Anti-aging emulsion for relieving irritation of retinol as well as preparation method and application of anti-aging emulsion
The anti-aging emulsion prepared by combining Icelandic lichen extract, sodium hyaluronate and polyamide-8 (and)pentaerythritol tetra(bis-tert-butylhydroxyhydrogenated cinnamic acid) ester with retinol, solves the irritability and instability of retinol in cosmetics, significantly improving the stability of the product and the skin care effect.
Patent Information
- Application Number
- CN202510321247.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-03-18
- Publication Date
- 2025-04-29
- Estimated Expiration
- 2045-03-18
AI Technical Summary
Retinol and its derivatives are prone to hypersensitivity reactions, drying and barrier damage when used in cosmetics, while its instability limits its application.
An anti-aging emulsion was prepared using the combination of Icelandic lichen extract, sodium hyaluronate and polyamide-8 (and)pentaerythritol tetra(bis-tert-butylhydroxyhydrogenated cinnamic acid) ester and retinol to improve the stability and skin-friendliness of retinol by homogenization and specific formulations.
It significantly extends the color change time of retinol, improves the stability of the product, reduces the water dispersion of the skin, increases the moisture content of the skin's stratum corneum, and maintains the anti-aging effect of retinol, effectively alleviating the irritation problems of retinol.
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Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of cosmetics, and particularly relates to an anti-aging lotion that alleviates the irritation of retinol, and a preparation method and application thereof. Background Art
[0002] The information disclosed in this background technology section is only intended to enhance the understanding of the overall background of the invention, and should not necessarily be regarded as an admission or any form of suggestion that the information constitutes the prior art already known to a person skilled in the art.
[0003] In recent years, with the booming development of the appearance economy, "anti-aging" and "anti-photoaging" related products have attracted more and more attention from consumers. Retinol and its derivatives are recognized as anti-wrinkle and anti-aging active substances and are widely used in cosmetics. However, a series of hypersensitivity reactions will occur when using products containing retinol and its derivatives. Both natural and synthetic retinols are specific agonists of transient receptor potential channel vanilloid subtype 1 (TRPV1) receptors, which can cause nociceptive sensory neuron excitation and induce hypersensitivity reactions. Another effect of retinol and its derivatives on the skin is dryness and peeling of the skin. 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 the transepidermal water loss (TEWL) value, causing dry skin and damaged skin barrier. At the same time, the phototoxic substances produced by the decomposition of retinol by ultraviolet irradiation can also cause strong irritation, resulting in damaged skin barrier.
[0004] At present, the development and design of retinol products are mostly to alleviate the irritation of retinol by adding soothing and moisturizing ingredients, but the inventors have found that many consumers with weak skin tolerance still experience symptoms such as stinging, erythema, burning and dryness after applying skin care products containing such substances. At the same time, the instability of retinol also limits the application of retinol in cosmetics. Retinol has 5 double bonds, active chemical properties, and is easily affected by factors such as oxygen and temperature and undergoes oxidative degradation. After oxidative degradation, the biological activity disappears and color changes occur at the same time. Therefore, while ensuring the efficacy of retinol, how to alleviate the irritation of retinol and improve the stability of retinol products has been a technical problem that researchers in this field have continued to pay attention to for many years. Summary of the invention
[0005] In view of the deficiencies in the prior art, the present invention aims to provide an anti-aging lotion, preparation method and application for alleviating the irritation of retinol. Specifically, the present invention uses Icelandic lichen extract, sodium hyaluronate (400Da~3KDa), sodium hyaluronate (1W~3W Da), polyamide-8 (and) pentaerythritol tetra (di-tert-butyl hydroxyhydrocinnamic acid) ester, and retinol as the main ingredients to prepare the emulsion. After experimental verification, the prepared anti-aging lotion has the effect of significantly repairing barrier damage and improving skin hydration, while not affecting the anti-aging effect of retinol, and can be used to alleviate the irritation problem of retinol, and retinol and Icelandic lichen extract, sodium hyaluronate (400Da~3KDa), sodium hyaluronate (1W~3W Da), polyamide-8 (and) pentaerythritol tetra (di-tert-butyl hydroxyhydrocinnamic acid) ester combination can significantly improve the color change problem of retinol. Based on the above research results, the present invention is completed.
[0006] In order to achieve the above technical objectives, the technical solution provided by the present invention is as follows:
[0007] In a first aspect of the present invention, there is provided an anti-aging lotion for alleviating the irritation of retinol, wherein the anti-aging lotion comprises at least the following components in parts by weight:
[0008] 2-15 parts of Iceland lichen extract, 0.01-0.1 parts of sodium hyaluronate (400Da-3KDa), 0.05-0.5 parts of sodium hyaluronate (1W-3W Da), 0.1-0.6 parts of polyamide-8 (and) pentaerythritol tetra(di-tert-butyl hydroxyhydrocinnamate) ester and 0.01-0.1 parts of retinol.
[0009] Furthermore, the polyamide-8 (and) pentaerythritol tetrakis (di-tert-butyl hydroxyhydrocinnamate) ester is a composition of polyamide-8 and pentaerythritol tetrakis (di-tert-butyl hydroxyhydrocinnamate) ester, and the mass ratio of the two is 0.1-1:99-99.9.
[0010] Furthermore, the anti-aging lotion also contains cosmetic auxiliary ingredients commonly used in lotions, such as emulsifiers, oils, polyols, thickeners, preservatives, chelating agents and solvents (such as water), etc., which are not specifically limited here.
[0011] The second aspect of the present invention provides a method for preparing the above-mentioned anti-aging lotion for alleviating the irritation of retinol, the preparation method comprising:
[0012] S1. Preparation of aqueous phase: Mix sodium hyaluronate (400Da-3KDa), sodium hyaluronate (1W-3W Da) and water, heat to 80-90°C, and stir to dissolve;
[0013] S2. Preparation of oil phase: heating polyamide-8 (and) pentaerythritol tetra(di-tert-butyl hydroxyhydrocinnamate) to 70-90° C. to melt;
[0014] S3, homogenizing the water phase and the oil phase; adding the Icelandic lichen extract and retinol after cooling.
[0015] The third aspect of the present invention provides use of the anti-aging emulsion in the preparation of cosmetics.
[0016] The fourth aspect of the present invention provides a cosmetic, which contains at least the above-mentioned anti-aging lotion. The cosmetic is a skin care product. Experiments have shown that the cosmetic prepared by the present invention can significantly prolong the color change problem of retinol, and can significantly reduce the TEWL value and increase the moisture content of the stratum corneum of the skin. At the same time, the anti-aging effect is significant, and the irritation problem caused by the use of retinol ingredients can be effectively improved.
[0017] Beneficial technical effects of one or more of the above technical solutions:
[0018] (1) Due to the structural problem of retinol, it is easily affected by temperature and oxygen and oxidatively degraded. After degradation, it changes color and loses its biological activity. The present invention uses Iceland lichen extract, sodium hyaluronate (400Da~3KDa), sodium hyaluronate (1W~3WDa), polyamide-8 (and) pentaerythritol tetra (di-tert-butyl hydroxyhydrocinnamate), and retinol as main active ingredients to prepare an anti-aging lotion that can significantly prolong the color change time of retinol and greatly improve the stability of the product.
[0019] (2) It has been verified through experiments 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 lotion prepared by the invention can significantly reduce the TEWL value, increase the moisture content of the stratum corneum of the skin, and alleviate the barrier damage caused by retinol and the reduction of the skin's water retention capacity.
[0021] (4) The preparation method of the anti-aging lotion for alleviating the irritation of retinol obtained by the above technical scheme is simple and easy, cost-saving, and the raw materials are easy to obtain, which is suitable for mass production. Through human efficacy experimental tests, the anti-aging effect is equivalent to that of the lotion containing only retinol, so it has good practical application value. DETAILED DESCRIPTION
[0022] It should be noted that the following detailed descriptions are all illustrative and intended to provide further explanation of the present invention. Unless otherwise specified, all technical and scientific terms used herein have the same meanings as those commonly understood by those skilled in the art to which the present invention belongs.
[0023] It should be noted that the terms used herein are only for describing specific embodiments and are not intended to limit the exemplary embodiments according to the present application. As used herein, unless the context clearly indicates otherwise, the singular form is also intended to include the plural form. In addition, it should be understood that when the terms "comprise" and / or "include" are used in this specification, it indicates the presence of features, steps, operations, devices, components and / or combinations thereof.
[0024] In a typical embodiment of the present invention, an anti-aging lotion for alleviating the irritation of retinol is provided, wherein the anti-aging lotion comprises at least the following components in parts by weight:
[0025] 2-15 parts of Iceland lichen extract, 0.01-0.1 parts of sodium hyaluronate (400Da-3KDa), 0.05-0.5 parts of sodium hyaluronate (1W-3W Da), 0.1-0.6 parts of polyamide-8 (and) pentaerythritol tetra(di-tert-butyl hydroxyhydrocinnamate) ester and 0.01-0.1 parts of retinol.
[0026] Furthermore, the polyamide-8 (and) pentaerythritol tetrakis (di-tert-butyl hydroxyhydrocinnamate) ester is a composition of polyamide-8 and pentaerythritol tetrakis (di-tert-butyl hydroxyhydrocinnamate) ester, and the mass ratio of the two is 0.1-1:99-99.9.
[0027] Furthermore, the anti-aging lotion also contains cosmetic auxiliary ingredients commonly used in lotions, such as emulsifiers (further such as polyglyceryl-6 stearate, polyglyceryl-6 behenate), oils (further such as squalane, 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., which are not specifically limited here.
[0028] The extraction and preparation method of the Icelandic lichen extract may be any one or more of the following, preferably method 1.
[0029] Method 1:
[0030] (1) Preparation of low 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, and stirred and heated to 70-90°C for 1-2 hours until a clear and uniform transparent liquid is formed. Then water is added thereto and stirred to obtain a low eutectic solvent.
[0031] (2) Adding the Icelandic lichen powder to the DES prepared in step (1) for ultrasonic extraction, filtering and concentrating the extract, adding glycerin 1 to 1.2 times the mass of the concentrate, stirring and mixing evenly, filtering to obtain the Icelandic lichen extract①, wherein the concentration is 0.15 to 0.20 g / g based on the crude drug amount.
[0032] In the step (1), the molar ratio of HBA to HBD is preferably 1:2;
[0033] The volume fraction of the added water is 10-50% (preferably 30%, v / v) of the transparent liquid.
[0034] In the step (2), the preparation method of the Iceland lichen powder is as follows: the Iceland lichen is washed, dried, crushed, and sieved through a 60-100 mesh sieve to obtain the powder.
[0035] The mass ratio of the Iceland lichen powder to the DES liquid is 1:10-30, preferably 1:20 (w / w).
[0036] The specific conditions of ultrasonic extraction are: ultrasonic extraction at 30-50° C. (preferably 40° C.) for 10-50 min (preferably 40 min), setting the ultrasonic power to 200-300 W and the ultrasonic frequency to 30-50 KHz.
[0037] The concentration is reduced pressure concentration, specifically carried out at 50-60° C.; the volume of the obtained concentrated solution is 1 / 3-1 / 8 of the volume before concentration.
[0038] Method 2:
[0039] (1) adding Iceland lichen powder to an ethanol solution at a material-liquid mass ratio of 1:15-1:20, adjusting the pH to acidic, adding cellulase for heating enzymolysis, performing ultrasonic extraction after the enzymolysis, and filtering to obtain a filtrate;
[0040] (2) The filtrate obtained in step (1) is concentrated until the filtrate has no alcohol taste, glycerin of 1 to 1.2 times the mass of the concentrated solution is added, the mixture is stirred and mixed evenly, and the Icelandic lichen extract ② is obtained after filtration. The concentration is 0.15 to 0.20 g / g based on the crude drug amount.
[0041] In the step (1), the preparation method of the Iceland lichen powder is: wash, dry, crush and pass the Iceland lichen through a 60-100 mesh sieve. The ethanol is a high-concentration ethanol, and the concentration of the ethanol solution is 70% or more, preferably 85%; the pH is 4.0-6.0 (preferably 5.0); the specific conditions for heating and enzymatic hydrolysis are: the mass fraction of the added cellulase is 0.1-1% (preferably 0.4%), 40-60°C (preferably 50°C), and the enzymatic hydrolysis is 1-5h (preferably 2h); the ultrasonic extraction conditions are: ultrasonic extraction 10-60min (preferably 30min), the ultrasonic power is set to 100-1000W (preferably 500W), and the ultrasonic frequency is 10-50KHz (preferably 30KHz).
[0042] In the step (2), the concentration is carried out under reduced pressure, specifically at 50-60°C.
[0043] Method 3:
[0044] (1) adding Iceland lichen powder to an ethanol solution at a material-liquid mass ratio of 1:8 to 1:12, performing ultrasonic extraction, and filtering to obtain a filtrate after the ultrasonic extraction is completed;
[0045] (2) The filtrate obtained in step (1) is concentrated until the filtrate has no alcohol taste, glycerol is added in an amount of 1 to 1.2 times the mass of the concentrated solution, and the mixture is stirred and mixed evenly. After filtering, the Icelandic lichen extract ③ is obtained. The concentration is 0.15 to 0.20 g / g based on the crude drug amount.
[0046] In the step (1), the preparation method of the Iceland lichen powder is: washing, drying, crushing, and passing through a 60-100 mesh sieve to obtain the Iceland lichen. 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 the end of ultrasonication, the extracts are combined and filtered.
[0047] In the step (2), the concentration is carried out under reduced pressure, specifically at 50-60°C.
[0048] In another specific embodiment of the present invention, a method for preparing the above-mentioned anti-aging lotion for alleviating the irritation of retinol is provided, and the preparation method comprises:
[0049] S1. Preparation of aqueous phase: Mix sodium hyaluronate (400Da-3KDa), sodium hyaluronate (1W-3W Da) and water, heat to 80-90°C, and stir to dissolve;
[0050] S2. Preparation of oil phase: heating polyamide-8 (and) pentaerythritol tetra(di-tert-butyl hydroxyhydrocinnamate) to 70-90° C. to melt;
[0051] S3, homogenizing the water phase and the oil phase; adding the Icelandic lichen extract and retinol after cooling.
[0052] Furthermore, the aqueous phase in step S1 may also include a polyol (such as dipropylene glycol, butylene glycol), a thickener (such as carbomer, xanthan gum), and a chelating agent (such as EDTA-2Na);
[0053] The oil phase in step S2 may also include an emulsifier (such as polyglyceryl-6 stearate, polyglyceryl-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 min.
[0055] Furthermore, the preparation method further comprises:
[0056] S4. When the temperature drops to 75°C, add a pH regulator (such as tromethamine), stir to dissolve, and continue to cool after stirring evenly;
[0057] S5. When the temperature drops to 65-70°C, add preservatives (such as 1,2-hexanediol, p-hydroxyacetophenone), stir to dissolve, and continue to cool after dissolution;
[0058] S6. When the temperature drops to 45°C, add the Icelandic lichen extract and other raw materials (such as dipotassium glycyrrhizinate) in sequence, stir to dissolve and disperse evenly, and continue to cool;
[0059] S7: When the temperature drops below 40°C, add retinol, stir to dissolve and disperse evenly.
[0060] In another specific embodiment of the present invention, there is provided use of the anti-aging emulsion in the preparation of cosmetics.
[0061] In another specific embodiment of the present invention, a cosmetic is provided, the cosmetic comprising at least the above-mentioned anti-aging lotion. The cosmetic is a skin care product. Experiments have shown that the cosmetic prepared by the present invention can significantly prolong the color change problem of retinol, and can significantly reduce the TEWL value and increase the moisture content of the stratum corneum of the skin. At the same time, the anti-aging effect is significant, and the irritation problem caused by the use of retinol ingredients can be effectively improved.
[0062] The present invention is further described below in conjunction with examples. The present invention is further described below by way of examples, but the present invention is not limited to the scope of the embodiments described. Based on the embodiments in the present invention, any variation of the present invention by those skilled in the art without making a creative premise all belongs to the protection scope of the present invention. Meanwhile, in the embodiments of the present invention, unless otherwise specified, all preparation raw materials are commercially available products well known to those skilled in the art.
[0063] Examples 1-3 and Comparative Examples 1-5:
[0064] The specific scheme is shown in Table 1 below, calculated by mass fraction.
[0065] In the examples of the present invention and the comparative examples, the mass ratio of polyamide-8 to pentaerythritol tetra(di-tert-butyl hydroxyhydrocinnamate) in polyamide-8 (and) pentaerythritol tetra(di-tert-butyl hydroxyhydrocinnamate) is 99.5:0.5; the mass ratio of polyglycerol-6 stearate to polyglycerol-6 behenate is 9:1.
[0066] The Icelandic lichen extract ①, the Icelandic lichen extract ②, and the Icelandic lichen extract ③ in the examples and comparative examples of the present invention are obtained by the following method:
[0067] The Icelandic lichen extract ① is prepared by the following method:
[0068] (1) Preparation of low 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 1:2. The solvent is heated to 80° C. using a magnetic heating stirrer and stirred for 1.5 h until a clear and uniform transparent liquid is formed. 30% (V / V) distilled water is added thereto and stirred to obtain a low eutectic solvent.
[0069] (2) Wash, dry, crush and sieve the Icelandic lichen. Accurately weigh a certain amount of Icelandic lichen powder, add DES, the material-liquid mass ratio is 1:20, ultrasonic extraction is performed at 40°C for 40 minutes, the ultrasonic power is set to 300W, the ultrasonic frequency is set to 40KHz, the extract is filtered and concentrated at 55°C to a concentrate of about 1 / 5 of the original volume, 1.1 times the mass of glycerol is added to the concentrate, stirred and mixed evenly, and filtered to obtain the Icelandic lichen extract①. The concentration is 0.1579g / g based on the crude drug amount.
[0070] The Icelandic lichen extract ② is prepared by the following method:
[0071] (1) Wash, dry, crush and sieve the Iceland lichen. Accurately weigh a certain amount of Iceland lichen powder, add 85% ethanol solution, the material-liquid mass ratio is 1:15, adjust the pH to 5.0, add 0.4% cellulase (10000U / g) of the total mass of the ethanol solution, and hydrolyze in a 50℃ water bath for 2h. After the hydrolysis, perform ultrasonic extraction for 30min, the ultrasonic power is 500W, the ultrasonic frequency is 30KHz, and filter after the ultrasonication.
[0072] (2) The filtrate obtained in step (1) was concentrated under reduced pressure at 55° C. until the filtrate had no alcohol taste, glycerol in an amount of 1.12 times the mass of the concentrate was added, the mixture was stirred and mixed evenly, and the Icelandic lichen extract ② was obtained after filtration. The concentration of the extract was 0.1587 g / g based on the crude drug amount.
[0073] The Icelandic lichen extract ③ is prepared by the following method:
[0074] (1) Wash, dry, crush and sieve the Iceland lichen. Accurately weigh a certain amount of Iceland lichen powder, add 55% ethanol solution, the material-liquid mass ratio is 1:10, and ultrasonic extraction is performed for 30 minutes at an ultrasonic power of 500 W and an ultrasonic frequency of 30 KHz. Repeat the extraction twice. After the ultrasonication, 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 taste, glycerol in an amount of 1.1 times the mass of the concentrate was added, the mixture was stirred and mixed evenly, and the Icelandic lichen extract ③ was obtained after filtration. The concentration of the extract was 0.1592 g / g based on the crude drug amount.
[0076] Table 1 Specific examples and comparative examples ingredient list
[0077]
[0078]
[0079] Preparation method:
[0080] S1: Preparation of water phase: add the raw materials in phase A respectively, heat to 85°C and stir to dissolve; S2: Preparation of oil phase: add the raw materials in phase B respectively, heat to 80°C and melt;
[0081] S3: Combine phase A and phase B, start homogenization (3000 rpm), homogenize for 12 minutes, and start cooling after homogenization;
[0082] S4: When the temperature drops to about 75°C, add phase C, stir to dissolve, and continue to cool after stirring evenly;
[0083] S5: When the temperature drops to 65-70°C, add phase D, stir to dissolve, and continue to cool after dissolution;
[0084] S6: When the temperature drops to 45°C, add the components of phase E in sequence, stir to dissolve and disperse evenly, and continue to cool;
[0085] S7: When the temperature drops below 40°C, add the F phase ingredients, stir to dissolve and disperse evenly to obtain the product.
[0086] Test Example 1: Stability Test
[0087] The samples of Examples 1 to 4 and Comparative Examples 1 to 6 were observed for stability under the conditions of open room temperature, sealed at 40°C, and sealed hot and cold cycle (-18°C, 4°C, 45°C, cycle every 3 days). The stability of the product was judged by whether color change occurred. The samples were observed daily and the color change time of the products was observed. The specific results are shown in Table 2 below.
[0088] Table 2 Stability test results
[0089] Open room temperature Sealed 45℃ Sealed hot and cold cycles 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 can be seen from Table 2, comparative example 6 does not contain the composition, and color change occurs within one week under the conditions of open room temperature, sealed at 40°C, and sealed hot and cold cycles; comparative examples 3-5 all experience color change within 5-12 days under the conditions of open room temperature, sealed at 40°C, and sealed hot and cold cycles, indicating that the Icelandic lichen extract, sodium hyaluronate (400Da~3KDa) and sodium hyaluronate (1W~3W Da), polyamide-8 (and) pentaerythritol tetra(di-tert-butyl hydroxyhydrocinnamate) ester alone have no obvious improvement effect on 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 (400Da~3KDa), sodium hyaluronate (1W~3W Da) and polyamide-8 (and) pentaerythritol tetra(di-tert-butyl hydroxyhydrocinnamate) ester can significantly improve the color change phenomenon of retinol; and the Icelandic lichen extract prepared by extraction method 1 has a more significant synergistic effect.
[0091] Test Example 2: Human body moisturizing and repairing efficacy test
[0092] Subject screening: Accurately weigh 1g of the sample of comparative example 6 and apply it on the inner side of the subject's forearm, apply it evenly with 20 circles, once in the morning and once in the evening for 2 consecutive days, and select subjects with tingling, burning, and pain feedback. A total of 32 subjects who met the criteria were screened out, including 26 females and 6 males, aged 23 to 38 years old.
[0093] Test environment: Temperature: 20.0℃-22℃; Relative humidity: 40%-60%.
[0094] Sample usage: The subject rinses the inner side of the forearm with clean water, wipes it clean with a paper towel, and waits for 30 minutes in a constant temperature and humidity environment. The inner side of the left and right forearms of each subject is divided into 5 square areas, each area is 2×2 cm in size, and 1g of each of Examples 1-4 and Comparative Examples 1-6 is applied in circles 20 times until it is completely absorbed. The application frequency is once in the morning and once in the evening, and the application is continued for 2 days. The indicators are tested before use, 2 days after use, and 3 days after use.
[0095] Skin Transdermal Water Loss Test: Use Vapormeter SWL5001 to test the TEWL value before use and 2 days after use. Take the average value after 3 tests. The lower the value, the less transdermal water loss. Unit: g / (h·m 2 ).
[0096] Skin stratum corneum moisture content test: Use the skin stratum corneum moisture content tester MoistureMeterMSC1201 to test the skin moisture content before use, 2 days after use, and 2 days after use and 3 days after rest. The average value is taken for 3 tests. The higher the value, the higher the moisture content of the skin stratum corneum. Unit: AU.
[0097] Data analysis: EXCEL software was used to perform descriptive statistics on each measurement value, including mean and standard deviation. Graph Pad Prism 8 software was used to perform relevant statistical analysis on the test data, and the data in the charts were expressed as mean±SD. First, descriptive statistics were performed on the data, and the D'agostino&Pearson test was used to test the normal distribution of the data. The statistical analysis method before and after the sample was used was as follows: if p>0.05 and the data was normally distributed, a paired t-test was used for analysis; if p<0.05 and the data was non-normally distributed, a Wilcoxon signed rank test was used for analysis.
[0098] Improvement after using the sample (rate of change) = (data after use - data before use) / data before use
[0099] ×100%
[0100] Judgment criteria: If there is a significant difference in the measurement indicators at any visit time point before and after the use of the sample, and the difference shows a significant positive trend, the sample is judged to have the corresponding efficacy.
[0101] The results of the skin percutaneous water loss test are shown in Table 3:
[0102] Table 3 Statistical results of skin transepidermal water loss (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] As shown in Table 3, after 2 days of use, the TEWL value of Comparative Example 6 increased significantly, indicating that retinol can damage the skin barrier. Examples 1-4, Comparative Examples 1-3, and 5 can significantly reduce the TEWL value, indicating that they have significant barrier repair effects. The change rate of the embodiment is significantly greater than that of the comparative example, and the change rate of Examples 2 and 3 is the most significant. The results show that the synergistic effect of the Icelandic lichen extract prepared by extraction method 1 with sodium hyaluronate (400Da~3KDa), sodium hyaluronate (1W~3W Da) and polyamide-8 (and) pentaerythritol tetra (di-tert-butyl hydroxyhydrocinnamate) ester is more significant; Icelandic lichen extract ① with sodium hyaluronate (400Da~3KDa), sodium hyaluronate (1W~3WDa) and polyamide-8 (and) pentaerythritol tetra (di-tert-butyl hydroxyhydrocinnamate) ester can synergistically reduce the TEWL value and repair the damaged barrier.
[0107] The test results of the moisture content of the skin stratum corneum are shown in Table 4:
[0108] Table 4 Statistical results of moisture content of skin stratum corneum (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, after 2 days of use and after 2 days of use and 3 days of discontinuation, the stratum corneum water content of Comparative Example 6 was significantly reduced, indicating that retinol can reduce the water retention of the skin. After 2 days of use, Examples 1-4 and Comparative Examples 1-5 can significantly increase the stratum corneum water content. After 2 days of use and 3 days of discontinuation, the stratum corneum water content of Examples 1-4, Comparative Examples 1-3, and 5 was significantly increased, among which the increase rate of the Examples was significantly greater than that of the Comparative Examples, and the increase rate of Examples 2 and 3 was the most significant. The results showed that the synergistic effect of the Icelandic lichen extract prepared by extraction method 1 with sodium hyaluronate (400Da~3KDa), sodium hyaluronate (1W~3W Da) and polyamide-8 (and) pentaerythritol tetra(di-tert-butyl hydroxyhydrocinnamate) ester was more significant; the Icelandic lichen extract ① with sodium hyaluronate (400Da~3KDa), sodium hyaluronate (1W~3WDa) and polyamide-8 (and) pentaerythritol tetra(di-tert-butyl hydroxyhydrocinnamate) ester could synergistically increase the water content of the stratum corneum, and the effect was still significant after 3 days of discontinuation.
[0113] Test Example 3: Evaluation of anti-aging efficacy in humans
[0114] Example 3 and Comparative Example 6 were tested for their anti-aging efficacy on human skin, and a total of 34 subjects completed the test, including 5 males and 29 females, aged 30 to 48 years old, with an average age of 35.04±4.50, which met the voluntary inclusion and exclusion criteria of the subjects.
[0115] How to use: After using toner, take an appropriate amount of sample and apply it evenly on the face, pat until absorbed, and then carry out normal skin care steps. Use it once in the morning and evening every day. Keep other skin care habits unchanged and use it continuously for 28 days.
[0116] Detection time: before using the sample (D0), 7 days after using the sample (D7), and 28 days after using the sample (D28).
[0117] Test instrument: Skin elasticity tester Cutometer MPA580 (CK Company, Germany).
[0118] Test requirements: Test 3 times and take the average value.
[0119] Parameter explanation: The higher the R2, R7, and Q1 values are, the firmer the skin is and the better the anti-aging effect is.
[0120] The results are shown in Tables 5-7.
[0121] Table 5 Descriptive statistics of skin elasticity R2 value (n=34)
[0122]
[0123] Statistical analysis results: “*”: The difference is statistically significant (0.01≤P<0.05); “**”: The difference is statistically significant (0.001≤P<0.01); “***”: The difference is statistically significant (P<0.001)
[0124] Table 6 Descriptive statistics of skin elasticity R7 value (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 value (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, the skin elasticity R2 of Example 3 and Comparative Example 6 was significantly improved after 7 days and 28 days of use, and the improvement rate was not much different; the skin elasticity R7 of Example 3 and Comparative Example 6 was significantly improved after 28 days of use, and the improvement rate of Example 3 was higher than that of Comparative Example 6; the skin elasticity Q1 of Example 3 and Comparative Example 6 was significantly improved after 7 days and 28 days of use, and the 7-day improvement rate of Example 3 was higher than that of Comparative Example 6. The results show that the anti-aging effect of retinol is not significantly reduced after adding the composition of Icelandic lichen extract ① and sodium hyaluronate (400Da~3KDa), sodium hyaluronate (1W~3W Da) and polyamide-8 (and) pentaerythritol tetra(di-tert-butyl hydroxyhydrocinnamate), and the effect is equivalent.
[0132] It should be noted that the above examples are only used to illustrate the technical solution of the present invention rather than to limit it. Although the present invention is described in detail with reference to the given examples, those skilled in the art may modify or replace the technical solution of the present invention as needed without departing from the spirit and scope of the technical solution of the present invention.
Claims
1. An anti-aging lotion for alleviating the irritation of retinol, characterized in that: The anti-aging lotion comprises at least the following components in parts by weight: 2-15 parts of Iceland lichen extract, 0.01-0.1 parts of sodium hyaluronate (400Da-3KDa), 0.05-0.5 parts of sodium hyaluronate (1W-3WDa), 0.1-0.6 parts of polyamide-8 (and) pentaerythritol tetra(di-tert-butylhydroxyhydrocinnamate) ester and 0.01-0.1 parts of retinol.
2. The anti-aging lotion for alleviating retinol irritation according to claim 1, characterized in that: The polyamide-8 (and) pentaerythritol tetrakis (di-tert-butyl hydroxyhydrocinnamate) ester is a composition of polyamide-8 and pentaerythritol tetrakis (di-tert-butyl hydroxyhydrocinnamate) ester, and the mass ratio of the two is 0.1-1:99-99.
9.
3. The anti-aging lotion for alleviating retinol irritation according to claim 1, characterized in that: The anti-aging lotion also contains cosmetic auxiliary ingredients commonly used in lotions, including emulsifiers, oils, polyols, thickeners, preservatives, chelating agents and solvents (including water).
4. The anti-aging lotion for alleviating retinol irritation according to claim 1, characterized in that: The extraction and preparation method of the Icelandic lichen extract is any one or more of the following; preferably method 1; Specifically, method one: (1) Preparation of low 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, and stirred and heated to 70-90°C for 1-2 hours until a clear and uniform transparent liquid is formed. Then water is added thereto and stirred to obtain a low eutectic solvent. (2) adding the Icelandic lichen powder to the DES prepared in step (1) for ultrasonic extraction, filtering and concentrating the extract, adding glycerin in an amount of 1 to 1.2 times the mass of the concentrate, stirring and mixing evenly, and filtering to obtain the Icelandic lichen extract①; Method 2: (1) adding Iceland lichen powder to an ethanol solution at a material-liquid mass ratio of 1:15-1:20, adjusting the pH to acidic, adding cellulase for heating enzymolysis, performing ultrasonic extraction after the enzymolysis, and filtering to obtain a filtrate; (2) Concentrating the filtrate obtained in step (1) until the filtrate has no alcohol taste, adding glycerin in an amount of 1 to 1.2 times the mass of the concentrated solution, stirring and mixing evenly, and filtering to obtain the Icelandic lichen extract②; Method 3: (1) adding Iceland lichen powder to an ethanol solution at a material-liquid mass ratio of 1:8 to 1:12, performing ultrasonic extraction, and filtering to obtain a filtrate after the ultrasonic extraction is completed; (2) The filtrate obtained in step (1) is concentrated until the filtrate has no alcohol taste, glycerin in an amount of 1 to 1.2 times the mass of the concentrated solution is added, the mixture is stirred and mixed evenly, and the Icelandic lichen extract is obtained after filtering.
5. The anti-aging lotion for alleviating retinol irritation according to claim 4, characterized in that: In the method 1, In the step (1), the molar ratio of HBA to HBD is 1:2; The volume fraction of water added is 10-50% (preferably 30%, v / v) of the transparent liquid; In the step (2), the preparation method of the Iceland lichen powder is as follows: washing, drying, crushing, and passing through a 60-100 mesh sieve to obtain the Iceland lichen powder; The mass ratio of the Iceland lichen powder to the DES liquid is 1:10-30, preferably 1:20 (w / w); The specific conditions of ultrasonic extraction are: ultrasonic extraction at 30-50°C (preferably 40°C) for 10-50min (preferably 40min), setting the ultrasonic power to 200-300W, and the ultrasonic frequency to 30-50KHz; The concentration is carried out under reduced pressure, specifically at 50-60°C; In the second method, In the step (1), the preparation method of the Iceland lichen powder is as follows: the Iceland lichen is washed, dried, crushed, and sieved through a 60-100 mesh sieve to obtain the powder; the ethanol is a high-concentration ethanol, and the concentration of the ethanol solution is 70% or more, preferably 85%; the pH is 4.0-6.0 (preferably 5.0); the specific conditions for heating enzymatic hydrolysis are: the mass fraction of the added cellulase is 0.1-1% (preferably 0.4%), 40-60°C (preferably 50°C), and the enzymatic hydrolysis is 1-5h (preferably 2h); the ultrasonic extraction conditions are: ultrasonic extraction for 10-60min (preferably 30min), the ultrasonic power is set to 100-1000W (preferably 500W), and the ultrasonic frequency is 10-50KHz (preferably 30KHz); In the step (2), the concentration is carried out under reduced pressure, specifically at 50-60° C.; In the third method, In the step (1), the preparation method of the Iceland lichen powder is as follows: washing, drying, crushing, and passing through a 60-100 mesh sieve to obtain the Iceland lichen powder; 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 the end of ultrasonication, the extracts are combined and filtered; In the step (2), the concentration is carried out under reduced pressure, specifically at 50-60°C.
6. The method for preparing the anti-aging lotion for alleviating the irritation of retinol according to any one of claims 1 to 5, characterized in that: The preparation method comprises: S1. Preparation of aqueous phase: Mix sodium hyaluronate (400Da-3KDa), sodium hyaluronate (1W-3W Da) and water, heat to 80-90°C, and stir to dissolve; S2. Preparation of oil phase: heating polyamide-8 (and) pentaerythritol tetra(di-tert-butyl hydroxyhydrocinnamate) to 70-90° C. to melt; S3, homogenizing the water phase and the oil phase; adding the Icelandic lichen extract and retinol after cooling.
7. The preparation method according to claim 6, characterized in that: The aqueous phase in step S1 also includes polyol, thickener and chelating agent; The oil phase in step S2 also includes emulsifier and oil; In step S3, the specific conditions for homogenization are: homogenization at 2000-5000 rpm for 5-20 min.
8. The preparation method according to claim 6, characterized in that: The preparation method further comprises: S4. When the temperature drops to 75°C, add the pH regulator, stir to dissolve, and continue to cool after stirring evenly; S5. When the temperature drops to 65-70°C, add preservatives, stir to dissolve, and continue to cool after dissolution; S6. When the temperature drops to 45°C, add the Icelandic lichen extract and other raw materials in sequence, stir to dissolve and disperse evenly, and continue to cool; S7: When the temperature drops below 40°C, add retinol, stir to dissolve and disperse evenly.
9. Use of the anti-aging emulsion according to any one of claims 1 to 5 in the preparation of cosmetics.
10. A cosmetic, characterized in that: The cosmetic comprises at least the anti-aging lotion according to any one of claims 1 to 5; further, the cosmetic is a skin care product.
Citation Information
Patent Citations
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