Anti-aging emulsion for relieving retinol irritation, preparation method and application thereof

Abstract

The present application belongs to the technical field of cosmetics, and particularly relates to an anti-aging emulsion for relieving retinol irritation and a preparation method and application thereof. Specifically, the emulsion is prepared by taking Icelandic lichen extract, sodium hyaluronate (400Da-3KDa), sodium hyaluronate (1W-3W Da), polyamide-8 (and) pentaerythritol tetra (bis-tert-butyl hydroxyl hydrogenated cinnamic acid) ester and retinol as main components. It is verified by experiments that the prepared anti-aging emulsion has the effects of significantly repairing damaged skin barrier and improving skin hydration, does not affect the anti-aging effect of retinol, can be used for relieving the irritation of retinol, and the organic combination of retinol and the above-mentioned raw materials can obviously improve the color change problem of retinol, so that the anti-aging emulsion has good practical application value.

Description

Technical Field

[0001] This invention belongs to the field of cosmetic technology, specifically relating to an anti-aging lotion that alleviates the irritation of retinol, its preparation method, and its application. Background Technology

[0002] The information disclosed in this background section is intended only to enhance understanding of the overall background of the invention and is not necessarily to be construed as an admission or in any way implying that such information constitutes prior art known to those skilled in the art.

[0003] In recent years, with the booming development of the "appearance economy," products related to "anti-aging" and "anti-photoaging" have received increasing attention from consumers. Retinol and its derivatives are recognized as anti-wrinkle and anti-aging active ingredients and are widely used in cosmetics. However, using products containing retinol and its derivatives can cause a series of hypersensitivity reactions. Both natural and synthetic retinol are agonists of the transient receptor potential channel vanillic acid subtype 1 (TRPV1) receptor, which can excite nociceptive sensory neurons and induce hypersensitivity reactions. Another effect of retinol and its derivatives on the skin is that they can cause dryness and peeling. In most cases, retinol is converted into retinoic acid to act on the skin. All-trans retinoic acid can increase the overexpression of aquaporin 3 (AQP3) in normal human skin, thereby increasing transepidermal water loss (TEWL) values, causing dry skin, and leading to damage to the skin barrier. At the same time, the phototoxic substances produced by the decomposition of retinol under ultraviolet radiation can also cause strong irritation, leading to damage to the skin barrier.

[0004] Currently, the development and design of retinol products often mitigates retinol's irritation by adding soothing and moisturizing ingredients. However, the inventors have discovered that many consumers with sensitive skin still experience stinging, redness, burning, and dryness after applying skincare products containing these substances. Furthermore, the instability of retinol limits its application in cosmetics. Retinol has five double bonds, making it chemically reactive and easily oxidized and degraded by factors such as oxygen and temperature. Oxidative degradation results in the loss of biological activity and discoloration. Therefore, while ensuring the efficacy of retinol, mitigating its irritation and improving the stability of retinol products have been a long-standing technical challenge for researchers in this field. Summary of the Invention

[0005] To address the shortcomings of existing technologies, the present invention aims to provide an anti-aging emulsion that alleviates retinol irritation, along with its preparation method and applications. Specifically, the present invention prepares an emulsion using Icelandic lichen extract, sodium hyaluronate (400 Da–3 kDa), sodium hyaluronate (1 W–3 W Da), polyamide-8 (and) pentaerythritol tetra(bis-tert-butylhydroxyhydrocinnamic acid) ester, and retinol as the main components. Experimental verification has shown that the prepared anti-aging emulsion significantly repairs damaged skin barriers and enhances skin hydration, while not affecting the anti-aging efficacy of retinol. It can be used to alleviate the irritation problem of retinol. Furthermore, the combination of retinol with Icelandic lichen extract, sodium hyaluronate (400 Da–3 kDa), sodium hyaluronate (1 W–3 W Da), polyamide-8 (and) pentaerythritol tetra(bis-tert-butylhydroxyhydrocinnamic acid) ester can significantly improve the color change problem of retinol. Based on the above research results, the present invention is thus completed.

[0006] To achieve the above-mentioned technical objectives, the present invention provides the following technical solution:

[0007] In a first aspect, the present invention provides an anti-aging emulsion that alleviates the irritation of retinol, said anti-aging emulsion comprising at least the following components in parts by weight:

[0008] Icelandic lichen extract 2-15 parts, sodium hyaluronate (400 Da~3 KDa) 0.01-0.1 parts, sodium hyaluronate (1 W~3 W Da) 0.05-0.5 parts, polyamide-8 (and) pentaerythritol tetra(bis-tert-butylhydroxyhydrocinnamic acid) ester 0.1-0.6 parts and retinol 0.01-0.1 parts.

[0009] Furthermore, the polyamide-8 (and) pentaerythritol tetra(bis-tert-butylhydroxyhydrogenated cinnamic acid) ester is a composition of polyamide-8 and pentaerythritol tetra(bis-tert-butylhydroxyhydrogenated cinnamic acid) ester, with a mass ratio of 0.1-1:99-99.9.

[0010] Furthermore, the anti-aging emulsion also contains commonly used cosmetic excipients in emulsions, such as emulsifiers, oils, polyols, thickeners, preservatives, chelating agents, and solvents (such as water), etc., which are not specifically limited here.

[0011] A second aspect of the present invention provides a method for preparing the above-mentioned anti-aging emulsion that alleviates the irritation of retinol, the method comprising:

[0012] S1. Preparation of aqueous phase: Sodium hyaluronate (400 Da ~ 3 K Da), sodium hyaluronate (1 W ~ 3 W Da) and water are mixed and heated to 80-90℃ and stirred to dissolve;

[0013] S2. Preparation of the oil phase: Polyamide-8 (and) pentaerythritol tetra(bis-tert-butylhydroxyhydrocinnamic acid) ester is heated to 70-90℃ to melt;

[0014] S3. Homogenize the aqueous and oil phases together; after cooling, add Icelandic lichen extract and retinol.

[0015] A third aspect of the present invention provides the application of the above-described anti-aging emulsion in the preparation of cosmetics.

[0016] A fourth aspect of the present invention provides a cosmetic product comprising at least the aforementioned anti-aging lotion. The cosmetic product is a skincare product. Experiments have demonstrated that the cosmetic product prepared according to the present invention can significantly delay the retinol color change problem, and in terms of efficacy, it can significantly reduce TEWL values, increase the moisture content of the stratum corneum, and has significant anti-aging effects, while effectively improving the irritation problems associated with using retinol.

[0017] The beneficial technical effects of one or more of the above technical solutions are as follows:

[0018] (1) Due to the structural problems of retinol, it is easily oxidized and degraded by temperature and oxygen. After degradation, it changes color and loses its biological activity. The anti-aging emulsion prepared by this invention with Icelandic lichen extract, sodium hyaluronate (400 Da ~ 3 K Da), sodium hyaluronate (1 W ~ 3 W Da), polyamide-8 (and) pentaerythritol tetra(bis-tert-butylhydroxyhydrocinnamic acid) ester and retinol as the main active ingredients can significantly prolong the color change time of retinol and greatly improve the stability of the product.

[0019] (2) Experimental results show that Icelandic lichen extract ① has better skin care effects than Icelandic lichen extract ② and Icelandic lichen extract ③, thus making the product more effective.

[0020] (3) Experimental verification shows that the anti-aging emulsion prepared by this invention can significantly reduce TEWL value, increase the moisture content of the stratum corneum of the skin, and alleviate barrier damage and reduced skin water retention caused by retinol.

[0021] (4) The preparation method of the anti-aging emulsion that alleviates the irritation of retinol obtained by the above technical solution is simple and easy to implement, saves costs, and the raw materials are easy to obtain. It is suitable for mass production. Through human efficacy test, the anti-aging effect is comparable to that of emulsion containing only retinol. Therefore, it has good practical application value. Detailed Implementation

[0022] It should be noted that the following detailed description is illustrative and intended to provide further explanation of the invention. Unless otherwise specified, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains.

[0023] It should be noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the exemplary embodiments according to this application. As used herein, the singular form is intended to include the plural form as well, unless the context clearly indicates otherwise. Furthermore, it should be understood that when the terms "comprising" and / or "including" are used in this specification, they indicate the presence of features, steps, operations, devices, components, and / or combinations thereof.

[0024] In a typical embodiment of the present invention, an anti-aging emulsion for alleviating the irritation of retinol is provided, the anti-aging emulsion comprising at least the following components in parts by weight:

[0025] Icelandic lichen extract 2-15 parts, sodium hyaluronate (400 Da~3 KDa) 0.01-0.1 parts, sodium hyaluronate (1 W~3 W Da) 0.05-0.5 parts, polyamide-8 (and) pentaerythritol tetra(bis-tert-butylhydroxyhydrocinnamic acid) ester 0.1-0.6 parts and retinol 0.01-0.1 parts.

[0026] Furthermore, the polyamide-8 (and) pentaerythritol tetra(bis-tert-butylhydroxyhydrogenated cinnamic acid) ester is a composition of polyamide-8 and pentaerythritol tetra(bis-tert-butylhydroxyhydrogenated cinnamic acid) ester, with a mass ratio of 0.1-1:99-99.9.

[0027] Furthermore, the anti-aging emulsion also contains commonly used cosmetic excipients in emulsions, such as emulsifiers (further, such as polyglycerol-6 stearate, polyglycerol-6 behenate), oils (further, such as squalane, isononyl isononanoate), polyols (further, such as dipropylene glycol, butylene glycol), thickeners (further, such as carbomer, xanthan gum), preservatives (further, such as 1,2-hexanediol, p-hydroxyacetophenone), chelating agents (further, such as EDTA-2Na), pH adjusters (further, such as tromethamine), and solvents (such as water), etc., without specific limitations.

[0028] The extraction and preparation method of the Icelandic lichen extract can be any one or more of the following, with method one being preferred.

[0029] Method 1:

[0030] (1) Preparation of eutectic solvent DES: The hydrogen bond acceptor (HBA) is choline chloride and the hydrogen bond donor (HBD) is glycerol. HBA and HBD are mixed in a molar ratio of 1:1-3, stirred and heated to 70-90℃ and maintained for 1-2 hours until a clear and uniform transparent liquid is formed. Then water is added to it and stirred to obtain the eutectic solvent.

[0031] (2) Icelandic lichen powder was added to the DES prepared in step (1) for ultrasonic extraction. After filtration and concentration, 1 to 1.2 times the mass of the concentrate was added to the extract and stirred until homogeneous. After filtration, Icelandic lichen extract ① was obtained. The concentration was 0.15 to 0.20 g / g based on the amount of crude drug.

[0032] In step (1), the molar ratio of HBA to HBD is preferably 1:2;

[0033] The volume fraction of water added is 10-50% (preferably 30%, v / v) of the transparent liquid.

[0034] In step (2), the Icelandic lichen powder is prepared by washing, drying, crushing, and passing the Icelandic lichen through a 60-100 mesh sieve.

[0035] The mass ratio of Icelandic lichen powder to DES liquid is 1:10-30, preferably 1:20 (w / w).

[0036] The specific conditions for ultrasonic extraction are as follows: ultrasonic extraction at 30-50℃ (preferably 40℃) for 10-50 min (preferably 40 min), with ultrasonic power set at 200-300W and ultrasonic frequency at 30-50KHz.

[0037] The concentration is a vacuum concentration, specifically carried out at 50-60℃; the volume of the resulting concentrated liquid is 1 / 3 to 1 / 8 of the volume before concentration.

[0038] Method 2:

[0039] (1) Add Icelandic lichen powder to ethanol solution, with a material-to-liquid mass ratio of 1:15-1:20, adjust pH to acidic, add cellulase for enzymatic hydrolysis by heating, and perform ultrasonic extraction after enzymatic hydrolysis. After ultrasonic extraction, filter to obtain filtrate.

[0040] (2) Concentrate the filtrate obtained in step (1) until the filtrate has no alcohol odor, add 1 to 1.2 times the mass of the concentrate with glycerol, stir and mix evenly, and filter to obtain Icelandic lichen extract ②. The concentration is 0.15 to 0.20 g / g based on the crude drug weight.

[0041] In step (1), the Icelandic lichen powder is prepared by washing, drying, pulverizing, and passing the Icelandic lichen through a 60-100 mesh sieve. The ethanol is high-concentration ethanol, with an ethanol solution concentration of 70% or higher, preferably 85%; the pH is 4.0-6.0 (preferably 5.0); the specific conditions for heating and enzymatic hydrolysis are: adding cellulase at a mass fraction of 0.1-1% (preferably 0.4%), at 40-60℃ (preferably 50℃), and hydrolyzing for 1-5 hours (preferably 2 hours); the ultrasonic extraction conditions are: ultrasonic extraction for 10-60 minutes (preferably 30 minutes), with an ultrasonic power of 100-1000W (preferably 500W) and an ultrasonic frequency of 10-50KHz (preferably 30KHz).

[0042] In step (2), the concentration is vacuum concentration, specifically carried out at 50-60°C.

[0043] Method 3:

[0044] (1) Add Icelandic lichen powder to ethanol solution, with a material-to-liquid mass ratio of 1:8-1:12, and perform ultrasonic extraction. After ultrasonic extraction, filter to obtain filtrate.

[0045] (2) Concentrate the filtrate obtained in step (1) until the filtrate has no alcohol odor, add 1 to 1.2 times the mass of the concentrate of glycerol, stir and mix evenly, and filter to obtain Icelandic lichen extract ③. The concentration is 0.15 to 0.20 g / g based on the amount of crude drug.

[0046] In step (1), the Icelandic lichen powder is prepared by washing, drying, pulverizing, and passing the Icelandic lichen through a 60-100 mesh sieve. The concentration of the ethanol solution is 40%-60%. The specific method of ultrasonic extraction includes: ultrasonic extraction for 10-60 minutes, ultrasonic power of 100-1000W, ultrasonic frequency of 10-50KHz, repeated extraction 2-3 times, and after ultrasonic extraction, the extracts are combined and filtered.

[0047] In step (2), the concentration is vacuum concentration, specifically carried out at 50-60°C.

[0048] In another specific embodiment of the present invention, a method for preparing the above-mentioned anti-aging emulsion that alleviates the irritation of retinol is provided, the preparation method comprising:

[0049] S1. Preparation of aqueous phase: Sodium hyaluronate (400 Da ~ 3 K Da), sodium hyaluronate (1 W ~ 3 W Da) and water are mixed and heated to 80-90℃ and stirred to dissolve;

[0050] S2. Preparation of the oil phase: Polyamide-8 (and) pentaerythritol tetra(bis-tert-butylhydroxyhydrocinnamic acid) ester is heated to 70-90℃ to melt;

[0051] S3. Homogenize the aqueous and oil phases together; after cooling, add Icelandic lichen extract and retinol.

[0052] Furthermore, the aqueous phase in step S1 may also include polyols (such as dipropylene glycol, butanediol), thickeners (such as carbomer, xanthan gum), and chelating agents (such as EDTA-2Na).

[0053] The oil phase in step S2 may also include emulsifiers (such as polyglycerol-6 stearate, polyglycerol-6 behenate) and oils (such as squalane, isononyl isononanoate).

[0054] In step S3, the specific conditions for homogenization are: homogenization at 2000-5000 rpm for 5-20 minutes.

[0055] Furthermore, the preparation method further includes:

[0056] S4. When the temperature drops to 75℃, add a pH adjuster (such as tromethamine), stir to dissolve, and continue to cool after stirring evenly.

[0057] S5. When the temperature drops to 65-70℃, add the preservative (such as 1,2-hexanediol, p-hydroxyacetophenone), stir to dissolve, and continue to cool down after dissolution.

[0058] S6. When the temperature drops to 45℃, add Icelandic lichen extract and other raw materials (such as dipotassium glycyrrhizate) in sequence, stir to dissolve and disperse evenly, and continue to cool down;

[0059] S7: When the temperature drops below 40℃, add retinol, stir to dissolve and disperse evenly, and you have the product.

[0060] In another specific embodiment of the present invention, the application of the above-mentioned anti-aging emulsion in the preparation of cosmetics is provided.

[0061] In another specific embodiment of the present invention, a cosmetic product is provided, which at least comprises the aforementioned anti-aging lotion. The cosmetic product is a skincare product. Experiments have shown that the cosmetic product prepared by the present invention can significantly delay the retinol color change problem, and in terms of efficacy, it can significantly reduce the TEWL value, increase the moisture content of the stratum corneum, and has significant anti-aging effects. Furthermore, it can effectively improve the irritation problem caused by using retinol.

[0062] The present invention will be further described below with reference to embodiments. The present invention is further illustrated by means of embodiments, but this does not limit the present invention to the scope of the embodiments described. Based on the embodiments of the present invention, any changes to the present invention by those skilled in the art without inventive step are within the protection scope of the present invention. Furthermore, in the embodiments of the present invention, unless otherwise specified, all raw materials used in the preparation are commercially available products well known to those skilled in the art.

[0063] Examples 1-3 and Comparative Examples 1-5:

[0064] The specific plan is shown in Table 1 below, calculated in parts by weight.

[0065] In the embodiments and comparative examples of the present invention, the mass ratio of polyamide-8 to pentaerythritol tetra(bis-tert-butylhydroxyhydrogenated cinnamic acid) ester in polyamide-8 (and) pentaerythritol tetra(bis-tert-butylhydroxyhydrogenated cinnamic acid) ester is 99.5:0.5; and the mass ratio of polyglycerol-6 stearate to polyglycerol-6 behenate is 9:1.

[0066] Icelandic lichen extract ①, Icelandic lichen extract ②, and Icelandic lichen extract ③ in the embodiments and comparative examples of this invention were obtained using the following methods:

[0067] The Icelandic lichen extract ① was prepared using the following method:

[0068] (1) Preparation of eutectic solvent DES: The hydrogen bond acceptor (HBA) is choline chloride and the hydrogen bond donor (HBD) is glycerol. HBA and HBD are mixed in a 1:2 molar ratio. The solvent is heated to 80°C using a magnetic stirrer and stirred for 1.5 h until a clear and uniform transparent liquid is formed. 30% (V / V) distilled water is added to the mixture and stirred to obtain the eutectic solvent.

[0069] (2) Icelandic lichen was washed, dried, pulverized, and passed through a 60-mesh sieve. A certain mass of Icelandic lichen powder was accurately weighed, and DES was added at a material-to-liquid mass ratio of 1:20. The mixture was ultrasonically extracted at 40℃ for 40 min with an ultrasonic power of 300W and an ultrasonic frequency of 40KHz. After filtration, the extract was concentrated under reduced pressure at 55℃ to about 1 / 5 of its original volume. Glycerin of 1.1 times its mass was added to the concentrate, and the mixture was stirred and mixed evenly. After filtration, Icelandic lichen extract ① was obtained. The concentration, based on the crude drug weight, was 0.1579 g / g.

[0070] The Icelandic lichen extract ② was prepared using the following method:

[0071] (1) Icelandic lichen was washed, dried, crushed, and passed through a 60-mesh sieve. A certain mass of Icelandic lichen powder was accurately weighed and added to an 85% ethanol solution at a material-to-liquid mass ratio of 1:15. The pH was adjusted to 5.0, and 0.4% cellulase (10000U / g) of the total mass of the ethanol solution was added. The mixture was enzymatically hydrolyzed in a 50℃ water bath for 2 hours. After the enzymatic hydrolysis was completed, ultrasonic extraction was performed for 30 minutes at a power of 500W and a frequency of 30KHz. The mixture was then filtered after ultrasonic extraction.

[0072] (2) The filtrate obtained in step (1) was concentrated under reduced pressure at 55°C until the filtrate had no alcohol odor. Glycerin with a mass of 1.12 times that of the concentrate was added, and the mixture was stirred and mixed evenly. After filtration, Icelandic lichen extract ② was obtained. The concentration was 0.1587 g / g based on the amount of crude drug.

[0073] The Icelandic lichen extract ③ was prepared using the following method:

[0074] (1) Wash, dry, crush and pass Icelandic lichen through a 60-mesh sieve. Accurately weigh a certain amount of Icelandic lichen powder, add 55% ethanol solution, the material-to-liquid mass ratio is 1:10, ultrasonically extract for 30 min, ultrasonic power is 500W, ultrasonic frequency is 30KHz, repeat the extraction twice, after ultrasonic extraction, combine the extracts and filter.

[0075] (2) The filtrate obtained in step (1) was concentrated under reduced pressure at 55°C until the filtrate had no alcohol odor. Glycerin of 1.1 times the mass of the concentrate was added, and the mixture was stirred and mixed evenly. After filtration, Icelandic lichen extract ③ was obtained. The concentration was 0.1592 g / g based on the amount of crude drug.

[0076] Table 1. List of components for specific embodiments and comparative examples.

[0077]

[0078]

[0079] Preparation method:

[0080] S1: Preparation of the aqueous phase: Add the raw materials from phase A separately, heat to 85℃ and stir to dissolve; S2: Preparation of the oil phase: Add the raw materials from phase B separately, heat to 80℃ and melt.

[0081] S3: Combine phase A and phase B, start homogenization (3000 rpm), homogenize for 12 minutes, and start cooling after homogenization is complete;

[0082] S4: When the temperature drops to about 75℃, add phase C, stir to dissolve, and continue to cool after stirring evenly.

[0083] S5: When the temperature drops to 65-70℃, add phase D, stir to dissolve, and continue to cool down after dissolution is complete.

[0084] S6: When the temperature drops to 45℃, add the E phase components in sequence, stir to dissolve and disperse evenly, and continue to cool down;

[0085] S7: When the temperature drops below 40℃, add the F phase component, stir to dissolve and disperse evenly, and you will get the product.

[0086] Test Example 1: Stability Test

[0087] The stability of the samples from Examples 1-4 and Comparative Examples 1-6 was observed under open room temperature, sealed 40°C, and sealed hot and cold cycling conditions (-18°C, 4°C, 45°C, once every 3 days). The stability of the product was judged by whether color change occurred. The color change time of the product was observed daily. The specific results are shown in Table 2 below.

[0088] Table 2 Stability test results

[0089] Open room temperature Sealed at 45℃ Sealed hot and cold circulation Example 1 20 days 42 days 18 days Example 2 23 days 53 days 19 days Example 3 23 days 56 days 25 days Example 4 21 days 49 days 21 days Comparative Example 1 16 days 24 days 12 days Comparative Example 2 14 days 18 days 12 days Comparative Example 3 9 days 5 days 7 days Comparative Example 4 12 days 10 days 9 days Comparative Example 5 8 days 6 days 7 days Comparative Example 6 7 days 6 days 5 days

[0090] As shown in Table 2, Comparative Example 6, which does not contain the composition, exhibited color change within one week under open-air room temperature, sealed 40°C, and sealed hot and cold cycling conditions. Comparative Examples 3-5 exhibited color change within 5-12 days under open-air room temperature, sealed 40°C, and sealed hot and cold cycling conditions. This indicates that Icelandic lichen extract, sodium hyaluronate (400 Da ~ 3 K Da), sodium hyaluronate (1 W ~ 3 W Da), polyamide-8 (and) pentaerythritol tetra(bis-tert-butylhydroxyhydrocinnamic acid) ester alone did not significantly improve the color change of retinol. Compared with Comparative Examples 1-6, Examples 1-4 significantly prolonged the color change time, indicating that the combination of Icelandic lichen extract, sodium hyaluronate (400 Da ~ 3 K Da), sodium hyaluronate (1 W ~ 3 W Da), and polyamide-8 (and) pentaerythritol tetra(bis-tert-butylhydroxyhydrocinnamic acid) ester can significantly improve the color change phenomenon of retinol; and the Icelandic lichen extract prepared by extraction method one has a more significant synergistic effect.

[0091] Experiment Example 2: Human Body Moisturizing and Repairing Efficacy Test

[0092] Subject selection: 1g of the sample from Comparative Example 6 was accurately weighed and applied to the inner forearm of the subject. The sample was spread evenly in a circular motion 20 times. The sample was applied once in the morning and once in the evening for two consecutive days. Subjects who reported a stinging, burning, or painful sensation were selected. A total of 32 subjects who met the criteria were selected, including 26 females and 6 males, aged 23 to 38 years.

[0093] Test environment: Temperature: 20.0℃-22℃; Relative humidity: 40%-60%.

[0094] Sample usage: The subject rinsed the inner forearm with water, wiped it clean with a tissue, and waited in a constant temperature and humidity environment for 30 minutes. The inner forearm of each subject was divided into 5 square areas, each 2×2cm in size. 1g of each of Examples 1-4 and Comparative Examples 1-6 was applied in circular motions 20 times until completely absorbed. The application frequency was once in the morning and once in the evening for 2 consecutive days. The indicators were measured before use, after 2 days of use, and 3 days after discontinuation.

[0095] Transepidermal water loss (TEWL) test: The TEWL values ​​were measured before and 2 days after application using a Vapormeter SWL5001. Three tests were performed, and the average value was taken. A lower value indicates less transepidermal water loss. Unit: g / (h·m³) 2 ).

[0096] Skin stratum corneum moisture content test: The skin moisture content was tested before use, 2 days after use, and 3 days after discontinuation using the MoistureMeter MSC1201 skin stratum corneum moisture content tester. The average value of the three tests was taken. The higher the value, the higher the moisture content of the skin stratum corneum. Unit: AU.

[0097] Data Analysis: Descriptive statistics, including mean and standard deviation, were performed on each measurement using Excel software. Graph Pad Prism 8 software was used for relevant statistical analysis of the test data. The data in the graphs are presented as mean ± SD. First, descriptive statistics were performed on the data, and the D'agostino & Pearson test was used to test for normality. The statistical analysis methods before and after using the sample are as follows: if p > 0.05, the data is normally distributed, and a paired t-test is used for analysis; if p < 0.05, the data is non-normally distributed, and the Wilcoxon signed-rank test is used for analysis.

[0098] Improvement / reduction (rate of change) after sample use = (Data after use - Data before use) / Data before use

[0099] ×100%

[0100] Judgment criteria: If there is a significant difference in the measured index at any time point before and after the use of the sample, and the difference shows a significant positive trend, then the sample is judged to have the corresponding efficacy.

[0101] The results of the transdermal water loss test are shown in Table 3:

[0102] Table 3. Statistical results of transdermal water loss from skin (n=32)

[0103]

[0104]

[0105] Statistical analysis results: "-": no statistically significant difference (P≥0.05); "*": statistically significant difference (0.01≤P<0.05); "**": statistically significant difference (0.001≤P<0.01); "***": statistically significant difference (P<0.001).

[0106] Table 3 shows that after 2 days of use, the TEWL value of Comparative Example 6 increased significantly, indicating that retinol damages the skin barrier. Examples 1-4 and Comparative Examples 1-3 and 5 significantly reduced the TEWL value, indicating a significant barrier repair effect. The change rate of the examples was significantly greater than that of the comparative examples, with the change rates of Examples 2 and 3 being the most significant. The results show that the Icelandic lichen extract prepared by extraction method one has a more significant synergistic effect with sodium hyaluronate (400 Da~3 KDa), sodium hyaluronate (1 W~3 W Da), and polyamide-8 (and) pentaerythritol tetra(bis-tert-butylhydroxyhydrocinnamic acid) ester; Icelandic lichen extract ① can synergistically reduce the TEWL value and repair the damaged barrier with sodium hyaluronate (400 Da~3 KDa), sodium hyaluronate (1 W~3 W Da), and polyamide-8 (and) pentaerythritol tetra(bis-tert-butylhydroxyhydrocinnamic acid) ester.

[0107] The results of the skin stratum corneum moisture content test are shown in Table 4:

[0108] Table 4. Statistical results of skin stratum corneum moisture content (n=32)

[0109]

[0110]

[0111] Statistical analysis results: "-": no statistically significant difference (P≥0.05); "*": statistically significant difference (0.01≤P<0.05); "**": statistically significant difference (0.001≤P<0.01); "***": statistically significant difference (P<0.001).

[0112] As shown in Table 4, the stratum corneum moisture content of Comparative Example 6 decreased significantly after 2 days of use and after a 3-day discontinuation, indicating that retinol reduces the skin's water retention. After 2 days of use, Examples 1-4 and Comparative Examples 1-5 all significantly increased the stratum corneum moisture content. After 2 days of use and a 3-day discontinuation, the stratum corneum moisture content of Examples 1-4, Comparative Examples 1-3, and 5 significantly increased, with the increase rate of the Examples being significantly greater than that of the Comparative Examples, and the increase rates of Examples 2 and 3 being the most significant. The results showed that the Icelandic lichen extract prepared by extraction method one had a more significant synergistic effect with sodium hyaluronate (400 Da~3 KDa), sodium hyaluronate (1 W~3 W Da), and polyamide-8 (and) pentaerythritol tetra(bis-tert-butylhydroxyhydrocinnamic acid) ester; Icelandic lichen extract① could synergistically increase the moisture content of the stratum corneum with sodium hyaluronate (400 Da~3 KDa), sodium hyaluronate (1 W~3 W Da), and polyamide-8 (and) pentaerythritol tetra(bis-tert-butylhydroxyhydrocinnamic acid) ester, and the effect was still significant 3 days after discontinuation.

[0113] Experimental Example 3: Evaluation of Anti-aging Efficacy in Human Body

[0114] Example 3 and Comparative Example 6 were tested for their anti-aging effects on human skin. A total of 34 participants completed the test, including 5 males and 29 females, aged 30 to 48 years, with an average age of 35.04 ± 4.50 years, meeting the criteria for voluntary inclusion and exclusion of participants.

[0115] How to use: After using toner, take an appropriate amount of sample and apply it evenly to the face. Pat gently until absorbed, then proceed with your normal skincare routine. Use once in the morning and once in the evening, keeping other skincare habits unchanged, for 28 consecutive days.

[0116] Testing time: before using the sample (D0), 7 days after using the sample (D7), and 28 days after using the sample (D28).

[0117] Testing instrument: Cutometer MPA580 (CK GmbH, Germany).

[0118] Test requirements: Perform the test 3 times and take the average value.

[0119] Parameter explanation: The higher the values ​​of R2, R7, and Q1, the higher the skin firmness and the better the anti-aging effect.

[0120] The results are shown in Table 5-7.

[0121] Table 5. Descriptive statistics of skin elasticity R² values ​​(n=34)

[0122]

[0123] Statistical analysis results: "*": Statistically significant difference (0.01 ≤ P < 0.05); "**": Statistically significant difference (0.001 ≤ P < 0.01); "***": Statistically significant difference (P < 0.001)

[0124] Table 6. Descriptive statistics of skin elasticity R7 values ​​(n=34)

[0125]

[0126]

[0127] Statistical analysis results: "-": no statistically significant difference (P≥0.05); "***": statistically significant difference (P<0.001)

[0128] Table 7. Descriptive statistics of skin elasticity Q1 values ​​(n=34)

[0129]

[0130] (Note: "*": The difference is statistically significant (0.01≤P<0.05); "***": The difference is statistically significant (P<0.001).)

[0131] As shown in Tables 5-7, skin elasticity R2 significantly improved in both Example 3 and Comparative Example 6 after 7 and 28 days of use, with little difference in the improvement rate. Skin elasticity R7 significantly improved in both Example 3 and Comparative Example 6 after 28 days of use, with Example 3 showing a higher improvement rate than Comparative Example 6. Skin elasticity Q1 significantly improved in both Example 3 and Comparative Example 6 after 7 and 28 days of use, with Example 3 showing a higher improvement rate after 7 days. The results indicate that the anti-aging efficacy of retinol was not significantly reduced after adding Icelandic lichen extract ① to the combination of sodium hyaluronate (400 Da ~ 3 K Da), sodium hyaluronate (1 W ~ 3 W Da), and polyamide-8 (and) pentaerythritol tetra(bis-tert-butylhydroxyhydrogenated cinnamic acid) ester, and the efficacy was comparable.

[0132] It should be noted that the above examples are only used to illustrate the technical solutions of the present invention and not to limit it. Although the present invention has been described in detail with reference to the given examples, those skilled in the art can modify or make equivalent substitutions to the technical solutions of the present invention as needed, without departing from the spirit and scope of the technical solutions of the present invention.

Claims

1. An anti-aging emulsion that alleviates the irritation of retinol, characterized in that, The anti-aging emulsion contains at least the following components in parts by weight: Icelandic lichen extract 2-15 parts, sodium hyaluronate (400 Da~3 KDa) 0.01-0.1 parts, sodium hyaluronate (1 W~3 W Da) 0.05-0.5 parts, polyamide-8 and pentaerythritol tetra(bis-tert-butylhydroxyhydrocinnamic acid) ester 0.1-0.6 parts, and retinol 0.01-0.1 parts; The extraction and preparation methods of the Icelandic lichen extract are any one or more of the following: Specifically, Method 1: (1) Preparation of eutectic solvent DES: The hydrogen bond acceptor (HBA) is choline chloride and the hydrogen bond donor (HBD) is glycerol. HBA and HBD are mixed in a molar ratio of 1:1-3, stirred and heated to 70-90℃ and maintained for 1-2 h until a clear and uniform transparent liquid is formed. Then water is added to it and stirred to obtain the eutectic solvent. (2) Add Icelandic lichen powder to the DES prepared in step (1) for ultrasonic extraction. After filtering and concentrating the extract, add 1 to 1.2 times the mass of glycerol to the concentrate, stir and mix evenly, and filter to obtain Icelandic lichen extract ①. Method 2: (1) Add Icelandic lichen powder to ethanol solution, with a material-to-liquid mass ratio of 1:15-1:20, adjust pH to acidic, add cellulase for enzymatic hydrolysis by heating, and perform ultrasonic extraction after enzymatic hydrolysis. After ultrasonic extraction, filter to obtain filtrate. (2) Concentrate the filtrate obtained in step (1) until the filtrate has no alcohol smell, add 1 to 1.2 times the mass of the concentrate of glycerol, stir and mix evenly, and filter to obtain Icelandic lichen extract ②; Method 3: (1) Add Icelandic lichen powder to an ethanol solution with a material-to-liquid mass ratio of 1:8-1:12 and perform ultrasonic extraction. After ultrasonic extraction, filter to obtain the filtrate. (2) Concentrate the filtrate obtained in step (1) until the filtrate has no alcohol smell, add 1 to 1.2 times the mass of the concentrate of glycerol, stir and mix evenly, and filter to obtain Icelandic lichen extract ③.

2. The anti-aging emulsion for alleviating retinol irritation as described in claim 1, characterized in that, The polyamide-8 and pentaerythritol tetra(bis-tert-butylhydroxyhydrogenated cinnamic acid) ester are a combination of polyamide-8 and pentaerythritol tetra(bis-tert-butylhydroxyhydrogenated cinnamic acid) ester, with a mass ratio of 0.1-1:99-99.

9.

3. The anti-aging emulsion for alleviating retinol irritation as described in claim 1, characterized in that, The anti-aging emulsion also contains commonly used cosmetic excipients in emulsions, including emulsifiers, oils, polyols, thickeners, preservatives, chelating agents, and solvents.

4. The anti-aging emulsion for alleviating retinol irritation as described in claim 3, characterized in that, Solvents include water.

5. The anti-aging emulsion for alleviating retinol irritation as described in claim 1, characterized in that, The extraction and preparation method of the Icelandic lichen extract is Method 1.

6. The anti-aging emulsion for alleviating retinol irritation as described in claim 1, characterized in that, In the first method, In step (1), the molar ratio of HBA to HBD is 1:2; The volume fraction of water added is 10-50% of the transparent liquid; In step (2), the Icelandic lichen powder is prepared by washing, drying, crushing, and passing the Icelandic lichen through a 60-100 mesh sieve. The mass ratio of Icelandic lichen powder to DES liquid is 1:10-30; The specific conditions for ultrasonic extraction are as follows: ultrasonic extraction at 30-50℃ for 10-50 min, with ultrasonic power set at 200-300W and ultrasonic frequency at 30-50KHz. The concentration is a vacuum concentration, specifically carried out at 50-60℃. In the second method, In step (1), the Icelandic lichen powder is prepared by washing, drying, pulverizing, and passing the Icelandic lichen through a 60-100 mesh sieve; the ethanol is high-concentration ethanol with a concentration of 70% or higher; the pH is 4.0-6.0; the specific conditions for heating and enzymatic hydrolysis are: adding cellulase at a mass fraction of 0.1-1%, at 40-60℃, and hydrolyzing for 1-5 hours; the conditions for ultrasonic extraction are: ultrasonic extraction for 10-60 minutes, with an ultrasonic power of 100-1000W and an ultrasonic frequency of 10-50KHz. In step (2), the concentration is vacuum concentration, specifically carried out at 50-60°C. In method three, In step (1), the Icelandic lichen powder is prepared by washing, drying, pulverizing, and passing the Icelandic lichen through a 60-100 mesh sieve; the concentration of the ethanol solution is 40%-60%; the specific method of ultrasonic extraction includes: ultrasonic extraction for 10-60 min, ultrasonic power of 100-1000 W, ultrasonic frequency of 10-50 KHz, repeated extraction 2-3 times, and after ultrasonic extraction, the extracts are combined and filtered. In step (2), the concentration is vacuum concentration, specifically carried out at 50-60°C.

7. The anti-aging emulsion for alleviating retinol irritation as described in claim 6, characterized in that, In the first method, In step (1), the molar ratio of HBA to HBD is 1:2; The volume fraction of water added is 30% of the transparent liquid. v / v ; In step (2), the Icelandic lichen powder is prepared by washing, drying, crushing, and passing the Icelandic lichen through a 60-100 mesh sieve. The mass ratio of Icelandic lichen powder to DES solution is 1:

20. w / w ; The specific conditions for ultrasonic extraction are as follows: ultrasonic extraction at 40℃ for 40 min, with ultrasonic power set to 200~300W and ultrasonic frequency set to 30~50KHz. The concentration is a vacuum concentration, specifically carried out at 50-60℃. In the second method, In step (1), the Icelandic lichen powder is prepared by washing, drying, pulverizing, and passing the Icelandic lichen through a 60-100 mesh sieve; the ethanol is high-concentration ethanol with a solution concentration of 85%; the pH is 5.0; the specific conditions for heating and enzymatic hydrolysis are: adding 0.4% cellulase at 50°C for 2 hours; the conditions for ultrasonic extraction are: ultrasonic extraction for 30 minutes, with an ultrasonic power of 500W and an ultrasonic frequency of 30KHz. In step (2), the concentration is vacuum concentration, specifically carried out at 50-60°C. In method three, In step (1), the Icelandic lichen powder is prepared by washing, drying, pulverizing, and passing the Icelandic lichen through a 60-100 mesh sieve; the concentration of the ethanol solution is 40%-60%; the specific method of ultrasonic extraction includes: ultrasonic extraction for 10-60 min, ultrasonic power of 100-1000 W, ultrasonic frequency of 10-50 KHz, repeated extraction 2-3 times, and after ultrasonic extraction, the extracts are combined and filtered. In step (2), the concentration is vacuum concentration, specifically carried out at 50-60°C.

8. A method for preparing the anti-aging emulsion for alleviating retinol irritation according to any one of claims 1-7, characterized in that, The preparation method includes: S1. Preparation of the aqueous phase: Mix 400 Da~3 KDa sodium hyaluronate, 1 W~3 W Da sodium hyaluronate and water, heat to 80-90℃ and stir to dissolve; S2. Preparation of the oil phase: Polyamide-8 and pentaerythritol tetra(bis-tert-butylhydroxyhydrocinnamic acid) ester are heated to 70-90℃ to melt; S3. Homogenize the aqueous and oil phases together; after cooling, add Icelandic lichen extract and retinol.

9. The preparation method according to claim 8, characterized in that, The aqueous phase in step S1 also includes polyols, thickeners, and chelating agents; The oil phase in step S2 also includes emulsifiers and greases; In step S3, the specific conditions for homogenization are: homogenization at 2000-5000 rpm for 5-20 minutes.

10. The preparation method according to claim 8, characterized in that, The preparation method further includes: S4. When the temperature drops to 75℃, add the pH adjuster, stir to dissolve, and continue to cool after stirring evenly. S5. When the temperature drops to 65~70℃, add the preservative, stir to dissolve, and continue to cool down after dissolution. S6. When the temperature drops to 45℃, add Icelandic lichen extract and other raw materials in sequence, stir to dissolve and disperse evenly, and continue to cool down; S7: When the temperature drops below 40℃, add retinol, stir to dissolve and disperse evenly, and you have the product.

11. The use of the anti-aging emulsion according to any one of claims 1-7 in the preparation of cosmetics.

12. A cosmetic product, characterized in that, The cosmetic product comprises at least the anti-aging emulsion as described in any one of claims 1-7.

13. The cosmetic product as described in claim 12, characterized in that, The cosmetics in question are skincare products.

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