stand at 4℃ for 12 h, centrifuge to collect the precipitate, freeze dry to obtain crude polysaccharide of Polygonatum odoratum fermentation (molecular weight 2-100 kDa, polysaccharide content ≥65%). s3. Take 10g of the above-mentioned crude polysaccharide from fermented Polygonatum odoratum, dissolve it in 200mL of deionized water, adjust the pH to 8.0 with 20% sodium hydroxide solution, add a mixture of sodium tripolyphosphate and sodium trimetaphosphate, and react at 60℃ and 200rpm for 3h. s4. After the reaction was completed, the pH was adjusted to 7.0 with glacial acetic acid, and the solution was placed in a dialysis bag (molecular weight cutoff 3500 Da) and dialyzed for 48 hours. The deionized water was replaced every 6 hours. The dialysate was freeze-dried to obtain phosphorylated Polygonatum polysaccharide.

[0027] Explanation of key parameters: Determination of degree of phosphorylation substitution (DS): The molybdenum blue colorimetric method was used. The calculation formula was: DS = (162 × P) / (31 - 102 × P), where P is the mass fraction of phosphorus in the sample (%), 162 is the molar mass of glucose unit, 31 is the molar mass of phosphorus, and 102 is the increase in molar mass after a hydroxyl group is substituted by a phosphate group.

[0028] Optimal Range Verification: This invention prepared phosphorylated Polygonatum polysaccharides with substitution degrees of 0.05, 0.10, 0.12, 0.15, and 0.20, respectively. Their DPPH radical scavenging rate and transdermal absorption rate were tested. The results showed that both indicators reached their peak values ​​when the substitution degree was between 0.12 and 0.15. Too low a substitution degree resulted in insufficient activity, while too high a degree led to increased molecular steric hindrance and hindered transdermal absorption. The phosphorylated Polygonatum polysaccharide obtained in this preparation example had a substitution degree of 0.13.

[0029] Preparation Example 2: Preparation of Selenized-Phosphorylated Composite Modified Polygonatum Polysaccharide 1. Formula: 10g of phosphorylated Polygonatum polysaccharide obtained in Example 1, chemical reagents (8g sodium selenite, 50mL glacial acetic acid), and 150mL deionized water.

[0030] 2. Preparation steps: s1. Dissolve phosphorylated Polygonatum polysaccharide in deionized water, add glacial acetic acid, stir well to obtain a reaction solution; s2. Slowly add sodium selenite solution (8g sodium selenite dissolved in 50mL deionized water) to the reaction solution and react for 6h at 40℃ and 150rpm. s3. After the reaction was completed, the pH was adjusted to 7.0 with the chemical reagent triethanolamine, and the solution was placed in a dialysis bag (molecular weight cutoff 3500 Da) for dialysis for 72 hours. The deionized water was changed every 6 hours until the inorganic selenium content in the effluent was less than 0.01 μg / mL (detected by atomic fluorescence spectrometry). s4. The dialysate was freeze-dried to obtain selenized-phosphorylated composite modified Polygonatum polysaccharide.

[0031] Explanation of key parameters: Selenium content determination: Atomic fluorescence spectrometry was used. The selenium content of the product obtained in this preparation example was 132 μg / g, and it existed entirely in the form of organic selenium (selenium polysaccharide), with no free inorganic selenium residue.

[0032] Safety Statement: According to the "Cosmetic Safety Technical Specifications (2022 Edition)," the total selenium content in cosmetics must not exceed 0.5 μg / g. The maximum addition amount of the compound modified Polygonatum polysaccharide in the final product of this invention is 5%, therefore the total selenium content in the final product is approximately 0.0066 μg / g, which is far below the safety limit.

[0033] Preparation Example 3: Preparation of Carboxymethylated Poria cocos Polysaccharide-Ceramide 3 Complex 1. Formula: 10g of crude polysaccharide from Poria cocos, chemical reagents (12g of chloroacetic acid, 1.5g of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride, 0.8g of N-hydroxysuccinimide), 32g of ceramide, and 200mL of deionized water.

[0034] 2. Preparation steps: s1. Dissolve the crude polysaccharide of Poria cocos in 200 mL of 20% sodium hydroxide solution, alkalize at 30 °C for 1 h, add chloroacetic acid, and react at 60 °C for 3 h to obtain the crude carboxymethylated Poria cocos polysaccharide; s2. The pH was adjusted to 7.0 with glacial acetic acid, followed by dialysis and freeze-drying to obtain carboxymethylated Poria cocos polysaccharide; s3. Take 8g of carboxymethylated Poria cocos polysaccharide, dissolve it in 150mL of deionized water, add 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride and N-hydroxysuccinimide, and activate at room temperature for 30min. s4. Add anhydrous ethanol solution of ceramide 3 (2g ceramide 3 dissolved in 20mL anhydrous ethanol), react at 30℃ and 200rpm for 24h, dialyze, freeze dry to obtain carboxymethylated Poria cocos polysaccharide-ceramide 3 complex.

[0035] Explanation of key parameters: Determination of carboxymethylation degree: The acid-base titration method was used, and the calculation formula was: DS=(0.162×A) / (1-0.058×A), where A is the amount of glacial acetic acid consumed to neutralize 1g of sample (mmol).

[0036] Ceramide 3 grafting rate determination: High performance liquid chromatography was used. The calculation formula is: grafting rate = (mass of ceramide 3 in the complex / total mass of the complex) × 100%.

[0037] Optimal Range Verification: This invention prepared complexes with grafting rates of 5%, 10%, 15%, 20%, and 25%, and tested their water solubility and skin barrier repair capabilities. The results showed that when the grafting rate was 15%-20%, the water solubility was good and the repair effect was optimal. Excessively high grafting rates resulted in overly strong hydrophobicity of the complex, making it difficult to disperse in the aqueous phase. The grafting rate of the product obtained in this preparation example was 18%.

[0038] Preparation Example 4: Preparation of ferulic acid-α-tocopherol-1,3-diglyceride 1. Formula: 10g ferulic acid, 15g α-tocopherol, chemical reagents (5g glycerol, 0.5g p-toluenesulfonic acid, 100mL toluene).

[0039] 2. Preparation steps: s1. Ferulic acid, glycerol and p-toluenesulfonic acid were added to toluene and refluxed at 110°C for 4 hours. The water produced in the reaction was separated by a water separator to obtain ferulic acid monoglyceride. s2. Add α-tocopherol and continue reflux for 6 hours. After the reaction is complete, remove toluene by vacuum distillation. s3. The residue was separated by silica gel column chromatography (eluent: petroleum ether / ethyl acetate = 5:1) to give ferulic acid-α-tocopherol-1,3-diglyceride. Example

[0040] Example 1: Anti-aging essence of compound modified Polygonatum odoratum fermented extract 1. Raw material formula (percentage by mass): Selenized-phosphorylated modified Polygonatum polysaccharide 5%, ferulic acid-α-tocopherol-1,3-diglyceride 2%, carboxymethylated Poria cocos polysaccharide-ceramide 3 complex 3%, glycerol 8%, propylene glycol 5%, sodium hyaluronate 0.2%, carbomer 0.2%, compound preservative 0.6%, triethanolamine appropriate amount (to adjust pH to 5.5-6.5), and deionized water added to 100%.

[0041] 2. Preparation steps: s1. Carbomer is uniformly dispersed in deionized water and allowed to swell for 24 hours to obtain the aqueous phase; s2. Add glycerol, propylene glycol, and sodium hyaluronate to the aqueous phase and stir until completely dissolved; s3. Selenized-phosphorylated composite modified Polygonatum polysaccharide, ferulic acid-α-tocopherol-1,3-diglyceride, and carboxymethylated Poria cocos polysaccharide-ceramide 3 complex were added sequentially and stirred at 40℃ and 300rpm for 2h. Stable nanocomposites were formed through intermolecular hydrogen bonding and hydrophobic interactions. s4. Add the compound preservative and stir well; s5. Adjust the pH to 5.5-6.5 with triethanolamine, stir well, and you will get the anti-aging essence.

[0042] Example 2: Concentration-modified Polygonatum odoratum fermentation extract anti-aging essence 1. Raw material formula (percentage by mass): Selenized-phosphorylated modified Polygonatum polysaccharide 3%, ferulic acid-α-tocopherol-1,3-diglyceride 1.5%, carboxymethylated Poria cocos polysaccharide-ceramide 3 complex 2%, glycerol 8%, propylene glycol 5%, sodium hyaluronate 0.2%, carbomer 0.2%, compound preservative 0.6%, triethanolamine appropriate amount (to adjust pH to 5.5-6.5), deionized water added to 100%.

[0043] 2. Preparation steps: Same as in Example 1 Example 3: Low-concentration compound modified Polygonatum odoratum fermented extract anti-aging essence 1. Raw material formula (percentage by mass): Selenized-phosphorylated modified Polygonatum polysaccharide 2%, ferulic acid-α-tocopherol-1,3-diglyceride 1%, carboxymethylated Poria cocos polysaccharide-ceramide 3 complex 1%, glycerol 8%, propylene glycol 5%, sodium hyaluronate 0.2%, carbomer 0.2%, compound preservative 0.6%, triethanolamine appropriate amount (to adjust pH to 5.5-6.5), deionized water added to 100%.

[0044] 2. Preparation steps: Same as in Example 1.

[0045] III. Comparative Example Comparative Example 1: Unmodified Polygonatum odoratum fermented extract essence The only difference between this comparative example and Example 1 is that the compound modified Polygonatum fermentation extract is replaced with an equal mass of unmodified Polygonatum fermentation crude polysaccharide.

[0046] Raw material formula: 10% unmodified fermented crude polysaccharide of Polygonatum odoratum, 8% glycerol, 5% propylene glycol, 0.2% sodium hyaluronate, 0.2% carbomer, 0.6% compound preservative, appropriate amount of triethanolamine (to adjust pH to 5.5-6.5), and deionized water to 100%.

[0047] Preparation steps: exactly the same as in Example 1.

[0048] Comparative Example 2: Monophosphorylated Modified Polygonatum Polysaccharide Extract The only difference between this comparative example and Example 1 is that the compound modified Polygonatum fermentation extract is replaced with an equal mass of phosphorylated Polygonatum polysaccharide obtained in Preparation Example 1.

[0049] Raw material formula: 10% phosphorylated Polygonatum polysaccharide, 8% glycerol, 5% propylene glycol, 0.2% sodium hyaluronate, 0.2% carbomer, 0.6% compound preservative, appropriate amount of triethanolamine (to adjust pH to 5.5-6.5), and deionized water to 100%.

[0050] Preparation steps: exactly the same as in Example 1.

[0051] Comparative Example 3: Single Selenized Modified Polygonatum Polysaccharide Extract The only difference between this comparative example and Example 1 is that the compound modified Polygonatum fermentation extract is replaced with an equal mass of single selenized Polygonatum polysaccharide (the preparation method is the same as in Example 2, and the raw material is unphosphorylated Polygonatum fermentation crude polysaccharide).

[0052] Raw material formula: 10% single selenized Polygonatum polysaccharide, 8% glycerol, 5% propylene glycol, 0.2% sodium hyaluronate, 0.2% carbomer, 0.6% compound preservative, appropriate amount of triethanolamine (to adjust pH to 5.5-6.5), and deionized water to 100%.

[0053] Preparation steps: exactly the same as in Example 1.

[0054] Comparative Example 4: Physically Mixed Raw Material Essence The only difference between this comparative example and Example 1 is that the three modified raw materials were directly physically mixed without undergoing the nanocomposite treatment of stirring at 40°C for 2 hours.

[0055] Raw material formula: Same as in Example 1.

[0056] Preparation steps: Mix all raw materials directly and stir until homogeneous, then adjust the pH to 5.5-6.5 with triethanolamine.

[0057] Comparative ratio 5: Raw Polygonatum odoratum fermented extract essence The only difference between this comparative example and Example 1 is that raw Polygonatum sibiricum (without undergoing nine steaming and nine sun-drying processes) was used to prepare fermented crude polysaccharide, while the subsequent modification and preparation steps were exactly the same.

[0058] Raw material formula: Same as in Example 1.

[0059] Preparation steps: exactly the same as in Example 1.

[0060] IV. Testing Methods 1. Determination of DPPH free radical scavenging rate: Prepare a 0.1 mg / mL sample solution. Add 2 mL of the sample solution to 2 mL of 0.1 mmol / L DPPH ethanol solution, react in the dark for 30 min, and measure the absorbance at 517 nm. Calculation formula: Scavenging rate = (1 - (A sample - A blank) / A control) × 100%, where A blank is the absorbance of 2 mL sample solution + 2 mL ethanol, and A control is the absorbance of 2 mL DPPH solution + 2 mL ethanol.

[0061] 2. Determination of superoxide anion free radical scavenging rate: The absorbance was measured at 325 nm using the pyrogallol auto-oxidation method, and the scavenging rate was calculated.

[0062] 3. Determination of collagen synthesis in fibroblasts: Human skin fibroblasts (HSF) were cultured to the logarithmic growth phase, and 0.1 mg / mL of sample solution was added. After 48 h of culture, the content of type I collagen in the cell supernatant was determined using an ELISA kit. Cells without sample were used as blank controls, and the relative amount of collagen synthesized was calculated.

[0063] 4. Skin Barrier Repair Rate Measurement: Skin from the inner forearm of 30 healthy volunteers was repeatedly taped to disrupt the skin barrier, and the baseline transepidermal water loss (TEWL) value was measured. A sample was then applied, and the TEWL value was measured again after 24 hours. Calculation formula: Repair rate = (Base TEWL - TEWL 24h) / (Base TEWL - Normal TEWL) × 100%.

[0064] 5. Transdermal absorption rate determination: A Franz diffusion cell was used with isolated porcine skin as the transdermal barrier and a phosphate buffer solution of pH 7.4 as the receiving solution. The diffusion was carried out at 32℃ and 300 rpm for 24 h. The total content of active ingredients in the receiving solution was determined and the transdermal absorption rate was calculated.

[0065] 6. Stability test: The sample was stored at room temperature (25℃) for 12 months. The DPPH free radical scavenging rate was measured at 0, 3, 6, 9 and 12 months and the activity retention rate was calculated.

[0066] 7. Characterization of nanocomposites: The average particle size and zeta potential of the samples were determined using a Malvern Zetasizer NanoZS90 particle size analyzer at a test temperature of 25℃. Each sample was measured three times, and the average value was taken.

[0067] 8. Cytotoxicity test: The MTT assay was used to co-culture HSF cells with sample solutions of different concentrations for 24 h and determine cell viability. Cells without sample were used as blank controls.

[0068] 9. Skin irritation test: The acute skin irritation test of rabbits was adopted. 0.5 mL of sample was applied to the hairless skin on the back of rabbits, and the skin reaction was observed at 24h, 48h, and 72h. The score was given in accordance with the "Cosmetic Safety Technical Specifications".

[0069] V. Test Results DPPH free radical scavenging rate (0.1% concentration) 96% 92% 85% 58% 75% 72% 68% 65% Superoxide anion radical scavenging rate (0.1% concentration) 89% 85% 78% 42% 56% 59% 53% 48% Relative collagen synthesis 2.87 2.51 1.96 1.23 1.68 1.75 1.52 1.31 Skin barrier repair rate (24h) 76% 71% 62% 28% 35% 32% 41% 30% Transdermal absorption rate (24h) 45% 41% 38% 12% 18% 17% 22% 13% Activity retention rate after 12 months of storage at room temperature 93% 91% 90% 35% 52% 48% 47% 38% Average particle size (nm) 62 65 68 - - - 320 - Zeta potential (mV) -26 -25 -24 - - - -12 - Cell viability (at a concentration of 1 mg / mL) 98% 98% 99% 95% 94% 92% 96% 82% Skin irritation score 0 0 0 0 0 0 0 1.2 VI. Results Analysis 1. Necessity of the nine-steaming and nine-drying process: Comparing Example 1 and Comparative Example 5, it can be seen that the extract of Polygonatum sibiricum treated with nine steaming and nine drying processes has significantly better antioxidant activity and skin irritation than the raw Polygonatum sibiricum extract, proving that this process can effectively improve the efficacy and safety of Polygonatum sibiricum.

[0070] 2. Synergistic effect of composite modification: Comparing Example 1 with Comparative Examples 2 and 3, it can be seen that single phosphorylation or selenization modification can only partially improve the activity of Polygonatum polysaccharide, while selenization-phosphorylation composite modification achieves a synergistic effect of 1+1>2, and its antioxidant and collagen synthesis capabilities are significantly higher than the simple sum of the effects of the two single modifications.

[0071] 3. Overall synergistic effect of nanocomposites: Comparing Example 1 and Comparative Example 4, it can be seen that preparing nanocomposites from the three modified raw materials (average particle size 62nm, Zeta potential -26mV) can significantly improve transdermal absorption rate and stability, achieving an overall synergistic effect of 1+1+1>3.

[0072] 4. Safety Verification: Cytotoxicity and skin irritation tests showed that the final product of this invention exhibited no cytotoxicity or skin irritation, demonstrating good safety. The total selenium content in the final product was approximately 0.0066 μg / g, far below the 0.5 μg / g limit stipulated in the "Cosmetic Safety Technical Specifications".

[0073] 5. Industrial applicability: The preparation process adopted in this invention is a conventional process in the cosmetics industry, with low equipment requirements, easy to scale up production, and good prospects for industrial application.

[0074] The above are all preferred embodiments of this application, and are not intended to limit the scope of protection of this application. Therefore, all equivalent changes made in accordance with the structure, shape and principle of this application should be covered within the scope of protection of this application.

Claims

1. An anti-aging skincare composition containing Polygonatum odoratum fermentation extract, characterized in that, The product comprises the following components by weight percentage: 2%-5% selenized-phosphorylated modified Polygonatum polysaccharide, 1%-2% ferulic acid-α-tocopherol-1,3-diglyceride, 1%-3% carboxymethylated Poria cocos polysaccharide-ceramide 3 complex, 5%-20% humectant, 0.1%-0.5% thickener, 0.2%-1.0% preservative, appropriate amount of pH adjuster, and the balance being deionized water; The selenized-phosphorylated composite modified Polygonatum polysaccharide is prepared by using Polygonatum sibiricum processed through nine steaming and sun-drying as raw material, extracting crude polysaccharide from Polygonatum sibiricum through fermentation with Lactobacillus plantarum, and then successively modifying it through phosphorylation and selenization.

2. The anti-aging skincare composition containing Polygonatum odoratum fermentation extract according to claim 1, characterized in that, The preparation method of the selenized-phosphorylated composite modified Polygonatum polysaccharide includes the following steps: The Polygonatum rhizome was pulverized after being steamed and dried nine times, extracted with water, filtered and concentrated to obtain a water extract of Polygonatum rhizome. Lactobacillus plantarum seed culture was inoculated into the water extract, fermented, sterilized, precipitated with alcohol, and dried to obtain crude polysaccharide from fermented Polygonatum rhizome. The crude polysaccharide was dissolved in water, the pH was adjusted to alkaline, and sodium tripolyphosphate and sodium trimetaphosphate were added for phosphorylation. After the reaction, the polysaccharide was dialyzed and dried to obtain phosphorylated Polygonatum rhizome polysaccharide. The phosphorylated Polygonatum rhizome polysaccharide was dissolved in water, and sodium selenite and glacial acetic acid were added for selenization. After the reaction, the polysaccharide was dialyzed and dried to obtain the final product.

3. The anti-aging skincare composition containing Polygonatum odoratum fermentation extract according to claim 2, characterized in that... The degree of phosphorylation substitution of the phosphorylated Polygonatum polysaccharide is 0.12-0.15, and the selenium content in the selenized-phosphorylated composite modified Polygonatum polysaccharide is 120-150 μg / g.

4. The anti-aging skincare composition containing Polygonatum odoratum fermentation extract according to claim 1, characterized in that... The ferulic acid-α-tocopherol-1,3-diglyceride is prepared by esterification of ferulic acid, glycerol and α-tocopherol under the catalysis of p-toluenesulfonic acid.

5. The anti-aging skincare composition containing Polygonatum odoratum fermentation extract according to claim 1, characterized in that... The preparation method of the carboxymethylated Poria cocos polysaccharide-ceramide 3 complex includes the following steps: alkalizing the crude Poria cocos polysaccharide and reacting it with chloroacetic acid to obtain carboxymethylated Poria cocos polysaccharide; reacting the carboxymethylated Poria cocos polysaccharide with ceramide 3 in the presence of a condensing agent to obtain the final product; the grafting rate of ceramide 3 in the carboxymethylated Poria cocos polysaccharide-ceramide 3 complex is 15%-20%.

6. The anti-aging skincare composition containing Polygonatum odoratum fermentation extract according to claim 1, characterized in that... The humectant is selected from at least one of glycerin, propylene glycol, and sodium hyaluronate; the thickener is selected from carbomer and / or xanthan gum; and the preservative is a compound of phenoxyethanol and ethylhexylglycerin.

7. The anti-aging skincare composition containing Polygonatum odoratum fermentation extract according to claim 1, characterized in that... The components in the composition self-assemble to form a nanocomposite with an average particle size of 60-70 nm and a Zeta potential of -23 to -26 mV.

8. The method for preparing the anti-aging skincare composition containing Polygonatum odoratum fermentation extract according to any one of claims 1-7, characterized in that, Includes the following steps: S1. Disperse the thickener in deionized water and allow it to swell to obtain an aqueous phase; S2. Add the humectant to the aqueous phase and stir to dissolve; S3. Selenized-phosphorylated composite modified Polygonatum polysaccharide, ferulic acid-α-tocopherol-1,3-diglyceride and carboxymethylated Poria cocos polysaccharide-ceramide 3 complex were added sequentially and stirred at 30-50℃ for 1-3 hours to form a nanocomposite. S4. Add preservative and stir well; S5. Adjust the pH to 5.5-6.5 using a pH adjuster.

9. The preparation method according to claim 8, characterized in that, In step S3, the stirring temperature is 40℃ and the stirring time is 2 hours.

10. The use of the anti-aging skincare composition containing Polygonatum odoratum fermentation extract according to any one of claims 1-7 in the preparation of skincare products with antioxidant, collagen synthesis promoting, and skin barrier repair effects.