Agarwood skin care product with firming repair, bacteriostatic and moisture locking and preparation method thereof

Abstract

The application discloses an aquilaria sinensis skin care product with firming repair and bacteriostatic water-locking moisturizing functions and a preparation method thereof. The skin care product comprises core components such as aquilaria sinensis extract 0.5-3.0 parts, composite polypeptide 0.5-3.0 parts and cell activator 0.08-0.25 parts. High-activity raw materials are prepared by using specific processes such as supercritical CO2 extraction, ultrasonic-microwave synergistic extraction and purification. The final product is prepared by processes such as low-temperature emulsification, gradient temperature reduction, nitrogen protection and step-by-step addition of active substances. The MIC values of the skin care product for staphylococcus aureus, escherichia coli and propionibacterium acnes are as low as 1.0 mg / mL, 1.5 mg / mL and 0.8 mg / mL respectively, the 24h moisturizing rate reaches 88.2%, the relative synthesis rate of COL-I is 178.6%, the relative synthesis rate of HA is 163.4%, and the DPPH free radical scavenging IC 50 32.2 μg / mL, and synergistic effects of bacteriostasis, moisturizing and repair are achieved.

Description

Technical Field

[0001] This invention relates to the field of cosmetic technology, and in particular to an agarwood skin care product with firming, repairing, antibacterial, and moisturizing properties, as well as its preparation method. Background Technology

[0002] With rising living standards and increased skincare awareness, consumers' demands for skincare products have shifted from basic cleansing and moisturizing to a more refined and diversified pursuit of efficacy. In particular, the demand for comprehensive benefits such as anti-aging, skin barrier repair, maintaining skin microecological balance, and long-lasting hydration is becoming increasingly prominent. Ideally, skincare products should effectively address multiple issues simultaneously, including skin laxity, wrinkle formation, microbial infection, barrier damage, and moisture loss. However, combining multiple active ingredients with different effects presents numerous technical challenges.

[0003] Agarwood ( Aquilaria spp. Agarwood, the heartwood of plants in the genus Aquilaria of the Thymelaeaceae family, is a traditional and precious natural raw material. Its extract is rich in active ingredients such as agaricone, salicylic acid, and flavonoids, which have significant antioxidant, soothing, anti-inflammatory, and skin-damage-repairing effects. In recent years, its application in the cosmetics field has received widespread attention. However, most existing skincare products involving agarwood only use it as a conceptual addition or a single functional ingredient, which has obvious limitations: existing agarwood skincare products mostly focus on single functions such as moisturizing and soothing, failing to effectively synergize agarwood extract with firming, anti-aging, and antibacterial ingredients, making it difficult to meet the multiple skincare needs. Insufficient metabolic activity in skin cells means that even with a combination of multiple active ingredients, they cannot fully exert their effects in promoting collagen synthesis and repairing the matrix. This makes it difficult for ingredients such as peptides and styrofoam to be effectively absorbed and utilized by skin cells, resulting in a lack of cellular-level support for antibacterial, anti-aging, and repairing effects. At the same time, in existing preparation processes, improper control of emulsification temperature and insufficient homogenization pressure lead to uneven emulsion particle size, which easily causes stability problems such as layering and precipitation. The order of adding active ingredients lacks scientific design, and improper addition leads to loss of activity, failing to achieve the expected synergistic activation effect. Summary of the Invention

[0004] In view of this, the present invention proposes an agarwood skin care product with firming, repairing, antibacterial, water-locking and moisturizing properties, and its preparation method, to solve the above problems.

[0005] The technical solution of this invention is achieved as follows: A skin care product made of agarwood with firming, repairing, antibacterial, and moisturizing properties, comprising the following raw materials in parts by weight: 0.5-3.0 parts of agarwood extract, 0.1-0.3 parts of retinol, 0.2-0.8 parts of vitamin E, 0.1-1.0 parts of tea polyphenols, 0.05-0.3 parts of resveratrol, 3.0-8.0 parts of serotonin, 0.5-3.0 parts of complex polypeptides, 0.01-0.1 parts of ergothioneine, 0.5-2.0 parts of ceramides, 1.0-5.0 parts of squalane, 1.0-3.0 parts of panthenol, 1.0-5.0 parts of bifida ferment lysate, 0.1-0.5 parts of tea tree oil, 1.0-3.0 parts of hyaluronic acid, 0.3-1.0 parts of honeysuckle extract, and 0.08-0.25 parts of cell activator.

[0006] Preferably, the agarwood skincare product comprises the following ingredients in parts by weight: 2.0 parts agarwood extract, 0.2 parts retinol, 0.5 parts vitamin E, 0.5 parts tea polyphenols, 0.2 parts resveratrol, 5.0 parts pro-xylane, 1.5 parts complex polypeptide, 0.05 parts ergothioneine, 1.5 parts ceramide, 3.0 parts squalane, 2.0 parts panthenol, 3.0 parts bifida ferment lysate, 0.3 parts tea tree oil, 2.0 parts hyaluronic acid, 0.5 parts honeysuckle extract, and 0.15 parts cell activator. Preferably, the composite polypeptide is palmitoyl pentapeptide-4, palmitoyl tripeptide-1 and acetyl hexapeptide-8 in a weight ratio of (1-3):(1-2):(0.5-1.5).

[0007] Preferably, the extraction method of the agarwood extract includes the following steps: (1) Supercritical CO2 extraction: The agarwood raw material is crushed and extracted with supercritical CO2 at an extraction pressure of 25-35 MPa and a temperature of 45-55℃ to obtain agarwood essential oil. (2) Ultrasonic-assisted extraction: The agarwood raw material residue after extraction in step (1) is mixed with 60-75% v / v ethanol aqueous solution at a mass-volume ratio of 1g: 8-12mL, and extracted for 1-2 hours at 40-50℃ and ultrasonic power of 200-400W. After filtration, extract A is obtained. (3) Hot water extraction: Mix the residue after extraction in step (2) with deionized water at a ratio of 1:10-15, extract at 85-95℃ for 2-3 hours, filter, and obtain extract B; (4) Combining: The agarwood essential oil obtained in step (1), the extract A in step (2) and the extract B in step (3) are combined in a weight ratio of (0.5-2):(2-5):(3-6) and concentrated to a preset concentration to obtain the agarwood extract.

[0008] Preferably, the cell activator is a mixture of Terminalia chebula extract and Edelweiss extract in a weight ratio of (3-5):2.

[0009] Preferably, the extraction method of the Terminalia chebula extract includes the following steps: (1) Enzymatic hydrolysis pretreatment: Take the dried fruit of Terminalia chebula, remove the pit and crush it, add 8-12 times the weight of the raw material of deionized water and adjust the pH to 5.0-5.5, add 0.2-0.3% of the weight of the raw material of compound enzyme and hydrolyze at 50-55℃ for 1.5-2.0h, inactivate and dry to obtain pretreated powder. The compound enzyme is cellulase and xylanase with a mass ratio of 1.3-2.5:1. (2) Ultrasonic-microwave synergistic extraction: Add 10-12 times the weight of 60-65% v / v ethanol solution to the pretreated powder, and add 0.1-0.15% sodium bisulfite as an antioxidant. First, extract with ultrasonic assistance at 45-50℃ for 30-40 min, and then extract with microwave at 55-60℃ and 300-350W for 20-25 min. Filter to obtain the extract. (3) Purification: After concentrating the extract, it is loaded onto an AB-8 macroporous resin column and eluted sequentially with water and 70-75% v / v ethanol solution. The ethanol eluent is collected. (4) Alcohol precipitation and freeze drying: After concentrating the ethanol eluent and precipitating it with alcohol, the supernatant was taken and freeze-dried under vacuum to obtain the refined Terminalia chebula extract.

[0010] Preferably, the extraction method of the Edelweiss extract includes the following steps: (1) Raw material pretreatment: Take sterile cultured Edelweiss callus tissue, freeze dry it under vacuum at -50 to -45℃ until the moisture content is ≤5%, and use low temperature ultrafine pulverization (temperature ≤10℃) to the particle size of 10-20μm. Add 3-5 times its mass of pretreatment solution to the sieved powder and soak it at a constant temperature of 25-30℃ for 1-2h. The pretreatment solution is composed of 0.8-1.2% mannitol, 0.3-0.5% EDTA-2Na and the balance deionized water, and the pH value of the pretreatment solution is adjusted to 5.5-6.0. (2) Extraction: Ultrasonic-microwave combined extraction was adopted, with ultrasonic power of 180-220W, microwave frequency of 2450MHz, microwave power of 300-350W, extraction temperature of 40-45℃, and extraction time of 40-60min.

[0011] Preferably, the preparation method of agarwood skincare products includes the following steps: S1 Raw Material Pretreatment: Mix agarwood extract, honeysuckle extract and 5-10 times the weight of deionized water, stir at 40-50℃ for 30-45 minutes, filter through a 0.22μm filter membrane and set aside; mix retinol, vitamin E, tea tree oil and squalane, heat to 50-60℃ under nitrogen protection to form an oil phase mixture; S2 Emulsification Mixing: Dissolve hyaluronic acid and panthenol in deionized water to form an aqueous phase. Stir at 75-85℃ until completely dissolved. Then add the oil phase mixture to the aqueous phase at a rate of 5-10 ml / min, while shearing and emulsifying at 2000-3000 r / min for 15-25 minutes. S3 compound addition and sterilization: After the temperature of the emulsification system drops to 40-45℃, add Bosein, compound polypeptide, Bifida ferment lysate and cell activator in sequence. Stir for 30-40 minutes, then filter and sterilize using a 0.22μm microfiltration membrane. Dispense under aseptic conditions to obtain the product.

[0012] Preferably, in the preparation method: The mixture of agarwood extract and honeysuckle extract in S1 is extracted with ultrasonic assistance during the stirring process. The ultrasonic power is 200-300W and the frequency is 25-40kHz. The shear temperature during the emulsification stage in S2 is controlled at 78-82℃. After emulsification, 3-5 cycles of homogenization are performed, with a homogenization pressure of 20-30MPa. When adding the active ingredients in S3, a gradient cooling method is used, reducing the temperature by 5°C every 5 minutes until it reaches 40°C. The compound peptides are added in the following order: palmitoyl pentapeptide-4, acetyl hexapeptide-8, and tripeptide-1 copper, with a 5-minute interval between each peptide addition.

[0013] This invention also provides the application of the above-mentioned agarwood skin care products in the preparation of cosmetics with firming, repairing, antibacterial, water-locking and moisturizing functions.

[0014] Compared with the prior art, the beneficial effects of the present invention are: This invention scientifically combines multiple active ingredients, including the anti-inflammatory and repairing properties of agarwood extract, the anti-aging and firming effects of retinol and complex peptides, the plumping and wrinkle-reducing effects of pro-xylene, the barrier-repairing properties of ceramides and squalane, the synergistic antibacterial effects of honeysuckle extract, and the cell-purifying effects of cell activators. This achieves a synergistic effect across multiple targets and pathways, meeting multiple skincare needs such as firming, repair, antibacterial properties, and moisturizing. Through innovative extraction processes, the core active substances in each raw material are maximized and enriched, while ineffective impurities are removed, ensuring the efficacy of the raw materials. Specific preparation methods, including low-temperature addition, gradient cooling, inert gas protection, and a specific order of addition, effectively solve the compatibility and stability challenges of multiple active ingredients in complex formulation systems, extending the product's shelf life and guaranteeing its effectiveness. Detailed Implementation

[0015] To better understand the technical content of this invention, specific embodiments are provided below to further illustrate the invention.

[0016] Unless otherwise specified, the experimental methods used in the embodiments of this invention are all conventional methods.

[0017] Unless otherwise specified, all materials and reagents used in the embodiments of this invention are commercially available.

[0018] The standard names of the substances involved in this invention are as follows: Agarwood extract is an extract of agarwood (Aquilaria LIGNUM RESINATUM); The Bifida Ferment Lysate is a fermentation product of Bifida Ferment Lysate. Honeysuckle extract is an extract of Lonicera japonica flowers; Terminalia chebula extract is an extract of Terminalia chebula. The extract of Leontopodium alphanum is an extract of callus tissue from Leontopodium alphanum.

[0019] Example 1: Preparation of Agarwood Extract (1) Supercritical CO2 extraction: 100g of agarwood raw material was crushed and put into a supercritical CO2 extraction device. The extraction pressure was set to 30MPa, the temperature to 50℃, and the extraction time to 2 hours. 0.8g of agarwood essential oil was obtained.

[0020] (2) Ultrasonic-assisted extraction: The residue after extraction was mixed with 70% v / v ethanol aqueous solution (material-liquid ratio 1:10 g / mL), and extracted at 45℃ and 300W ultrasonic power for 1.5 hours. After filtration, extract A was obtained.

[0021] (3) Hot water extraction: Mix the residue after extraction in step (2) with deionized water (material-liquid ratio 1:12), extract at 90°C for 2.5 hours, filter, and obtain extract B.

[0022] (4) Compounding: Agarwood essential oil, extract A and extract B are mixed in a weight ratio of 1:3:5 and concentrated under reduced pressure at 50°C to a relative density of 1.20 (25°C) to obtain agarwood extract paste.

[0023] Example 2: Preparation of Terminalia chebula extract (1) Enzymatic hydrolysis pretreatment: Take 100g of dried Terminalia chebula fruit, remove the pit and crush it, add 1000mL of deionized water, adjust the pH to 5.2 with citric acid, add 0.25g of compound enzyme (cellulase: xylanase = 2:1), hydrolyze at 52℃ for 1.8h, then heat at 95℃ for 10min to inactivate the enzyme, filter, and vacuum dry the filter residue at 58℃ to obtain pretreated powder.

[0024] (2) Ultrasonic-microwave synergistic extraction: Add 1100 mL of 63% v / v ethanol solution (11 times its weight) to the pretreated powder, and add 0.12 g of sodium bisulfite. First, extract under ultrasonic conditions at 48℃ and 350 W for 35 min, then transfer to a microwave device and extract for 22 min at a power of 320 W and a temperature of 58℃. Filter to obtain the extract.

[0025] (3) Purification: The extract was concentrated under reduced pressure to a relative density of 1.10 (25℃), and loaded onto an AB-8 macroporous resin column (column diameter: column height = 1:10). First, it was eluted with 3 column volumes of deionized water at a flow rate of 2.2 BV / h, and then eluted with 4 column volumes of 72% v / v ethanol solution at a flow rate of 1.3 BV / h. The ethanol eluent was collected.

[0026] (4) Alcohol precipitation and freeze drying: The ethanol eluent was concentrated until no alcohol odor was detected, and 4 times the volume of anhydrous ethanol was added. The mixture was refrigerated at 4°C for 14 hours, filtered, and the supernatant was freeze-dried under vacuum to obtain refined Terminalia chebula extract powder. The tannin content was found to be 15.3%, and the chebulic acid content was 4.1%.

[0027] Example 3: Preparation of Edelweiss Extract (1) Raw material pretreatment: 100g of sterile cultured Edelweiss callus was freeze-dried at -48℃ to a moisture content of 4.5%, and then ultra-finely pulverized at 8℃ to a particle size of 15μm. Four times its weight of pretreatment solution (containing 1.0% mannitol, 0.4% EDTA-2Na, pH 5.8) was added to the powder and soaked at 28℃ for 1.5h.

[0028] (2) Extraction: The pretreated mixture was subjected to ultrasonic-microwave synergistic extraction. The ultrasonic power was set to 200W, the microwave frequency to 2450MHz, the microwave power to 320W, the extraction temperature to 42℃, and the extraction time to 50min. After extraction, the mixture was filtered, the filtrate was collected, the residue was washed with a small amount of extraction solvent, the filtrates were combined, concentrated under reduced pressure, and then freeze-dried to obtain Edelweiss extract powder.

[0029] Example 4: Preparation of Agarwood Skincare Products The following raw materials were weighed by weight: 2.0 parts of agarwood extract obtained in Example 1, 0.2 parts of retinol, 0.5 parts of vitamin E, 0.5 parts of tea polyphenols, 0.2 parts of resveratrol, 5.0 parts of boswellia carterii, 1.5 parts of complex polypeptide (palmitoyl pentapeptide-4: palmitoyl tripeptide-1: acetyl hexapeptide-8 = 2:1.5:1), 0.05 parts of ergothioneine, 1.5 parts of ceramide, 3.0 parts of squalane, 2.0 parts of panthenol, 3.0 parts of bifida ferment lysate, 0.3 parts of tea tree oil, 2.0 parts of hyaluronic acid, 0.5 parts of honeysuckle extract, and 0.15 parts of cell activator (Terminalia chebula extract from Example 2: Edelweiss extract from Example 3 = 4:2).

[0030] Preparation method: S1. Raw material pretreatment: Agarwood extract, honeysuckle extract, and 8 times their weight of deionized water were mixed and stirred for 40 minutes at 45°C and 250W with ultrasonic assistance. The mixture was then filtered through a 0.22μm filter membrane to obtain aqueous premix A. Retinol, vitamin E, tea tree oil, and squalane were mixed and heated to 55°C under nitrogen protection and stirred until dissolved to obtain oil phase mixture B.

[0031] S2. Emulsification and Mixing: Hyaluronic acid and panthenol were added to the remaining deionized water and heated to 80°C with stirring to dissolve, forming the aqueous phase C. While stirring at 2500 rpm, the oil phase mixture B was slowly added to the aqueous phase C at a rate of 8 ml / min. After the addition was complete, the system temperature was maintained at 80°C, and shear emulsification was continued at 2500 rpm for 20 minutes. Subsequently, the mixture was homogenized four times under a pressure of 25 MPa to obtain the primary emulsion D.

[0032] S3. Compound Addition and Sterilization: Place the primary emulsion D in a water bath and gradually decrease the temperature by 5°C every 5 minutes until the system temperature reaches 40°C. Under gentle stirring, add Bosein, Bifida ferment lysate, and cell activator sequentially. Then, add palmitoyl pentapeptide-4, acetyl hexapeptide-8, and palmitoyl tripeptide-1 sequentially at 5-minute intervals. Finally, add ergothioneine and ceramide, and continue stirring for 35 minutes to ensure homogeneity. Adjust the pH to 5.8 with lactic acid, filter through a 0.22μm microfiltration membrane for sterilization, and dispense under aseptic conditions to obtain the finished product.

[0033] Example 5: Preparation of Agarwood Skincare Products The preparation method is the same as in Example 4. The formula is as follows: 0.5 parts of agarwood extract, 0.1 parts of retinol, 0.2 parts of vitamin E, 0.1 parts of tea polyphenols, 0.05 parts of resveratrol, 3.0 parts of boswellia carterii, 0.5 parts of complex polypeptide, 0.01 parts of ergothioneine, 0.5 parts of ceramide, 1.0 part of squalane, 1.0 part of panthenol, 1.0 part of Bifida ferment lysate, 0.1 parts of tea tree oil, 1.0 part of hyaluronic acid, 0.3 parts of honeysuckle extract, and 0.08 parts of cell activator (Example 2 Terminalia chebula extract: Example 3 Edelweiss extract = 3:2).

[0034] Example 6: Preparation of Agarwood Skincare Products The preparation method is the same as in Example 4. The formula is as follows: 3.0 parts of agarwood extract, 0.3 parts of retinol, 0.8 parts of vitamin E, 1.0 part of tea polyphenols, 0.3 parts of resveratrol, 8.0 parts of boswellia carterii, 3.0 parts of complex polypeptide, 0.1 parts of ergothioneine, 2.0 parts of ceramide, 5.0 parts of squalane, 3.0 parts of panthenol, 5.0 parts of Bifida ferment lysate, 0.5 parts of tea tree oil, 3.0 parts of hyaluronic acid, 1.0 part of honeysuckle extract, and 0.25 parts of cell activator (Example 2 Terminalia chebula extract: Example 3 Edelweiss extract = 5:2).

[0035] Comparative Example 1 The difference between this comparative example and Example 4 is that no agarwood extract was added to the composition, while the other raw materials and preparation process are exactly the same as in Example 4.

[0036] Comparative Example 2 The difference between this comparative example and Example 4 is that the complex polypeptide is replaced with an equal weight of deionized water, while the other raw materials and preparation process are exactly the same as in Example 4.

[0037] Comparative Example 3 The difference between this comparative example and Example 4 is that no cell activator was added to the composition, while the other raw materials and preparation process are exactly the same as in Example 4.

[0038] Comparative Example 4 The difference between this comparative example and Example 4 is that the conventional high-temperature emulsification process was used in the preparation process: the oil phase mixture and the water phase were heated to 80°C respectively, mixed and then homogenized and emulsified at 80°C for 5 minutes, and then all the remaining active ingredients were added at a temperature above 50°C, stirred and cooled to room temperature.

[0039] Performance testing 1. Antibacterial activity test 1.1 Test strains: Staphylococcus aureus (ATCC 6538), Escherichia coli (ATCC 25922), and Propionibacterium acnes (ATCC 6919) were selected as test strains and cultured on nutrient agar medium to the logarithmic growth phase.

[0040] 1.2 Test Method: The micro-broth dilution method was used. Samples from Examples 4-6 and Comparative Examples 1-4 were diluted with sterile PBS to a series of concentrations (0.125-16 mg / mL). Inoculation solution (1×10⁻⁶) was then used. 6 After incubating at 37°C for 24 hours (CFU / mL), the minimum inhibitory concentration (MIC) was determined.

[0041] 1.3 Evaluation criteria: MIC≤2mg / mL indicates strong antibacterial activity; 2mg / mL<MIC≤8mg / mL indicates moderate antibacterial activity; 8mg / mL<MIC≤16mg / mL indicates weak antibacterial activity; MIC>16mg / mL indicates no antibacterial activity.

[0042] 2. Moisturizing performance test 2.1 Test Samples: Prepare a 5% aqueous solution of the sample, with deionized water as a blank control.

[0043] 2.2 Test method: The gravimetric method was used. The sample solution (2.0g) was placed in a petri dish and placed at a temperature of 25±1℃ and a relative humidity of 43±2% for 0h, 2h, 4h, 8h and 24h. The change in sample mass was measured and the moisture retention rate was calculated.

[0044] Moisture retention rate (%) = (Sample mass after placement / Initial sample mass) × 100% 2.3 Evaluation criteria: 24h moisturizing rate ≥80% is excellent; 60% ≤ 24h moisturizing rate <80% is good; 40% ≤ 24h moisturizing rate <60% is average; 24h moisturizing rate <40% is poor.

[0045] 3. Testing of indicators related to firming and repair 3.1 Collagen Synthesis Promotion Test 3.1.1 Cell model: Human dermal fibroblasts (HDF) were cultured in DMEM medium containing 10% fetal bovine serum.

[0046] 3.1.2 Test method: The sample was diluted to 100 μg / mL with culture medium and treated with HDF cells for 48 h. The content of type I collagen (COL-I) in the cell supernatant was detected by ELISA kit. The relative synthesis rate was calculated with blank culture medium as a control.

[0047] Relative synthesis rate (%) = (COL-I content in sample group / COL-I content in control group) × 100% 3.1.3 Evaluation criteria: A relative synthesis rate ≥ 150% is considered a significant promoter; 120% ≤ relative synthesis rate < 150% is considered a moderate promoter; 100% ≤ relative synthesis rate < 120% is considered a slight promoter; and a relative synthesis rate < 100% is considered a no promoter.

[0048] 3.2 Hyaluronic Acid Synthesis Promotion Test 3.2.1 Test method: Using the HDF cell model in 3.1.1, after the samples were treated for 48 hours, the hyaluronic acid (HA) content in the cell supernatant was determined using a hyaluronic acid detection kit, and the relative synthesis rate was calculated.

[0049] 3.2.2 Evaluation criteria: A relative synthesis rate ≥ 140% is considered a significant promoter; 110% ≤ relative synthesis rate < 140% is considered a moderate promoter; 100% ≤ relative synthesis rate < 110% is considered a slight promoter; and a relative synthesis rate < 100% is considered a no promoter.

[0050] 3.3 Antioxidant Activity Test 3.3.1 Test method: The sample was prepared into a series of concentrations (10-200 μg / mL) with anhydrous ethanol, and mixed with an equal volume of 0.1 mmol / L DPPH ethanol solution. The mixture was reacted at 37℃ in the dark for 30 min, and the absorbance at 517 nm was measured to calculate the free radical scavenging rate.

[0051] Clearance rate (%) = [1 - (sample absorbance - blank absorbance) / control group absorbance] × 100% 3.3.2 Evaluation Criteria: IC 50 (IC50) ≤ 50 μg / mL indicates strong antioxidant; 50 μg / mL < IC50 indicates strong antioxidant. 50 ≤100μg / mL is considered moderate antioxidant; IC50 50 >100μg / mL indicates weak antioxidant activity.

[0052] 4. Test Results 4.1 Results of antibacterial activity test Table 1. Minimum inhibitory concentrations (MIC, mg / mL) of different samples against the test strains

[0053] 4.2 Moisturizing performance test results Table 2. 24-hour humidification rate and evaluation of different samples

[0054] 4.3 Test Results of Tightening and Repair Related Indicators Table 3. Test results of firming and repair-related indicators for different samples

[0055] in conclusion: This invention, through comparative experiments of examples and comparative examples, verifies the decisive role of key components and preparation processes in the core efficacy of agarwood skincare products. Specific conclusions are as follows: 1. Antibacterial Activity: The MIC values ​​of Examples 4-6 against Staphylococcus aureus, Escherichia coli, and Propionibacterium acnes were 1.0-2.0 mg / mL, 1.5-2.5 mg / mL, and 0.8-1.2 mg / mL, respectively, all meeting the standard for potent antibacterial activity. However, Comparative Example 1, without the addition of agarwood extract, had MIC values ​​>16 mg / mL, showing no antibacterial activity. This demonstrates that agarwood extract can enhance the binding efficiency of other antibacterial components by regulating the permeability of bacterial cell membranes. Comparative Example 2 showed a MIC value of 8.0-10.0 mg / mL, indicating that the complex peptide not only has a firming effect but also reduces bacterial adhesion sites by regulating the metabolism of the stratum corneum, forming a synergistic effect with antibacterial components such as agarwood extract. Comparative Example 3 had a MIC value of 3.0-5.0 mg / mL, indicating that cell activators can enhance the antibacterial effect by promoting the synergistic effect of active ingredients, while Edelweiss extract indirectly improves the balance of the bacterial flora by soothing skin inflammation. Comparative Example 4... The MIC value is 4.5-8.0 mg / mL, indicating that the process design of low-temperature addition, gradient cooling and nitrogen protection can effectively preserve the activity of antibacterial components and ensure the long-lasting antibacterial effect.

[0056] 2. Moisturizing performance: The 24-hour moisturizing rate of Examples 4-6 was 82.3%-88.2%, all of which were rated as excellent. This is mainly due to the high molecular weight hyaluronic acid forming a water-locking film on the skin surface, the medium molecular weight filling the gaps in the stratum corneum, and the small molecular weight penetrating deep to replenish moisture. The polysaccharide components in the agarwood extract can enhance the hydrogen bonding force between water and the stratum corneum, thus prolonging the moisturizing effect. The moisturizing rate of Comparative Example 1 was only 52.8% (medium), indicating that the agarwood extract enhances the water-locking ability through the synergistic effect with hyaluronic acid and ceramide. After Comparative Examples 2 and 3 were deprived of the complex peptide and cell activator, respectively, the moisturizing rate decreased to 65.4%-72.1% (good), confirming that the complex peptide can promote the synthesis of the skin's own moisturizing factors, while the cell activator enhances the skin's moisture storage capacity by activating the metabolism of stratum corneum cells; this is lower than that of Example 4, verifying the importance of the cell activator in maintaining the integrity of the skin barrier; Comparative Example 4 had a lower moisturizing rate than Example 4 due to the degradation of hyaluronic acid and polymerization of ceramide caused by high-temperature emulsification and non-gradient cooling, proving that the emulsification homogenization process of the present invention can ensure the uniform dispersion of moisturizing ingredients, while gradient cooling avoids the destruction of the component structure and ensures long-lasting moisturizing performance.

[0057] 3. Firming and Repairing Efficacy: The relative synthesis rates of COL-I in Examples 4-6 were 158.9%-178.6%, HA was 148.2%-163.4%, and DPPH free radical scavenging IC 5032.2-42.7 μg / mL; Comparative Example 1 showed a COL-I synthesis rate of only 105.2%, a HA synthesis rate of 108.3%, and a 66.3% decrease in antioxidant capacity, confirming that agarwood extract exerts its core repair role by activating fibroblast activity and can provide a suitable cellular microenvironment for HA synthesis through anti-inflammatory repair effects. Comparative Example 2 showed a COL-I synthesis rate of 112.5%, indicating that the complex peptide is a key synergistic component in promoting collagen production; Comparative Example 3 showed IC 50 The concentration of COL-I and HA decreased when the concentration was increased to 58.9 μg / mL, indicating that the cell activator can enhance the metabolic activity of fibroblasts, improve the activity of the antioxidant system, and enhance the repair efficacy by activating autophagy. Comparative Example 4 showed a decrease in the relative synthesis rates of COL-I and HA compared to Example 4, with an IC50 concentration of 58.9 μg / mL. 50 The increase indicates that the process design of this invention, which involves gradient cooling, sequential addition of peptides, and nitrogen protection, can prevent the active ingredients from becoming ineffective and ensure the stability of the firming and repairing effects.

[0058] In summary, this invention achieves synergistic effects of antibacterial, moisturizing, and repairing efficacy by scientifically compounding core ingredients such as agarwood extract, complex peptides, and cell activators, and combining them with an ultrasonic-assisted extraction process, thus verifying the scientific nature of the formula design and the necessity of process optimization.

[0059] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A composition with firming, repairing, antibacterial, and moisturizing properties, characterized in that, The product contains the following ingredients in parts by weight: 0.5-3.0 parts agarwood extract, 0.1-0.3 parts retinol, 0.2-0.8 parts vitamin E, 0.1-1.0 parts tea polyphenols, 0.05-0.3 parts resveratrol, 3.0-8.0 parts boswellia carterii, 0.5-3.0 parts complex polypeptides, 0.01-0.1 parts ergothioneine, 0.5-2.0 parts ceramides, 1.0-5.0 parts squalane, 1.0-3.0 parts panthenol, 1.0-5.0 parts bifida ferment lysate, 0.1-0.5 parts tea tree oil, 1.0-3.0 parts hyaluronic acid, 0.3-1.0 parts honeysuckle extract, and 0.08-0.25 parts cell activator.

2. The composition according to claim 1, characterized in that, The ingredients include the following parts by weight: 2.0 parts agarwood extract, 0.2 parts retinol, 0.5 parts vitamin E, 0.5 parts tea polyphenols, 0.2 parts resveratrol, 5.0 parts boswellia carterii, 1.5 parts complex polypeptide, 0.05 parts ergothioneine, 1.5 parts ceramide, 3.0 parts squalane, 2.0 parts panthenol, 3.0 parts bifida ferment lysate, 0.3 parts tea tree oil, 2.0 parts hyaluronic acid, 0.5 parts honeysuckle extract, and 0.15 parts cell activator.

3. The composition according to claim 1, characterized in that, The complex polypeptide consists of palmitoyl pentapeptide-4, palmitoyl tripeptide-1, and acetyl hexapeptide-8 in a weight ratio of (1-3):(1-2):(0.5-1.5).

4. The agarwood skincare product as described in claim 1, characterized in that, The extraction method of the agarwood extract includes the following steps: (1) Supercritical CO2 extraction: The agarwood raw material is crushed and extracted with supercritical CO2 at an extraction pressure of 25-35 MPa and a temperature of 45-55℃ to obtain agarwood essential oil. (2) Ultrasonic-assisted extraction: The agarwood raw material residue after extraction in step (1) is mixed with 60-75% v / v ethanol aqueous solution at a mass-volume ratio of 1g: 8-12mL, and extracted for 1-2 hours at 40-50℃ and ultrasonic power of 200-400W. After filtration, extract A is obtained. (3) Hot water extraction: Mix the residue after extraction in step (2) with deionized water at a ratio of 1:10-15, extract at 85-95℃ for 2-3 hours, filter, and obtain extract B; (4) Combining: The agarwood essential oil obtained in step (1), the extract A in step (2) and the extract B in step (3) are combined in a weight ratio of (0.5-2):(2-5):(3-6) and concentrated to a preset concentration to obtain the agarwood extract.

5. The agarwood skincare product as described in claim 1, characterized in that, The cell activator is a Terminalia chebula extract and an Edelweiss extract in a weight ratio of (3-5):

2.

6. The composition according to claim 5, characterized in that, The extraction method of the Terminalia chebula extract includes the following steps: (1) Enzymatic hydrolysis pretreatment: Take the dried fruit of Terminalia chebula, remove the pit and crush it, add 8-12 times the weight of the raw material of deionized water and adjust the pH to 5.0-5.5, add 0.2-0.3% of the weight of the raw material of compound enzyme and hydrolyze at 50-55℃ for 1.5-2.0h, inactivate and dry to obtain pretreated powder. The compound enzyme is cellulase and xylanase with a mass ratio of 1.3-2.5:

1. (2) Ultrasonic-microwave synergistic extraction: Add 10-12 times the weight of 60-65% v / v ethanol solution to the pretreated powder, and add 0.1-0.15% sodium bisulfite by weight of the raw material. First, extract with ultrasonic assistance at 45-50℃ for 30-40 min, and then extract with microwave at 55-60℃ and 300-350W for 20-25 min. Filter to obtain the extract. (3) Purification: After concentrating the extract, the sample is loaded onto a macroporous resin column and eluted sequentially with water and 70-75% v / v ethanol solution. The ethanol eluent is collected. (4) Alcohol precipitation and freeze drying: After concentrating the ethanol eluent and precipitating it with alcohol, the supernatant was taken and freeze-dried under vacuum to obtain the refined Terminalia chebula extract.

7. The composition according to claim 5, characterized in that, The extraction method of the alpine edelweiss extract includes the following steps: (1) Raw material pretreatment: Take sterile cultured Edelweiss callus tissue, freeze dry it under vacuum at -50 to -45℃ until the moisture content is ≤5%, and use low temperature ultrafine grinding to a particle size of 10-20μm. Add 3-5 times its mass of pretreatment solution to the sieved powder and soak it at a constant temperature of 25-30℃ for 1-2h. The pretreatment solution consists of 0.8-1.2% mannitol, 0.3-0.5% EDTA-2Na and the remainder deionized water, and the pH value of the pretreatment solution is adjusted to 5.5-6.

0. (2) Extraction: Ultrasonic-microwave combined extraction was adopted, with ultrasonic power of 180-220W, microwave frequency of 2450MHz, microwave power of 300-350W, extraction temperature of 40-45℃, and extraction time of 40-60min.

8. The method for preparing the agarwood skincare product according to any one of claims 1-7, characterized in that, Includes the following steps: S1 Raw Material Pretreatment: Mix agarwood extract, honeysuckle extract and 5-10 times the weight of deionized water, stir at 40-50℃ for 30-45 minutes, filter through a 0.22μm filter membrane and set aside; mix retinol, vitamin E, tea tree oil and squalane, heat to 50-60℃ under nitrogen protection to form an oil phase mixture; S2 Emulsification Mixing: Dissolve hyaluronic acid and panthenol in deionized water to form an aqueous phase. Stir at 75-85℃ until completely dissolved. Then add the oil phase mixture to the aqueous phase at a rate of 5-10 ml / min, while shearing and emulsifying at 2000-3000 r / min for 15-25 minutes. S3 compound addition and sterilization: After the temperature of the emulsification system drops to 40-45℃, add Bosein, compound polypeptide, Bifida ferment lysate and cell activator in sequence. Stir for 30-40 minutes, then filter and sterilize using a 0.22μm microfiltration membrane. Dispense under aseptic conditions to obtain the product.

9. The method for preparing the agarwood skincare product as described in claim 8, characterized in that, The mixture of agarwood extract and honeysuckle extract in S1 is extracted with ultrasonic assistance during the stirring process. The ultrasonic power is 200-300W and the frequency is 25-40kHz. The shear temperature during the emulsification stage in S2 is controlled at 78-82℃. After emulsification, 3-5 cycles of homogenization are performed, with a homogenization pressure of 20-30MPa. When adding the active ingredients in S3, a gradient cooling method is used, reducing the temperature by 5°C every 5 minutes until it reaches 40°C. The compound peptides are added in the following order: palmitoyl pentapeptide-4, acetyl hexapeptide-8, and tripeptide-1 copper, with a 5-minute interval between each peptide addition.

10. An agarwood skincare product with firming, repairing, antibacterial, and moisturizing properties, characterized in that: The product dosage form of the agarwood skin care product comprising any one of claims 1-7 is a lotion, cream or serum.

Images