Anti-aging facial cream and preparation method thereof
By using natural active ingredients and specific processes, the problems of retinol ingredients are solved and the skin is irritating, achieving high transdermal absorption and significant anti-aging effects.
Patent Information
- Application Number
- CN202111466487.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2021-12-03
- Publication Date
- 2025-08-19
- Estimated Expiration
- 2041-12-03
AI Technical Summary
The retinol ingredients in existing anti-aging skin care products are unstable, have high irritation to the skin, and contain a large number of chemical synthetic substances, which have problems such as insufficient efficacy, easy to be allergic, and poor absorption.
Anti-aging creams are prepared using natural active ingredients, including anti-aging compositions, xanthan gum, glycerin and other components. Through specific process preparation methods, the transdermal absorption and stability are improved and collagen fiber generation is promoted.
It has achieved good stability and high transdermal absorption of anti-aging cream, which can repair the skin tissue form, accelerate the renewal of elastic fibers, and has significant anti-aging and firming skin effects.
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Figure CN116270373B_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the field of daily chemicals, and in particular to an anti-aging facial cream and a preparation method thereof. Background Art
[0002] Delicate, smooth, and elastic skin is the pursuit of every beauty enthusiast and a symbol of youthful vitality. With age and environmental influences, the skin inevitably develops signs of aging. The main manifestations of skin aging include dryness, roughness, paleness, lack of luster, sagging and loss of elasticity, wrinkles, and even skin atrophy, cracks, and age spots.
[0003] There are a wide variety of anti-aging skincare products available on the market, including those containing retinol. Retinol, a commonly used ingredient in anti-aging skincare products, and its many derivatives are collectively known as the "retinoids" family. These include retinal, retinoic acid (also known as "retinoic acid"), retinyl esters (such as retinyl palmitate, retinyl acetate, retinyl propionate, retinyl retinoate), and beta-carotene. These are frequently used in anti-aging products such as face creams, serums, and eye creams. However, there are some problems in the application of retinol: 1. Photoinstability: Since the tetraene side chain of retinol easily accepts the energy of light waves, its structure is easily changed under ultraviolet irradiation, resulting in loss of activity; 2. Activity attenuation problem: Experimental studies have shown that at room temperature, standard solutions of retinol, retinal, and retinol lipids have varying degrees of activity attenuation, among which retinol attenuates the most seriously; 3. Skin irritation: People with different skin types show different tolerance when using it, and may experience erythema, peeling, pain and other discomforts. Literature (Fu PP, Cheng SH, Coop L, et al. Photoreaction, phototoxicity, and photocarcinogenicity of retinoids[J]. Journal of Environmental Science and Health Part C: EnvironmentalCarcinogenesis&Ecotoxicology Reviews, 2003, 21(2):165-197.) found that compared with retinol, retinyl palmitate is less stable under UV light and has a stronger UVB photodegradation effect on retinoids, resulting in photosensitivity and phototoxicity. At the same time, due to the safety risks of retinoids, their use in skin care products is limited. Most skin care products contain a large amount of chemical synthetic substances or use many plant extracts with unclear active ingredients, which have problems such as insufficient efficacy, easy allergies, poor absorption, and greasiness.
[0004] Therefore, it is very necessary to develop anti-aging skin care products that are mainly made of natural active ingredients, have good stability, good absorbability and significant efficacy. Summary of the Invention
[0005] In order to solve the above technical problems, the present invention provides an anti-aging cream, which has good transdermal absorption, can repair skin tissue morphology, accelerate the renewal of elastic fibers, promote collagen fiber production, and achieve the effects of anti-aging and skin firming.
[0006] To this end, the technical solutions provided by this application are as follows:
[0007] A first aspect of the present invention provides an anti-aging facial cream.
[0008] According to the present invention, the anti-aging cream comprises the following components: component A, component B, component C and component D.
[0009] According to the present invention, the component A comprises water, xanthan gum and glycerin.
[0010] According to the present invention, the component B comprises glyceryl stearate / PEG-100 stearate, cetearyl alcohol, pentaerythrityl distearate, hydrogenated polyisobutene, caprylic / capric triglyceride, dimethicone, and isostearyl isostearate.
[0011] According to the present invention, the component C comprises methylisothiazolinone / iodopropynyl butylcarbamate, phenoxyethanol / ethylhexylglycerin.
[0012] According to the present invention, component D comprises an anti-aging composition.
[0013] According to the present invention, the anti-aging composition comprises an anti-wrinkle composition, soybean lecithin, palmitoyl pentapeptide-4, Dendrobium officinale stem extract, glycerin, caprylic / capric triglyceride, propylene glycol, and polysorbate-80.
[0014] According to the present invention, the anti-wrinkle composition comprises arginine / lysine polypeptide and water.
[0015] In the present invention, the Dendrobium officinale stem extract is a water extract. In some embodiments, the preparation method of the Dendrobium officinale stem extract comprises: extracting the Dendrobium officinale stem by mixing it with water, filtering, membrane separation, drying and crushing, and sterilizing.
[0016] In the present invention, the CAS number of caprylic / capric triglyceride is 73398-61-5, and the CAS number of arginine / lysine polypeptide is 936616-33-0.
[0017] According to the present invention, based on the total weight of the anti-aging cream, the weight ratios of the components of the anti-aging cream are 65.00wt%-79.00wt% of component A, 10.50wt%-24.50wt% of component B, 0.40wt%-1.00wt% of component C, and 5.00wt%-10.00wt% of component D.
[0018] According to the present invention, the anti-aging composition includes the following components in percentage by weight: 30.00wt%-70.00wt% of an anti-wrinkle composition, 0.50wt%-2.50wt% of soy lecithin, 2.50wt%-12.50wt% of glycerin, 0.25wt%-1.25wt% of caprylic / capric triglyceride, 15.00wt%-35.00wt% of propylene glycol, 0.25wt%-1.25wt% of polysorbate-80, 0.01wt%-0.03wt% of palmitoyl pentapeptide-4, 0.10wt%-0.20wt% of a Dendrobium officinale stem extract, and water To100.
[0019] According to the present invention, the anti-wrinkle composition comprises 0.001 wt%-0.005 wt% of arginine / lysine polypeptide and water To100, based on the weight of the anti-wrinkle composition.
[0020] According to the present invention, the amount of arginine / lysine polypeptide added to the anti-wrinkle composition is 0.001 wt%-0.005 wt%, based on the weight of the anti-wrinkle composition, for example, 0.001 wt%, 0.002 wt%, 0.003 wt%, 0.004 wt%, 0.005 wt%, and values between the above values.
[0021] According to the present invention, the amount of the anti-wrinkle composition added to the anti-aging composition is 30.00wt%-70.00wt%, for example, 30.00wt%, 40.00wt%, 50.00wt%, 60.00wt%, 70.00wt%, and values between the above values, based on the weight of the anti-aging composition.
[0022] According to the present invention, the amount of soy lecithin added to the anti-aging composition is 0.50wt%-2.50wt%, based on the weight of the anti-aging composition, for example, it can be 0.50wt%, 1.00wt%, 1.50wt%, 2.00wt%, 2.50wt%, and points between the above values.
[0023] According to the present invention, the amount of glycerol added to the anti-aging composition is 2.50 wt%-12.50 wt%, for example, 2.50 wt%, 5.00 wt%, 7.50 wt%, 10.00 wt%, 12.50 wt%, and values between the above values, based on the weight of the anti-aging composition.
[0024] According to the present invention, the amount of caprylic / capric triglyceride added to the anti-aging composition is 0.25wt%-1.25wt%, based on the weight of the anti-aging composition, for example, it can be 0.25wt%, 0.50wt%, 0.75wt%, 1.00wt%, 1.25wt%, and points between the above values.
[0025] According to the present invention, the amount of propylene glycol added to the anti-aging composition is 15.00 wt%-35.00 wt%, based on the weight of the anti-aging composition, for example, it can be 15.00 wt%, 20.00 wt%, 25.00 wt%, 30.00 wt%, 35.00 wt%, and points between the above values.
[0026] According to the present invention, the amount of polysorbate 80 added to the anti-aging composition is 0.25 wt %-1.25 wt %, for example, 0.25 wt %, 0.50 wt %, 0.75 wt %, 1.00 wt %, 1.25 wt %, and values between the above values, based on the weight of the anti-aging composition.
[0027] According to the present invention, the amount of palmitoyl pentapeptide-4 added to the anti-aging composition is 0.01 wt%-0.03 wt% based on the weight of the anti-aging composition, for example, it can be 0.01 wt%, 0.02 wt%, 0.03 wt%, and points between the above values.
[0028] According to the present invention, based on the weight of the anti-aging composition, the anti-aging composition includes 40.00wt%-60.00wt% of an anti-wrinkle composition, 0.75wt%-1.25wt% of soy lecithin, 2.50wt%-12.50wt% of glycerin, 0.50wt%-1.00wt% of caprylic / capric triglyceride, 20.00wt%-30.00wt% of propylene glycol, 0.50wt%-1.00wt% of polysorbate-80, 0.01wt%-0.03wt% of palmitoyl pentapeptide-4, 0.10wt%-0.20wt% of Dendrobium officinale stem extract, and water To100.
[0029] According to the present invention, the anti-aging cream is prepared by a preparation method comprising the following steps:
[0030] 1) Premix the xanthan gum and glycerin in component A, add to deionized water, and heat to 80-85°C with stirring. Keep stirring for 30 minutes until the xanthan gum is completely dispersed and dissolved. Set aside.
[0031] 2) Mix all ingredients in component B, heat to 80-85°C to melt the solid, and set aside;
[0032] 3) Add component B to component A and mix evenly. Homogenize for 3-5 minutes until emulsified.
[0033] 4) Cool down to below 40℃, add component C and component D, and stir to mix evenly;
[0034] 5) Pass through the membrane and discharge the material.
[0035] The second aspect of the present invention provides a method for preparing the anti-aging cream according to the first aspect of the present invention.
[0036] According to the present invention, the preparation method comprises the following steps:
[0037] 1) Premix the xanthan gum and glycerin in component A, add to deionized water, and heat to 80-85°C with stirring. Keep stirring for, e.g., 30 minutes until the xanthan gum is completely dispersed and dissolved, and set aside.
[0038] 2) Mix all ingredients in component B, heat to 80-85°C to melt the solid, and set aside;
[0039] 3) Add component B to component A and mix evenly. Homogenize for 3-5 minutes until emulsified.
[0040] 4) Cool down to below 40℃, add component C and component D, and stir to mix evenly;
[0041] 5) Pass through the membrane and discharge the material.
[0042] According to the present invention, the component A comprises water, xanthan gum and glycerin.
[0043] According to the present invention, the component B comprises glyceryl stearate / PEG-100 stearate, cetearyl alcohol, pentaerythrityl distearate, hydrogenated polyisobutene, caprylic / capric triglyceride, dimethicone, and isostearyl isostearate.
[0044] According to the present invention, the component C comprises methylisothiazolinone / iodopropynyl butylcarbamate, phenoxyethanol / ethylhexylglycerin.
[0045] According to the present invention, component D comprises an anti-aging composition.
[0046] According to the present invention, the anti-aging composition comprises an anti-wrinkle composition, soybean lecithin, palmitoyl pentapeptide-4, Dendrobium officinale stem extract, glycerin, caprylic / capric triglyceride, propylene glycol, and polysorbate-80.
[0047] According to the present invention, the anti-wrinkle composition comprises arginine / lysine polypeptide and water.
[0048] According to the present invention, based on the total weight of the anti-aging cream, the component A comprises the following components in percentage by weight: water to 100, 0.05wt%-0.10wt% xanthan gum, and 1.00wt%-4.00wt% glycerol.
[0049] According to the present invention, based on the total weight of the anti-aging cream, the component B includes the following components in percentage by weight: 1.50wt%-3.00wt% glyceryl stearate / PEG-100 stearate, 0.80wt%-1.50wt% cetearyl alcohol, 1.00wt%-2.00wt% pentaerythritol distearate, 2.00wt%-5.00wt% hydrogenated polyisobutene, 2.00wt%-5.00wt% caprylic / capric triglyceride, 1.00wt%-3.00wt% polydimethylsiloxane, and 2.00wt%-5.00wt% isostearyl isostearate.
[0050] According to the present invention, based on the weight of the anti-aging cream, the component D comprises the following components in percentage by weight: 5.00 wt % to 10.00 wt % of the anti-aging composition.
[0051] According to the present invention, the anti-aging composition includes the following components in percentage by weight: 30.00wt%-70.00wt% of an anti-wrinkle composition, 0.50wt%-2.50wt% of soy lecithin, 2.50wt%-12.50wt% of glycerin, 0.25wt%-1.25wt% of caprylic / capric triglyceride, 15.00wt%-35.00wt% of propylene glycol, 0.25wt%-1.25wt% of polysorbate-80, 0.01wt%-0.03wt% of palmitoyl pentapeptide-4, 0.10wt%-0.20wt% of a Dendrobium officinale stem extract, and water To100.
[0052] According to the present invention, the anti-wrinkle composition comprises 0.001 wt%-0.005 wt% of arginine / lysine polypeptide and water To100, based on the weight of the anti-wrinkle composition.
[0053] Beneficial effects of the present invention:
[0054] The anti-aging cream of the present invention has good stability, high transdermal penetration rate, and good transdermal absorption. It can repair skin tissue morphology, accelerate the renewal of elastic fibers, promote collagen fiber production, and has the effects of anti-aging and firming skin. BRIEF DESCRIPTION OF THE DRAWINGS
[0055] Figure 1 The amount of the anti-wrinkle composition added affects the particle size and zeta potential of the anti-aging composition;
[0056] Figure 2 The effect of the amount of soy lecithin added on the particle size and zeta potential of the anti-aging composition;
[0057] Figure 3 The effect of the amount of glycerol added on the particle size and zeta potential of the anti-aging composition;
[0058] Figure 4 The effect of the amount of caprylic / capric triglyceride added on the particle size and zeta potential of the anti-aging composition;
[0059] Figure 5 The effect of the amount of propylene glycol added on the particle size and zeta potential of the anti-aging composition;
[0060] Figure 6 The effect of the amount of polysorbate-80 added on the particle size and zeta potential of the anti-aging composition;
[0061] Figure 7 is the effect of shearing time on the particle size and zeta potential of the anti-aging composition;
[0062] Figure 8 is the effect of shear speed on the particle size and zeta potential of the anti-aging composition;
[0063] Figure 9 is the effect of homogenization pressure on the particle size and zeta potential of the anti-aging composition;
[0064] Figure 10 The effect of the number of homogenization times on the particle size and zeta potential of the anti-aging composition;
[0065] Figure 11 It is the interaction between the amount of anti-wrinkle composition added and the amount of soy lecithin added;
[0066] Figure 12 It is the interaction between the amount of anti-wrinkle composition added and the amount of propylene glycol added;
[0067] Figure 13 It is the interaction between the amount of Dendrobium officinale extract added and the amount of propylene glycol added;
[0068] Figure 14Fluorescent images (200X) obtained by laser confocal microscopy of the anti-aging compositions of Example 30 and Comparative Example 1;
[0069] Figure 15 are the slice scanning fluorescence images of Example 30 and Comparative Example 1;
[0070] Figure 16 The bright field superimposed images of the slice scans of Example 30 and Comparative Example 1 are shown. DETAILED DESCRIPTION
[0071] The present invention will be described in detail below with reference to the accompanying drawings and embodiments, but the present invention is not limited to the following embodiments.
[0072] Unless otherwise specified, the experimental methods described in the following examples are all conventional methods; the experimental materials and reagents described are all commercially available unless otherwise specified.
[0073] The raw materials used in the present invention are shown in Table 1.
[0074] Table 1 Raw materials and their sources
[0075]
[0076] The information of the instruments and equipment used in the present invention is shown in Table 2.
[0077] Table 2 Instrument / equipment information
[0078]
[0079] Examples 1-5
[0080] Table 3 Components and ratios of the anti-aging compositions of Examples 1-5
[0081]
[0082] Based on the weight of the anti-wrinkle composition, the anti-wrinkle composition includes 0.0024 wt % of arginine / lysine polypeptide and water To100.
[0083] Examples 6-9
[0084] Table 4 Components and proportions of the anti-aging compositions of Examples 6-9
[0085]
[0086] Based on the weight of the anti-wrinkle composition, the anti-wrinkle composition includes 0.0024 wt % of arginine / lysine polypeptide and water To100.
[0087] Examples 10-13
[0088] Table 5 Components and proportions of the anti-aging compositions of Examples 10-13
[0089]
[0090] Based on the weight of the anti-wrinkle composition, the anti-wrinkle composition includes 0.0024 wt % of arginine / lysine polypeptide and water To100.
[0091] Examples 14-17
[0092] Table 6 Components and ratios of the anti-aging compositions of Examples 14-17
[0093]
[0094] Based on the weight of the anti-wrinkle composition, the anti-wrinkle composition includes 0.0024 wt % of arginine / lysine polypeptide and water To100.
[0095] Examples 18-21
[0096] Table 7 Components and proportions of the anti-aging compositions of Examples 18-21
[0097]
[0098] Based on the weight of the anti-wrinkle composition, the anti-wrinkle composition includes 0.0024 wt % of arginine / lysine polypeptide and water To100.
[0099] The preparation method of the anti-aging composition of Examples 1-21 is as follows:
[0100] 1) According to the components and proportions of the anti-aging composition shown in Tables 3-7, soybean lecithin, glycerin, caprylic / capric triglyceride, and propylene glycol were weighed and dissolved at 50°C with magnetic stirring at 600 rpm / min. After the soybean lecithin was fully dissolved, heating was stopped and palmitoyl pentapeptide-4 was added and dissolved to obtain an oil phase. Polysorbate 80, the anti-wrinkle composition, and the aqueous extract of Dendrobium officinale stem were weighed and dissolved in water, and ultrasonically dissolved into a homogeneous system to obtain an aqueous phase.
[0101] 2) Add the oil phase to the water phase and allow to hydrate for 20 minutes to obtain a water-oil mixed solution;
[0102] 3) The water-oil mixture was sheared at 9000 rpm for 5 min to obtain crude ethosomes;
[0103] 4) The crude ethosomes were subjected to high-pressure homogenization at a pressure of 800 bar for 5 times to obtain an anti-aging composition.
[0104] Examples 22-30
[0105] Table 8 Process parameters for preparing the anti-aging compositions of Examples 22-30
[0106]
[0107] The preparation methods of the anti-aging compositions of Examples 22-30 are as follows:
[0108] 1) Weigh 1.00 wt% soy lecithin, 5.00 wt% glycerol, 1.00 wt% caprylic / capric triglyceride, and 25.00 wt% propylene glycol, dissolve them at 50°C with magnetic stirring at 600 rpm. After the soy lecithin is fully dissolved, stop heating, add 0.016 wt% palmitoyl pentapeptide-4, and dissolve to obtain an oil phase for later use; weigh 0.50 wt% polysorbate 80, 50.0 wt% anti-wrinkle composition, and 0.20 wt% Dendrobium officinale stem aqueous extract powder, dissolve them in deionized water, and ultrasonically dissolve them into a homogeneous system to obtain an aqueous phase for later use;
[0109] 2) Add the oil phase to the water phase and allow to hydrate for 20 minutes to obtain a water-oil mixed solution;
[0110] 3) High-speed shearing of the water-oil mixture to obtain crude ethosomes;
[0111] 4) homogenizing the crude ethosomes under high pressure to obtain an anti-aging composition.
[0112] Based on the weight of the anti-wrinkle composition, the anti-wrinkle composition includes 0.0024 wt % of arginine / lysine polypeptide and water To100.
[0113] The high-speed shear speed, shear time, high-pressure homogenization pressure, and homogenization times of the anti-aging compositions of Examples 22-30 are shown in Table 8.
[0114] Comparative Example 1
[0115] 1.00 wt% soy lecithin, 5.00 wt% glycerol, 1.00 wt% caprylic / capric triglyceride and 25.00 wt% propylene glycol were weighed and dissolved at 50°C and 600 rpm / min with magnetic stirring. After the soy lecithin was fully dissolved, heating was stopped and 0.016 wt% palmitoyl pentapeptide-4 was added and dissolved to obtain an oil phase; 0.50 wt% polysorbate-80, 50.0 wt% anti-wrinkle composition and 0.20 wt% water extract powder of Dendrobium officinale stem were weighed and dissolved in deionized water, and ultrasonically dissolved into a homogeneous system to obtain an aqueous phase; the oil phase was added to the aqueous phase and hydrated for 20 minutes to obtain the anti-aging composition of Comparative Example 1.
[0116] Based on the weight of the anti-wrinkle composition, the anti-wrinkle composition includes 0.0024 wt % of arginine / lysine polypeptide and water To100.
[0117] Test Example 1: Average Particle Size and Zeta Potential Measurement
[0118] The anti-aging composition was diluted 1:1000 with deionized water and measured using Malvern dynamic light scattering (DLS) at 25°C to determine its zeta potential, average particle size, and particle size distribution. Each sample was measured in triplicate.
[0119] According to the percentage scoring method, linear interpolation is used to assign a score to the average particle size, and different scores are assigned to samples with different average particle sizes. The average particle size is negatively correlated with the skin penetration rate. The average particle size scoring algorithm is shown in the following formula:
[0120]
[0121] Where: H max ——maximum average particle size of the sample; H——average particle size of the sample; H min ——Minimum average particle size of the sample.
[0122] 1. Experimental results of average particle size and Zeta potential of anti-aging composition
[0123] Depend on Figure 1 It can be seen that the amount of anti-wrinkle composition added significantly affects the average particle size of the anti-aging composition. As the amount of anti-wrinkle composition added increases, the average particle size decreases first and then increases. This trend is also observed in the absolute value of the zeta potential of the anti-aging composition. When the amount of anti-wrinkle composition added is 50.0wt%, the average particle size of the anti-aging composition is the smallest (100.32nm), and the zeta potential of the anti-aging composition is -39.51 mV. Therefore, 50wt% is selected as the optimal amount of the anti-wrinkle composition added.
[0124] Depend on Figure 2 It can be seen that the addition level of soy lecithin has a significant impact on the average particle size of the anti-aging composition. With increasing soy lecithin addition, the average particle size shows a trend of first decreasing and then increasing. The absolute values of the zeta potential of the anti-aging composition are all greater than 40 mV, indicating that the samples prepared using this formulation have relatively good stability. When the soy lecithin addition level is 1wt%, the average particle size of the anti-aging composition is the smallest (97.38 nm) and the PDI is 0.17. Therefore, 1wt% soy lecithin addition level is selected as the optimal addition level for the anti-aging composition.
[0125] Depend on Figure 3It can be seen that the amount of glycerol added has a significant impact on the average particle size of the anti-aging composition. With increasing glycerol addition, the average particle size shows a trend of first decreasing, then increasing, and then continuing to slow. However, the absolute value of the zeta potential shows a trend of first increasing, then decreasing. In the glycerol addition range of 2.5wt% to 5wt%, the average particle size of the anti-aging composition reaches its minimum (101.7 nm), with a PDI of 0.124, indicating a well-dispersed system. The zeta potential of the anti-aging composition is -53.67 mV. As the glycerol addition level increases further, the average particle size of the anti-aging composition increases, while the absolute value of the zeta potential decreases. Considering the average particle size and absolute value of the zeta potential of the anti-aging composition, 5wt% is selected as the optimal glycerol addition level.
[0126] Depend on Figure 4 It can be seen that the addition amount of caprylic / capric triglyceride has a significant effect on the average particle size of the anti-aging composition. As the addition amount increases, the average particle size shows a trend of first decreasing and then increasing, while the absolute value of the zeta potential shows a phenomenon of first increasing and then decreasing. When the addition amount of caprylic / capric triglyceride is 0.25wt%-1wt%, the average particle size of the anti-aging composition decreases with increasing caprylic / capric triglyceride addition amount, and the PDI is less than 0.3, indicating a well-dispersed system. The absolute value of the zeta potential of the anti-aging composition increases. At this time, the average particle size of the ethosome is 100.7 nm, the PDI is 0.202, and the zeta potential is -48.7 mV. When the addition amount of caprylic / capric triglyceride is 1wt%-1.25wt%, the average particle size of the anti-aging composition increases significantly with increasing caprylic / capric triglyceride addition amount, and the absolute value of the zeta potential of the anti-aging composition also decreases. Taking into account the average particle size and the absolute value of the Zeta potential of the anti-aging composition, 1 wt % is selected as the optimal addition amount of caprylic / capric triglyceride.
[0127] Depend on Figure 5 It can be seen that the amount of propylene glycol added significantly affects the average particle size of the anti-aging composition. With increasing propylene glycol addition, the average particle size shows a trend of first decreasing and then increasing, while the absolute value of the zeta potential shows a trend of first increasing and then decreasing. When the propylene glycol addition level is between 15wt% and 25wt%, the average particle size of the anti-aging composition continues to decrease, reaching 82.44 nm. With further increases in propylene glycol, the average particle size of the anti-aging composition increases significantly, with the PDI remaining around 0.2. This indicates that the sample systems obtained under various formulations are uniformly dispersed. Considering that smaller particle sizes have better skin permeability, 25wt% is selected as the optimal propylene glycol addition level.
[0128] Depend on Figure 6It can be seen that the addition amount of polysorbate 80 has a significant impact on the average particle size of the anti-aging composition. With increasing polysorbate 80 addition, the average particle size shows a trend of first decreasing and then increasing, while the absolute value of the zeta potential shows a phenomenon of first increasing and then decreasing. Within the polysorbate 80 addition range of 0.25wt% to 1wt%, the average particle size of the anti-aging composition decreases and then increases, but the overall change is not significant. At a polysorbate 80 addition amount of 0.5wt%, the minimum particle size is 83.79nm, the zeta potential is -33.0mV, and the PDI is 0.201. As the polysorbate 80 addition amount increases to 1.25wt%, the average particle size of the anti-aging composition significantly increases to 158.67nm. Considering the average particle size and absolute value of the zeta potential of the anti-aging composition, 0.5wt% is selected as the optimal polysorbate 80 addition amount.
[0129] Depend on Figure 7-8 As can be seen, with increasing high-speed shearing time, the average particle size of the anti-aging composition continuously decreases until it reaches equilibrium, while the absolute value of the zeta potential initially increases and then remains stable. At a shearing time of 3 minutes, the average particle size of the prepared ethosomes was 94.1 nm. This trend was also observed in the absolute value of the zeta potential of the anti-aging composition. Considering the improved skin permeability of smaller particles and production efficiency, a shearing time of 3 minutes was selected as the optimal process parameter for preparing the anti-aging composition. As the shearing speed increased, reaching 8000 rpm, the average particle size of the anti-aging composition decreased and then remained stable, reaching an average particle size of 90.83 nm. Considering production cost, a shearing speed of 8000 rpm was selected as the optimal process parameter for preparing the anti-aging composition.
[0130] Depend on Figure 9-10 As can be seen, with increasing high-pressure homogenization pressure, the average particle size of the anti-aging composition first decreases and then changes little, while the absolute value of the zeta potential first increases and then decreases. When the homogenization pressure is 700 bar, the average particle size of the prepared ethosomes is 82.5 nm, and the absolute value of the zeta potential of the anti-aging composition is the highest. Considering that smaller particles have better skin permeability and instrument energy consumption, 700 bar is selected as the optimal process parameter for preparing the anti-aging composition. The graphical data showing the effect of different homogenization times on the particle size and zeta potential of the ethosomes shows that after four homogenization cycles, the average particle size of the anti-aging composition is 83.4 nm. With increasing homogenization times, the average particle size of the anti-aging composition does not change much. Considering production cost, four homogenization cycles are selected as the optimal process parameter for preparing the anti-aging composition.
[0131] Test Example 2: Orthogonal Test
[0132] According to the test results of single factor, the factor A that the average particle size of the anti-aging composition is larger is selected. -1 High-pressure homogenization pressure, factor B -1 Homogenization times, factor C -1 The high-speed shear speed was subjected to an orthogonal test with three factors and three waters. The orthogonal experimental design is shown in Table 9.
[0133] Table 9 Optimization factors and levels of process parameters of anti-aging composition
[0134]
[0135] Experimental Example 3: Response Surface Experiment
[0136] According to the results of the single-factor experiment, the material with a larger average particle size of the anti-aging composition was selected as the response surface factors, namely, the amount of the anti-wrinkle composition added by factor A, the amount of soy lecithin added by factor B, and the amount of propylene glycol added by factor C. 17 groups of experiments were designed using Box-Behnken. The test results were based on the particle size score as the response value. The response surface experimental design is shown in Table 10.
[0137] Table 10 Response surface experimental design
[0138]
[0139] 2. Orthogonal results and analysis of the preparation method of anti-aging composition
[0140] Table 11 Orthogonal experimental design and results for optimizing process parameters of anti-aging composition
[0141]
[0142] The experiment was arranged according to the three-factor three-water orthogonal test table, and the results were shown in Table 11. The results show that the optimal process range for the anti-aging composition is high-pressure homogenization pressure 600-800 bar, homogenization times 3-5 times, and high-speed shear speed 7000-9000 rpm. The degree of influence of each factor on the comprehensive index is: A -1 >B -1 >C -1 , that is, within the range selected by the experimental design, the homogenization pressure has the greatest impact on the comprehensive index, followed by the number of homogenizations, and the shear speed has the least impact. The larger the index value, the better, so the optimal formula of the orthogonal is A -1 3B -1 3C -1 3, that is, the homogenization pressure is 800 bar, the number of homogenizations is 5 times, and the shear speed is 9000 rpm.
[0143] 3. Response surface design and results of the addition amount of anti-aging composition components
[0144] Table 12 Response surface experimental design and results
[0145]
[0146] The results of regression fitting analysis of the data are shown in Table 12. The quadratic regression equation obtained by regression fitting the three factors of the amount of anti-wrinkle composition added, the amount of soy lecithin added, and the amount of propylene glycol added is: Y = 98.87-7.12*A-7.88*B-28.07*C-2.68*A*B-9.55*A*C-0.54*B*C+5.24*A 2 -17.62*B 2 -34.51*C 2 The significance of the coefficients and the strength of the interaction between the combined factors are determined by P The value determines P The smaller the value, the more significant it is. From the variance analysis, we can see that P <0.0001 indicates that the regression model is extremely significant and the lack of fit P >0.05 indicates no significance, indicating that the model fits the experimental data well. 2 The regression model's adjusted coefficient of determination (R²adj) was 0.9981, indicating that the model explained 99.81% of the response variation, with only 0.19% of the variation not explained by the model, further demonstrating the model's effectiveness. ANOVA analysis of the model revealed that the anti-wrinkle composition level (A), soy lecithin level (B), propylene glycol level (C), the interaction term between the anti-wrinkle composition level and soy lecithin level (AB), the interaction term between the anti-wrinkle composition level and propylene glycol level (AC), and the quadratic terms of each factor significantly affected the response. The order of factors influencing the product's overall score was: (C) propylene glycol level > (B) soy lecithin level > anti-wrinkle composition level.
[0147] Table 13 Variance analysis table of regression model
[0148]
[0149] Note: **The difference is extremely significant. P <0.01; *Significant difference, P <0.05; NS, no significant difference, P >0.05
[0150] The response surface and contour plots of the interaction between the three factors of the amount of anti-wrinkle composition, the amount of soy lecithin added and the amount of propylene glycol added are as follows: Figure 11-13 The results show that the optimal formulation range for the anti-aging composition is 40wt%-60wt% of the anti-wrinkle composition, 0.75wt%-1.25wt% of soy lecithin, and 20wt%-30wt% of propylene glycol. The response surface plot and contour plots visually reflect the magnitude of the interaction between the two experimental factors on the response value. If the interaction between the two factors has a greater impact on the response value, the response surface plot becomes steeper, and the contour lines will be elliptical. If the interaction between the two factors has a less significant impact on the response value, the contour lines will be circular. In Figures (a) and (c), the response surfaces exhibit a certain degree of convexity and the contour plots exhibit elliptical shapes, indicating a significant interaction between the amount of arginine / lysine peptide added and the amount of soy lecithin added, and a significant interaction between the amount of the anti-wrinkle composition added and the amount of propylene glycol added.
[0151] The Box-Behnken response surface methodology experiment predicted the optimal formula parameters as follows: the addition amount of the anti-wrinkle composition is 50wt%, the addition amount of soy lecithin is 1wt%, and the addition amount of propylene glycol is 25wt%.
[0152] Test Example 4: Transdermal penetration rate
[0153] Test samples: Example 30, Comparative Example 1 Test purpose: To evaluate the percutaneous absorption ability of the product through ex vivo skin. System and management 1) Experimental animals:
[0154] 2) Name: SD rats (male, 7 weeks old) Category: SPF
[0155] 3) Source: Provided by Zhuhai Baishitong Biotechnology Co., Ltd. Laboratory Animal Production License No.: SCXK (Guangdong) 2016-004
[0156] 4) Reagents
[0157] Table 14 Reagent types
[0158]
[0159] 5) Instruments and equipment
[0160] Table 15 Instruments and Equipment
[0161]
[0162] Experimental Procedure and Dosing Method: After euthanizing quarantined SD rats, the back hair was shaved with a shaver. The dorsal skin was excised and rinsed with saline. Subcutaneous fat was removed, and the skin was cut into pieces approximately 2 cm in diameter and side length. 0.3 mL of each prepared marker was dropped onto a non-woven fabric of the same size and fixed to the depilated rat skin. After 15, 30, 60, and 120 minutes of exposure, the skin surface liquid was blotted dry and the skin was fixed in 4% paraformaldehyde solution.
[0163] Detection indicators 1) Laser confocal microscopy scanning analysis - the sample is FITC-labeled and observed using a single green fluorescence channel with an excitation wavelength of 488 nm and scanning observation above 530 nm.
[0164] 2) Slice scanning: The slices are scanned by a digital scanner to obtain fluorescence scanning images and white light (bright field) scanning images.
[0165] Results Analysis: Analyze confocal microscopy images and calculate fluorescence intensity: Fluorescence intensity = fluorescence value / mean fluorescence area. Overlay the fluorescence image with the brightfield scan using image processing software. Analyze the fluorescence penetration depth based on the brightfield overlay image.
[0166] All data were expressed as mean ± SD and analyzed using SPSS software. For measurement data with homogeneous variances or homogeneity after transformation, one-way analysis of variance was performed. If the variances remained unequal after transformation, the rank sum test was used for statistical analysis. The test level was α = 0.05.
[0167] The fluorescence intensity analysis of the anti-aging composition skin sheet is shown in Table 16, and the fluorescence image obtained by laser confocal microscopy is shown in Table 16. Figure 14 .
[0168] Table 16 Fluorescence intensity analysis
[0169]
[0170] Note: * indicates that the data are statistically significantly different from the control sample, p < 0.05.
[0171] The experimental results show that at the same exposure time, the fluorescence intensity of the anti-aging composition of Example 30 is greater than that of the comparative example, and there is a significant difference with the control sample (non-lipidated) at 15min, 30min, and 120min ( p <0.05).
[0172] Depend on Figure 15 The fluorescence images obtained by laser confocal microscopy show that under the same exposure time, the fluorescence intensity of the anti-aging composition of Example 30 is greater than that of the comparative example.
[0173] The fluorescence images and bright field images of the cortex were obtained by slice scanning. The fluorescence penetration depth is shown in Table 17. The fluorescence images are shown in Figure 15 , bright field overlay image see Figure 16 .
[0174] Table 17 Fluorescence penetration depth analysis
[0175]
[0176] Note: * indicates that the data are statistically significantly different from the control sample, p < 0.05.
[0177] As shown in the slice scanning fluorescence image and the slice scanning bright field overlay image, there is no significant difference in the penetration depth between the anti-aging composition of Example 30 and the comparative example.
Claims
1. An anti-aging cream, characterized in that The anti-aging cream comprises the following components: component A, component B, component C and component D; component A comprises water, xanthan gum and glycerin; component B comprises glyceryl stearate / PEG-100 stearate, cetearyl alcohol, pentaerythrityl distearate, hydrogenated polyisobutene, caprylic / capric triglyceride, dimethicone and isostearyl isostearate; component C comprises methylisothiazolinone / iodopropynyl butylcarbamate and phenoxyethanol / ethylhexylglycerin; and component D comprises an anti-aging composition; Based on the total weight of the anti-aging cream, the weight ratio of the components of the anti-aging cream is 65.00wt%-79.00wt% of component A, 10.50wt%-24.50wt% of component B, 0.40wt%-1.00wt% of component C, and 5.00wt%-10.00wt% of component D; Based on the weight of the anti-aging composition, the anti-aging composition includes the following components in percentage by weight: 40.00wt%-60.00wt% of an anti-wrinkle composition, 0.75wt%-1.25wt% of soy lecithin, 2.50wt%-12.50wt% of glycerin, 0.25wt%-1.00wt% of caprylic / capric triglyceride, 20.00wt%-30.00wt% of propylene glycol, 0.50wt%-1.00wt% of polysorbate 80, 0.01wt%-0.03wt% of palmitoyl pentapeptide-4, 0.10wt%-0.20wt% of a Dendrobium officinale stem extract, and water To100; The anti-wrinkle composition comprises, based on the weight of the anti-wrinkle composition, 0.001 wt% to 0.005 wt% of arginine / lysine polypeptide, water To100; The preparation method of the anti-aging composition comprises: 1) Weighing soy lecithin, glycerin, caprylic / capric triglyceride, and propylene glycol according to weight percentage, stirring and dissolving, stopping heating after the soy lecithin is fully dissolved, adding palmitoyl pentapeptide-4, and dissolving to obtain an oil phase; weighing polysorbate 80, an anti-wrinkle composition, and a Dendrobium officinale stem extract according to weight percentage, dissolving them in water, and ultrasonically dissolving them into a homogeneous system to obtain an aqueous phase; 2) Add the oil phase to the water phase for hydration reaction to obtain a water-oil mixed solution; 3) High-speed shearing the water-oil mixture at 7000-9000 rpm for 5 minutes to obtain crude ethosomes; 4) High-pressure homogenizing the crude ethosomes at a pressure of 600-800 bar for 3-5 times to obtain an anti-aging composition.
2. The anti-aging cream according to claim 1, characterized in that The anti-aging facial cream is prepared by a preparation method comprising the following steps: 1) Premix the xanthan gum and glycerin in component A, add to deionized water, and heat to 80-85°C with stirring. Keep stirring for 30 minutes until the xanthan gum is completely dispersed and dissolved. Set aside. 2) Mix all ingredients in component B, heat to 80-85°C to melt the solid, and set aside; 3) Add component B to component A and mix evenly. Homogenize for 3-5 minutes until emulsification is complete. 4) Cool down to below 40℃, add component C and component D, and stir to mix evenly; 5) Pass through the membrane and discharge the material.
3. The method for preparing the anti-aging cream according to claim 1, wherein The preparation method comprises the following steps: 1) Premix the xanthan gum and glycerin in component A, add to deionized water, stir, and heat to 80-85°C. Maintain the mixture and stir until the xanthan gum is completely dispersed and dissolved. Set aside. 2) Mix all ingredients in component B, heat to 80-85°C to melt the solid, and set aside; 3) Add component B to component A and mix evenly. Homogenize for 3-5 minutes until emulsification is complete. 4) Cool down to below 40℃, add component C and component D, and stir to mix evenly; 5) Pass through the membrane and discharge the material.
Citation Information
Patent Citations
Natural herbal anti-aging face cream and method for preparing same
CN105267102A