Composition with anti-aging effect and preparation method thereof

Abstract

The invention discloses a composition with an anti-aging effect and a method, and belongs to the technical field of cosmetic compositions.The composition is prepared from active ingredients and auxiliary materials, and the active ingredients comprise, by weight, 0.01-20% of chlorogenic acid, 0.01-20% of sodium hyaluronate, 0.01-20% of sodium hyaluronate, 0.01-20% of sodium hyaluronate and the balance water; 0.1 to 20% of a dracocephalum dracocephalum extract; 0.01 to 20 percent of fullerene; 0.1-30% of red yeast rice; 1-30% of kelp; the auxiliary material comprises 10%-40% of butanediol and the balance of deionized water; wherein the mass content ratio of C60 to C70 in the fullerene is (0.6-15): 1, and the invention discloses the composition which realizes multi-target anti-aging and is simple in process through the synergistic effect of the components.

Description

Technical Field

[0001] This invention relates to the field of cosmetic composition technology, and in particular to a composition with anti-aging effects and its preparation method. Background Technology

[0002] Skin aging is the result of the combined effects of internal physiological changes and external environmental factors, mainly manifested as wrinkles, skin laxity, decreased elasticity, and pigmentation. Currently, the core mechanisms of skin aging include free radical accumulation, UV damage, collagen loss, extracellular matrix destruction, skin glycation, and slowed cell metabolism.

[0003] In existing technologies, anti-aging cosmetics mostly use single active ingredients such as vitamin C, retinol, fullerene, etc., or simple compounded compositions, which have problems such as limited efficacy, poor synergy of ingredients, and low utilization rate of active ingredients. For example, fullerene is prone to agglomeration when used alone, and its poor dispersibility limits its antioxidant effect; plant extracts, without enzymatic hydrolysis and oxidation treatment, do not release their active ingredients sufficiently, making it difficult to exert their optimal efficacy. Therefore, developing a composition with strong synergistic effects, multi-target anti-aging, and effectively improved utilization rate of active ingredients has become an urgent technical problem to be solved in the cosmetics field. Summary of the Invention

[0004] In order to overcome the shortcomings of the prior art, the technical problem to be solved by the present invention is to propose a composition that achieves multi-target anti-aging through the synergistic effect of components and has a simple process.

[0005] To achieve this objective, the present invention adopts the following technical solution: This invention provides a composition with anti-aging effects, comprising, by weight percentage, active ingredients and excipients. The active ingredients include: chlorogenic acid 0.01-20%; dragon's blood extract 0.1-20%; fullerene 0.01-20%; red yeast rice 0.1-30%; kelp 1-30%; the excipients include butylene glycol 10%-40%; the balance being deionized water. The mass ratio of C60 to C70 in the fullerene is 0.6~15 : 1.

[0006] A preferred embodiment of the present invention is that the amount of butylene glycol used is 5-50 times the total weight of chlorogenic acid and dracaena extract.

[0007] The preferred technical solution of the present invention is that the composition is used to regulate the expression of aging genes, prevent ultraviolet damage, scavenge free radicals, enhance cell activity, reconstruct the extracellular matrix, reduce skin glycation, promote cell metabolism, increase collagen synthesis and / or shorten the skin renewal cycle.

[0008] The preferred technical solution of the present invention is that the composition is used to prepare cosmetics with the effects of brightening and whitening the skin, anti-wrinkle and fine line removal, firming the skin, enhancing skin elasticity and / or delaying skin aging, and the amount of the composition added to the cosmetics is 0.01-10%.

[0009] A method for preparing an anti-aging composition, characterized by comprising the following steps: Step S1: Preparation of component A: Step S1.1, alcohol dissolution: Place chlorogenic acid and dracaena extract in a reaction vessel, add butylene glycol as a solvent, and stir at 30°C for 15-20 minutes until completely dissolved; Step S1.2, Ultrasonic dispersion: Add fullerene to the solution obtained in step S1.1, wherein the mass ratio of C60 to C70 in the fullerene is 0.6~15:1, and perform ultrasonic treatment to disperse it uniformly; Step S1.3, Alkalization: Add alkali solution to the dispersion obtained in step S1.2, stir and mix evenly, adjust the pH value of the system to 7.0-8.5, and obtain component A; Step S2, Preparation of component B: Step S2.1, Enzymatic hydrolysis: After crushing the red yeast rice and kelp, add some deionized water to carry out the enzymatic hydrolysis reaction. The enzymatic hydrolysis time is 1-6 hours. Step S2.2, centrifugation: Filter the material after enzymatic hydrolysis in step S2.1 and centrifuge to extract the supernatant; Step S2.3, Oxidation: Add hydrogen peroxide to the supernatant obtained in step S2.2, and stir and oxidize at 25-40℃ for 30-120 min to obtain component B; Step S3, Mixing, Adjustment and Impurity Removal: Step S3.1, Dissolving: Mix component A obtained in step S1 with component B obtained in step S2, add the remaining deionized water, heat and stir to make them fully miscible, and adjust the pH of the mixture to 5.0-7.5. Step S3.2, centrifugation: Centrifuge the mixture obtained in step S3.1 to remove the precipitate and collect the supernatant, which is the anti-aging composition.

[0010] A preferred embodiment of the present invention is that, in step S1.2, the power of the ultrasonic treatment is 200-1000W and the treatment time is 10-60min.

[0011] A preferred embodiment of the present invention is that, in step S2.1, the enzymatic hydrolysis temperature is 40-60℃.

[0012] A preferred embodiment of the present invention is that, in step S2.3, the amount of hydrogen peroxide added is 0.1-5% of the total weight of the supernatant.

[0013] The preferred technical solution of the present invention is that, in step S3.1, the heating temperature is 40-80℃ and the heating and stirring time is 10-60min; in step S3.2, the centrifugation speed is 3000-5000r / min and the centrifugation time is 10-20min.

[0014] The preferred technical solution of the present invention is that the preparation method of the dragon blood extract is as follows: reflux extraction twice with 70% ethanol solution (material-liquid ratio 1:10), and the total phenol content is measured to be ≥15% after concentration of the extract; the purity of the chlorogenic acid is ≥98%.

[0015] The beneficial effects of this invention are as follows: 1. This invention utilizes butylene glycol to promote the penetration of active ingredients through the skin barrier, chlorogenic acid to promote collagen synthesis and resist UV damage, and dragon's blood extract to exert antioxidant and cell cycle regulation effects by inhibiting nuclear transcription factor NF-κB. Fullerene (in a specific ratio of C60 to C70) effectively scavenge free radicals. The active ingredients released after the enzymatic hydrolysis and oxidation of red yeast rice and kelp can reduce skin glycation and reconstruct the extracellular matrix. Through the synergistic effect of these components, multi-dimensional anti-aging is achieved. 2. This invention uses butanediol dissolution combined with ultrasonic dispersion process to solve the problem that fullerene is insoluble in water, improve its dispersibility and bioavailability, so that fullerene can be stably dispersed in the composition, improve water solubility, and make it easy to add to various water-based cosmetics; 3. This invention utilizes the red yeast rice's own biological enzymes for fermentation and enzymatic hydrolysis, eliminating the need for exogenous enzymes, effectively reducing production costs, and avoiding the risk of impurity residues caused by exogenous enzymes. The process is more environmentally friendly and safer. Furthermore, after enzymatic hydrolysis, the active ingredients of red yeast rice and kelp are fully released, and hydrogen peroxide oxidation further enhances the activity of the ingredients. 4. The composition of the present invention can be added to various cosmetics such as creams, lotions, and serums. The amount added is only 0.01-10%, which can take effect and achieve the effects of brightening skin, anti-wrinkle and firming. It is low in cost and has significant effects. Attached Figure Description

[0016] Figure 1 This is a flowchart of the composition preparation process provided in a specific embodiment of the present invention. Detailed Implementation

[0017] The technical solution of the present invention will be further described below with reference to the accompanying drawings and specific embodiments.

[0018] Example 1 A composition with anti-aging effects, comprising the following components by weight percentage: chlorogenic acid 1%, dragon's blood extract 5%, fullerene 0.5%, red yeast rice 10%, kelp 15%, butylene glycol 20%, and the balance being deionized water, wherein the mass ratio of C60 to C70 in the fullerene is C60:C70=5:1. A method for preparing an anti-aging composition includes the following steps: Step S1: Preparation of component A: Chlorogenic acid and dracaena extract were placed in a reaction vessel, butanediol was added as a solvent, and the mixture was stirred at 30°C for 15 min until completely dissolved. Fullerene was added and the mixture was ultrasonically treated at 400W for 20 min until no obvious particles were visible in the solution. 1 mol / L sodium hydroxide solution was added dropwise to adjust the pH to 7.5, and the mixture was stirred for 5 min to obtain component A. Step S2: Preparation of component B: After crushing red yeast rice and kelp, add 10 times the total weight of red yeast rice and kelp in deionized water. Use the biological enzymes of red yeast rice to ferment and hydrolyze at 45°C for 2 hours, stirring once every 30 minutes. After filtration, centrifuge at 3500 r / min for 15 minutes, collect the supernatant, add 1% hydrogen peroxide to the supernatant, and stir and oxidize at 30°C for 45 minutes to obtain component B. Step S3, Mixing, Adjustment and Impurity Removal: Mix component A and component B, add the remaining deionized water, stir at 50°C for 20 min, add 1 mol / L citric acid to adjust the pH to 6.0, centrifuge at 3500 r / min for 15 min, and collect the supernatant to obtain the composition.

[0019] Example 2 A composition with anti-aging effects, comprising the following components by weight percentage: chlorogenic acid 0.01%, dragon's blood extract 0.1%, fullerene 0.01%, red yeast rice 0.1%, kelp 1%, butylene glycol 10%, and the balance being deionized water, wherein the mass ratio of C60 to C70 in the fullerene is C60:C70=0.6:1; A method for preparing an anti-aging composition includes the following steps: Step S1: Preparation of component A: Chlorogenic acid and dracaena extract were placed in a reaction vessel, butanediol was added as a solvent, and the mixture was stirred at 30°C for 20 min until completely dissolved. Fullerene was added and ultrasonically treated at 200W power for 10 min until evenly dispersed. 1 mol / L sodium hydroxide solution was added dropwise to adjust the pH to 7.0 to obtain component A. Step S2: Preparation of component B: After crushing red yeast rice and kelp, add 20 times the total weight of red yeast rice and kelp in deionized water. Use the biological enzymes of red yeast rice to ferment and hydrolyze it in a sealed container at 40°C for 1 hour. After filtration, centrifuge at 3000 r / min for 10 min, collect the supernatant, add 0.1% hydrogen peroxide to the supernatant, and stir and oxidize at 25°C for 30 min to obtain component B. Step S3, Mixing, Adjustment and Impurity Removal: Mix component A and component B, add the remaining deionized water, stir at 40°C for 10 min, add 1 mol / L citric acid to adjust the pH to 5.0, centrifuge at 3000 r / min for 10 min, and collect the supernatant to obtain the composition.

[0020] Example 3 A composition with anti-aging effects, comprising the following components by weight percentage: chlorogenic acid 5%, dragon's blood extract 5%, fullerene 5%, red yeast rice 15%, kelp 15%, butylene glycol 25%, and the balance being deionized water, wherein the mass ratio of C60 to C70 in the fullerene is C60:C70=15:1. A method for preparing an anti-aging composition includes the following steps: Step S1: Preparation of component A: Chlorogenic acid and dracaena extract were placed in a reaction vessel, butanediol was added as a solvent, and the mixture was stirred at 30°C for 15 min until completely dissolved. Fullerene was added and the mixture was ultrasonically treated at 1000W power for 60 min until it was evenly dispersed. 1 mol / L sodium hydroxide solution was added dropwise to adjust the pH to 8.5 to obtain component A. Step S2, Preparation of Component B: After crushing red yeast rice and kelp, add 8 times the total weight of red yeast rice and kelp in deionized water. Use the biological enzymes of red yeast rice to ferment and hydrolyze at 60°C for 6 hours. After filtration, centrifuge at 5000 r / min for 20 min, collect the supernatant, add 5% hydrogen peroxide to the supernatant, and stir and oxidize at 40°C for 120 min to obtain component B. Step S3, Mixing, Adjustment and Removal: Mix component A and component B, add the remaining deionized water, stir at 80°C for 60 min, add 1 mol / L citric acid to adjust the pH to 7.5, centrifuge at 5000 r / min for 20 min, and collect the supernatant to obtain the composition.

[0021] Comparative Example 1 A composition with anti-aging effects, comprising the following components by weight percentage: chlorogenic acid 1%, dragon's blood extract 5%, red yeast rice 10%, kelp 15%, butylene glycol 20%, and the balance being deionized water. The method for preparing the anti-aging composition is the same as in Example 1, but fullerene is not added in step S1.

[0022] Comparative Example 2 A composition with anti-aging effects, wherein the components are the same as in Example 2 by weight percentage; The method for preparing the anti-aging composition is the same as in Example 2, but in step S2, the sealed fermentation and enzymatic hydrolysis step is omitted, and the red yeast rice is directly crushed and then added to 12 times the amount of deionized water, stirred at 45°C for 2 hours, without activating its own biological enzymes.

[0023] Comparative Example 3 A composition with anti-aging effects, wherein the components are the same as those in Example 3 by weight percentage; The method for preparing the anti-aging composition is the same as in Example 3, except that in step S1, after adding fullerene, the mixture is stirred at 300 r / min for 30 min without ultrasonic treatment.

[0024] Performance testing of anti-aging compositions: I. Test Sample Experimental group: Compositions prepared in Examples 1-3; Control group: The compositions prepared in comparative examples 1-4; Blank group: Deionized water.

[0025] II. Test Items and Methods 1. DPPH free radical scavenging rate test Methods: In accordance with the "Cosmetic Safety Technical Specifications" (2024 edition), each sample was diluted to a mass concentration of 1%. 2 mL of sample solution was taken and 2 mL of 0.1 mmol / L DPPH ethanol solution was added. The reaction was carried out in the dark for 30 min, and the absorbance at 517 nm was measured (sample A). The blank group was replaced with deionized water (blank A), and the control group was replaced with ethanol instead of DPPH solution (correct A). Calculation formula: Clearance rate (%) = [1 - (A sample - A pair) / A blank] × 100%.

[0026] 2. Collagen synthesis test Methods: Human skin fibroblasts (HSF) were cultured. The sample group was given 1% of the composition, while the control group was not given any composition. After 48 hours of culture, the content of type I collagen in the cell supernatant was detected by ELISA kit.

[0027] 3. Skin glycation inhibition rate Methods: Bovine serum albumin (BSA)-glucose system was used to simulate skin glycation. After adding the sample, the mixture was incubated at 37°C for 7 days, and the fluorescence intensity at 440 nm (characteristic fluorescence of glycation products) was measured. Calculation formula: Inhibition rate (%) = [(A pair - A sample) / A pair] × 100% (A pair is the fluorescence value of the system without sample / blank group).

[0028] 4. Cell viability Methods: MTT assay was used. HSF cells were co-cultured with 1% sample / equal volume of deionized water (blank group) for 24 h. The absorbance at 490 nm was measured and the cell viability was calculated (the viability of the control group was set at 100%).

[0029] 5. Human body anti-aging efficacy test (1) Test subjects: 30 healthy female subjects aged 35-55 were selected. All of them met the following conditions: obvious fine lines on the face (corners of the eyes, nasolabial folds), decreased skin elasticity, dull skin tone, no history of skin diseases and allergies, and no use of any anti-aging cosmetics in the month before the test.

[0030] (2) Test sample: an emulsion containing 5% of the composition in Example 1.

[0031] (3) Test period: 28 days (skin physiological renewal cycle). Apply to the face after cleansing in the morning and evening, using about 0.5g per application, and gently massage until fully absorbed.

[0032] (4) Testing instruments: The Courage+Khazaka MPA580 skin tester was used to detect skin wrinkle parameters (Rz: average wrinkle depth), elasticity parameters (R2: skin elasticity recovery rate), and brightness parameters (L value), combined with the subject's self-score and blind evaluation by a professional dermatologist.

[0033] III. Test Results Table 1

[0034] Table 2

[0035] IV. Results Analysis Regarding Table 1: The free radical scavenging rate, collagen synthesis, and glycation inhibition rate in Examples 1 to 3 were significantly higher than those in Comparative Examples 1 to 3, indicating the synergistic effect of active ingredients such as chlorogenic acid and fullerene, and the necessity of the combination of butanediol dissolution, enzymatic hydrolysis, and ultrasonic dispersion processes.

[0036] Compared to Example 1, which lacks fullerene, Comparative Example 1 showed a 33.7% decrease in DPPH scavenging rate, a 34% decrease in collagen synthesis, and a 33.6% decrease in skin anti-glycation inhibition rate. These significant decreases indicate that fullerene is a core component for free radical scavenging, collagen synthesis, and skin glycation inhibition. Comparative Example 2, using traditional extraction methods, resulted in insufficient release of active ingredients, leading to a 31.9% decrease in DPPH scavenging rate, a 28.4% decrease in collagen synthesis, and a 35% decrease in skin anti-glycation inhibition rate compared to Example 2. Therefore, traditional extraction methods cannot fully release the active ingredients of red yeast rice and kelp. This invention can better release the active ingredients of both. Comparative Example 3, which omits ultrasonic treatment compared to Example 3, showed a 30.4% decrease in DPPH scavenging rate, a 32.9% decrease in collagen synthesis, and a 33.1% decrease in skin anti-glycation inhibition rate. The lack of ultrasonic treatment resulted in poor fullerene dispersibility, leading to reduced utilization.

[0037] The efficacy indicators of the blank group were close to the baseline, proving that the efficacy of the embodiment comes from the active ingredients and optimized process, and the cell survival rate of all samples was close to 100%, indicating high safety.

[0038] Regarding Table 2: After 28 days, the average depth of facial wrinkles in the subjects decreased by 31.1% compared to baseline, with the most significant improvement in fine lines around the eyes, which showed noticeable fading after 14 days. The average depth of nasolabial folds decreased by 29.8% after 28 days, indicating that the composition can effectively reduce fine lines and improve wrinkle depth. The skin elasticity recovery rate (R2) increased by 33.6%, and the subjects' facial contours became firmer, indicating that the composition can enhance skin elasticity and reconstruct the extracellular matrix. The skin L value increased by 12.2%, improving dull skin tone and resulting in a more even and radiant overall skin tone, confirming the brightening and whitening effects of the composition. This invention's composition, through the multi-dimensional synergistic effects of chlorogenic acid, dragon's blood extract, fullerene, red yeast rice, and kelp, simultaneously achieves anti-photoaging, free radical scavenging, skin glycation inhibition, collagen synthesis promotion, wrinkle reduction, skin refinement, and brightening effects. In the preparation process, constant-temperature dissolution with 30°C butylene glycol ensures full dissolution of active ingredients; ultrasonic dispersion technology solves the fullerene dispersion problem; enzymatic hydrolysis increases the active ingredient extraction rate by more than 30% compared to traditional solvent methods; hydrogen peroxide precisely activates the extract activity; and uniform citric acid pH adjustment ensures system stability. Performance tests show that the composition achieves a DPPH scavenging rate of over 85%, a glycation inhibition rate of over 80%, and a 2.8-3.5 times increase in type I collagen synthesis compared to the control group. It also improves wrinkle depth, increases skin elasticity recovery rate by 33.6%, and increases skin L-value by 12.2%, making it suitable for various anti-aging cosmetics.

[0039] This invention has been described through preferred embodiments. Those skilled in the art will understand that various changes or equivalent substitutions can be made to these features and embodiments without departing from the spirit and scope of the invention. This invention is not limited to the specific embodiments disclosed herein; other embodiments falling within the scope of the claims are also within the protection scope of this invention.

Claims

1. A composition having an anti-aging effect, characterized by: The active ingredients and adjuvants include, by weight percentage: chlorogenic acid 0.01-20%; extract of Herba Epimedii 0.1-20%; fullerene 0.01-20%; monascus 0.1-30%; kelp 1-30%; the adjuvants include butanediol 10%-40%, and the balance is deionized water; The mass content ratio of C60 to C70 in the fullerene is 0.6-15:

1.

2. The composition with anti-aging effect according to claim 1, characterized in that: The amount of butanediol is 5-50 times the total weight of chlorogenic acid and extract of Herba Epimedii.

3. The composition with anti-aging effect according to claim 1, characterized in that: The composition is used for regulating expression of aging genes, preventing ultraviolet damage, scavenging free radicals, enhancing cell activity, restructuring extracellular matrix, reducing skin glycation, promoting cell metabolism, increasing collagen synthesis, and / or shortening skin renewal cycle.

4. The composition with anti-aging effect according to claim 1, characterized in that: The composition is used for preparing cosmetics with the effects of lightening and whitening skin, anti-wrinkle and fine line, skin tightening, enhancing skin elasticity, and / or delaying skin aging, and the addition amount of the composition in the cosmetics is 0.01-10%.

5. A method of preparing an anti-aging composition according to any one of claims 1 to 4, characterized in that, The method comprises the following steps: Step S1, preparing component A: Step S1.1, alcohol solution: placing chlorogenic acid and extract of Herba Epimedii in a reaction kettle, adding butanediol as a solvent, stirring at 30°C for 15-20 min until complete dissolution; Step S1.2, ultrasonic dispersion: adding fullerene to the solution obtained in step S1.1, and the mass content ratio of C60 to C70 in the fullerene is 0.6-15:1, and performing ultrasonic treatment to make it uniformly dispersed; Step S1.3, alkalization: adding lye to the dispersion obtained in step S1.2, stirring and mixing uniformly, adjusting the pH value of the system to 7.0-8.5 to obtain component A; Step S2, preparing component B: Step S2.1, enzymatic hydrolysis: after crushing monascus and kelp, adding part of deionized water for enzymatic hydrolysis reaction, and the enzymatic hydrolysis time is 1-6 hours; Step S2.2, centrifugation: filtering and centrifuging the material after enzymatic hydrolysis in step S2.1 to extract the supernatant; Step S2.3, oxidation: adding hydrogen peroxide to the supernatant obtained in step S2.2, stirring and oxidizing at 25-40°C for 30-120 min to obtain component B; Step S3, mixing, adjusting and impurity removal: Step S3.1, dissolution: mixing component A prepared in step S1 with component B prepared in step S2, adding the remaining deionized water, heating and stirring to make them fully miscible, and adjusting the pH value of the mixed solution to 5.0-7.5; Step S3.2, centrifugation: centrifuging the mixed solution obtained in step S3.1 to remove the precipitate, and collecting the obtained supernatant, which is the anti-aging composition.

6. The preparation method according to claim 5, characterized in that: In step S1.2, the ultrasonic treatment power is 200-1000W, and the treatment time is 10-60 min.

7. The preparation method according to claim 5, characterized in that: In the step S2.1, the enzymolysis temperature is 40-60℃.

8. The preparation method according to claim 5, characterized in that: In the step S2.3, the amount of hydrogen peroxide added is 0.1-5% of the total weight of the supernatant.

9. The preparation method according to claim 5, characterized in that: In the step S3.1, the heating temperature is 40-80℃, and the heating and stirring time is 10-60 min; in the step S3.2, the centrifugal speed is 3000-5000 r / min, and the centrifugal time is 10-20 min.

10. The composition with anti-aging effect according to claim 1, characterized in that: The preparation method of the Herba Epimedii extract is as follows: 70% ethanol solution (solid-liquid ratio 1:10) is used for reflux extraction for 2 times, and the total phenol content of the extracted solution after concentration is ≥15%; the purity of the chlorogenic acid is ≥98%.

Images