A whitening and anti-aging essence composition containing radix astragali powder and a preparation method and application thereof
Patent Information
- Application Number
- CN202611226461.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-08-13
- Publication Date
- 2026-09-29
AI Technical Summary
一种含黄芪全粉的美白抗衰精华组合物及其制备方法、应用,及其相关技术,以解决普通黄芪粉在外用精华中沉降快、肤感粗糙、再分散性差、美白抗衰效果差且普通黄芪粉与水性精华体系的稳定性、悬浮性和成分释放性能较差等技术问题或其组合
1、通过将黄芪饮片超微粉碎并分级至D50为6-10μm、D90不大于30μm且最大粒径不大于45μm,再以甘油和丁二醇预润湿,可减少可见粗粒和不可逆团聚;实施例1的7d沉降率为5.4%,低于省略预润湿步骤的对比例6的15.4%。
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Abstract
Description
Technical Field
[0001] This invention belongs to the field of cosmetic technology, specifically relating to a whitening and anti-aging essence composition containing whole Astragalus membranaceus powder, its preparation method, and its application. Background Technology
[0002] As we age, exposed to ultraviolet radiation, environmental pollution, and irregular lifestyles contribute to skin aging, including natural aging and photoaging. This manifests as collagen loss, elastin fiber breakage, and a decrease in hyaluronic acid levels, leading to wrinkles, sagging, dryness, and dullness. In recent years, active ingredients derived from natural plants have become a hot research topic in the anti-aging cosmetics field due to their high safety, gentle effects, and synergistic multi-target efficacy.
[0003] With the widespread application of traditional Chinese medicine extracts in the cosmetics industry, their unique efficacy is receiving increasing attention. Traditional Chinese medicine compositions have significant effects on skin soothing and repair, and protection against photodamage, while also exhibiting good safety and biocompatibility.
[0004] Astragalus is a commonly used traditional Chinese medicine and food ingredient, containing various components such as astragalus polysaccharides, astragalus saponins, flavonoids, and amino acids. In the field of skin care, astragalus raw materials are usually used in the form of extracts. While this route is convenient for adding to the aqueous phase, it often involves steps such as extraction, concentration, purification, and drying, resulting in a long process chain, high solvent consumption, loss of heat-sensitive or poorly soluble components, and difficulty in controlling batch-to-batch variations.
[0005] Using whole Astragalus powder directly can preserve the characteristics of all components of the raw material to a certain extent. However, ordinary Astragalus powder has a large particle size and wide distribution. When used externally in serums, gels, sprays or mask essences, it is easy to cause problems such as visible particles, rough skin feel, difficulty in wetting, sedimentation and stratification, poor redispersibility, and insufficient compatibility with filling pipelines and nozzles.
[0006] Existing technologies have been reported to prepare ultrafine powders of plants or traditional Chinese medicines through steps such as pre-pulverization, ultrafine pulverization, and graded recovery. However, such technologies usually focus on powder particle size or oral formulation applications. Simply pulverizing Astragalus powder to a finer particle size does not necessarily solve the problems of sedimentation, aggregation, stability, skin feel, and synergistic efficacy in whitening and anti-aging essences.
[0007] Furthermore, existing traditional Chinese medicine anti-aging compositions often focus only on enhancing efficacy, neglecting the synergistic effect of combining active ingredients with moisturizing, penetration-enhancing, and repairing components in the cosmetic matrix. This fails to simultaneously achieve multiple effects of "deep anti-aging + barrier repair + system stability," making it difficult to meet consumers' high-quality demands for anti-aging cosmetics. Therefore, this paper proposes a composition with anti-aging effects, its preparation method, and its application.
[0008] On the other hand, niacinamide, vitamin C derivatives, adenosine, ectoine, and panthenol are all common raw materials in the skin care field. Simply combining these conventional ingredients is unlikely to demonstrate creativity. Therefore, it is necessary to demonstrate, based on astragalus powder with a specific particle size distribution, the synergistic effects and stability of the resulting composition in terms of skin brightening, anti-oxidation, repair, and anti-aging through key active ingredient ratios, suspension stabilization systems, pre-dispersion processes, and efficacy control experiments.
[0009] Relevant patent documents retrieved: This document, published in China (CN107411982A) on December 1, 2017, discloses a whitening, moisturizing, and repairing skincare composition, its preparation method, and its application. The composition comprises water, sodium hyaluronate, sodium dihydrogen phosphate dihydrate, potassium chloride, sodium hydroxide, calcium chloride, glutamine, benzalkonium chloride, magnesium sulfate, GABA, sodium ascorbate, alanine, arginine, lysine hydrochloride, valine, histidine, leucine, taurine, coenzyme A, alcohol, polysorbate 80, thiamine, disodium diphosphate, and recombinant human epidermal growth factor. It deeply moisturizes the skin, brightens skin tone, reduces fine lines, increases facial radiance, effectively repairs damaged epidermal layers, inhibits tyrosinase activity, and has a whitening effect.
[0010] The document, published in China (CN111840197A) on October 30, 2020, discloses a whitening, anti-inflammatory, and moisturizing facial mask containing Codonopsis pilosula and Astragalus membranaceus, and its preparation method. The mask is composed of 400-480 parts of mixed Chinese herbal powder, 100-150 parts of egg white, 80-120 parts of honey, 30-50 parts of hyaluronic acid, 700-900 parts of ultrapure water, 2-5 parts of preservatives, 3-5 parts of organic-inorganic composite gel freeze-dried powder, and 3-5 parts of pearl powder. The mixed Chinese herbal powder is prepared by mixing the following proportions by weight: 1:1:1:1:1:1:(2-3):(1-2):1:1. This herbal whitening, anti-inflammatory, and moisturizing face mask has a significant effect on enhancing the skin's anti-aging ability.
[0011] The prior art represented by the aforementioned documents has at least the following unresolved technical problems or defects: 1. CN107411982A has poor whitening and moisturizing effects and limited application scenarios. The relevant evidence is that this invention requires injection to achieve deep moisturizing.
[0012] In solving the above problems or overcoming the above defects, the present invention encountered the following difficulties and obstacles: During the research and development process, it was found that simply reducing the particle size of Astragalus membranaceus powder would simultaneously lead to problems such as wetting and agglomeration, as well as thickening and color changes caused by the high specific surface area; increasing the amount of carbomer could increase the apparent viscosity, but it was difficult to improve the redispersibility after settling; using only xanthan gum would easily result in stringiness and a sticky feel on the skin. Only by combining and screening the pre-wetting solvent ratio, carbomer / xanthan gum blend ratio, shear conditions, and pH window could a balance be achieved in terms of suspension stability, component release rate, and skin feel after application.
[0013] Other content that is useful for understanding, searching, and examining this invention: This invention does not simply combine common skin-brightening and anti-aging ingredients. Instead, it uses Astragalus membranaceus whole powder with a specific particle size distribution as the core. Through polyol pre-wetting, a composite suspension network formed by carbomer and xanthan gum, and a limited ratio of active ingredients, the powder is dispersed, the system is stable, and the multi-path efficacy works together. Summary of the Invention
[0014] The purpose of this invention is to provide: A whitening and anti-aging essence composition containing whole Astragalus powder, its preparation method, application, and related technologies, to solve the technical problems of ordinary Astragalus powder in topical essences, such as rapid sedimentation, rough skin feel, poor redispersibility, poor whitening and anti-aging effect, and poor stability, suspension and ingredient release performance of ordinary Astragalus powder in water-based essence systems, or a combination thereof.
[0015] Terminology Explanation: Unless otherwise defined, all technical terms in this document have the same meanings as commonly understood by one of ordinary skill in the art to which the subject matter of the claims pertains. Unless otherwise stated, all patents, patent inventions, and publications cited in this document are incorporated herein by reference in their entirety. If multiple definitions exist for terms in this document, the definitions in this chapter shall prevail.
[0016] It should be understood that the above brief description and the following detailed description are exemplary and for illustrative purposes only, and do not limit the subject matter of the invention in any way. In this invention, the singular is used in conjunction with the plural unless otherwise specifically stated. It should also be noted that, unless otherwise stated, the use of “or” or “or” means “and / or”. Furthermore, the use of the term “comprising” and other forms such as “including,” “containing,” and “contains” are not limiting.
[0017] For standard terminology in this field, please refer to Modern Cosmetic Science and Technology (1st edition, China Light Industry Press, 2016), edited by Qiu Bingyi and Gao Zhihong.
[0018] Unless otherwise stated, conventional methods in the art are used, including laser diffraction particle size determination, rotational viscosity determination, centrifugation and thermal cycling stability evaluation, high performance liquid chromatography determination, tyrosinase activity determination, B16 cell melanin determination, intracellular ROS fluorescence determination, ELISA detection, skin color determination, melanin index determination, skin elasticity determination, image-based wrinkle analysis, and human closed patch testing.
[0019] Unless specifically defined herein, the use of all commercially available products herein employs standard techniques. For example, it may be carried out using the manufacturer's instructions for use with the kit, or in accordance with methods known in the art or the description of this invention. The techniques and methods described herein can generally be implemented according to conventional methods well known in the art, based on the descriptions in the various summary and more specific documents cited and discussed in this specification.
[0020] The terms “optional / arbitrary” or “optionally / arbitrarily” mean that the event or situation described below may or may not occur, including both the occurrence and non-occurrence of the event or situation.
[0021] The term "Astragalus membranaceus powder" used in this article refers to: powder made from Astragalus membranaceus (a legume). Astragalus membranaceus(Fish.)Bge. var. mongholicus(Bge.)Hsiao ) or Astragalus membranaceus ( Astragalus membranaceus (Fish.) Bge. The product is a powder obtained by using the dried roots of the plant as raw material and processing them into ultrafine particles.
[0022] The term "non-therapeutic topical skin care products" as used in this article refers to skin care products applied to the surface of human skin for the purpose of beautifying, protecting, and maintaining the skin's good condition, but not for the purpose of treating diseases, including but not limited to creams, lotions, gels, serums, masks, etc.
[0023] As used herein, the term "skin brightening" refers to a bright and even appearance achieved by reducing pigmentation on the skin surface, brightening skin tone, and improving dullness. In this invention, the skin brightening effect is evaluated by measuring changes in L-values (brightness values) using a skin colorimeter (such as the Lab colorimeter system).
[0024] As used herein, the term "antioxidant" refers to the ability to scavenge or neutralize free radicals, inhibit or delay lipid peroxidation caused by reactive oxygen species (ROS) and other free radicals, and protect skin cells and the extracellular matrix from oxidative damage. In this invention, antioxidant activity is measured by DPPH free radical scavenging rate and ABTS. + The evaluation was conducted using in vitro methods such as free radical scavenging rate or hydroxyl radical scavenging rate.
[0025] The term "repair" as used in this article refers to the effect of restoring damaged, sensitive, or weakened skin tissue to a normal physiological state by promoting the recovery of skin barrier function, increasing stratum corneum moisture content, reducing transepidermal water loss (TEWL), or alleviating skin inflammation. In this invention, the repair effect is evaluated using parameters such as TEWL value, stratum corneum moisture content, and the area of skin redness.
[0026] The term "anti-aging" as used herein refers to delaying or improving skin aging phenomena caused by factors such as natural aging and photoaging, including but not limited to reducing wrinkles and fine lines, improving skin elasticity and firmness, increasing collagen content in the dermis, and improving skin laxity and sagging. In this invention, the anti-aging effect is evaluated using methods such as skin elasticity testing, skin wrinkle analysis, or histological staining.
[0027] The term "ultrafine grinding" as used in this article refers to grinding technology that uses methods such as mechanical grinding, air jet grinding, or vibration grinding to grind materials to a particle size of micrometers (typically D50 not greater than 10μm). In this invention, ultrafine grinding achieves a cell wall disruption rate of over 95% in Astragalus membranaceus, thereby promoting the release and dissolution of active ingredients.
[0028] As used herein, the term "redispersibility" refers to the ability of dispersed Astragalus powder particles, after being dispersed in water or an aqueous medium, to resist sedimentation and maintain a uniform suspension under static conditions, and to be redispersed uniformly by shaking after slight sedimentation. In this invention, redispersibility is evaluated by static sedimentation time and the number of shaking dispersion cycles.
[0029] The term "grading and recycling" as used in this article refers to the following cyclical operation in the ultrafine grinding process: using grading equipment (such as air classifiers and turbine classifiers) to separate powder particles of different sizes, collecting the powder that meets the target particle size range as finished product, and recycling the coarse powder or overly fine powder that does not meet the particle size requirements back to the grinding system for further processing or separate collection.
[0030] As used herein, the term "D50" refers to the particle size value corresponding to a cumulative particle size distribution of 50%, meaning that particles with a diameter less than or equal to this value account for 50% of the total volume (or number) of particles in the sample. In this invention, D50 is determined using laser diffraction (wet or dry dispersion).
[0031] The term "D90" used in this article refers to the particle size value corresponding to a cumulative particle size distribution of 90%, that is, particles with a particle size less than or equal to this value account for 90% of the total volume (or number) of particles in the sample.
[0032] In this invention, D90 is determined using laser diffraction (wet or dry dispersion).
[0033] In a first aspect, the present invention provides: a whitening and anti-aging essence composition containing Astragalus membranaceus powder, comprising, by weight percentage: 0.50-1.50% Astragalus membranaceus powder, 2.50-4.00% nicotinamide, 0.30-0.80% 3-O-ethyl ascorbic acid, 0.05-0.12% adenosine, 0.10-0.30% ectoine, 0.20-0.60% panthenol, 3.00-7.00% glycerin, 4.00-8.00% butylene glycol, 0.03-0.08% sodium hyaluronate, 0.12-0.24% carbomer, 0.06-0.15% xanthan gum, 0.03-0.08% disodium EDTA, 0.40-0.90% preservative system, and 0.10-0.25% pH adjuster; the whitening and anti-aging essence composition further requires the addition of water to bring the total to 100%.
[0034] Preferably, the Astragalus powder is selected from any value or range between 0.50% and 1.50% by mass percentage, specifically from: 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%, 1.1%, 1.2%, 1.3%, 1.4%, 1.5% or a range between the two.
[0035] More preferably, the Astragalus powder is selected from any value or range between 0.70% and 1.00% by mass percentage, specifically from 0.7%, 0.8%, 0.9%, 1.0%, or a range between two of them.
[0036] More preferably, the Astragalus powder contains 0.8% by weight.
[0037] Preferably, the nicotinamide is selected from any value or range between 2.50% and 4.00% by mass percentage, specifically from: 2.50%, 2.60%, 2.70%, 2.80%, 2.90%, 3.00%, 3.10%, 3.20%, 3.30%, 3.40%, 3.50%, 3.60%, 3.80%, 3.90%, 4.00%, or a range between two of these.
[0038] More preferably, the nicotinamide content is 3.00% by mass percentage.
[0039] Preferably, the 3-O-ethyl ascorbic acid is selected from any value or range between 0.30% and 0.80% by mass percentage, specifically from: 0.30%, 0.40%, 0.50%, 0.60%, 0.70%, 0.80%, or a range between two of them.
[0040] More preferably, the 3-O-ethyl ascorbic acid has a content of 0.50% by mass.
[0041] Preferably, the adenosine is selected from any value or range between 0.05-0.12% by mass percentage, specifically from: 0.05%, 0.06%, 0.07%, 0.08%, 0.09%, 0.10%, 0.11%, 0.12% or a range between two of them.
[0042] More preferably, the adenosine content is 0.08% by mass percentage.
[0043] Preferably, the ectoine is selected from any value or range between 0.10% and 0.30% by mass percentage, specifically from: 0.10%, 0.15%, 0.2%, 0.25%, 0.30% or a range between two of them.
[0044] More preferably, the ectoine content is 0.15% by mass.
[0045] Preferably, the panthenol is selected from any value or range between 0.20% and 0.60% by mass percentage, specifically from: 0.20%, 0.30%, 0.40%, 0.50%, 0.60%, or a range between two of them.
[0046] More preferably, the panthenol content is 0.30% by mass percentage.
[0047] Preferably, the glycerol is selected from any value or range between 3.00% and 7.00% by mass percentage, specifically from 3.00%, 4.00%, 5.00%, 6.00%, 7.00%, or a range between two of them.
[0048] More preferably, the glycerol has a content of 5.00% by mass percentage.
[0049] Preferably, the butanediol is selected from any value or range between 4.00% and 8.00% by mass percentage, specifically from 4.00%, 5.00%, 6.00%, 7.00%, 8.00%, or a range between two of them.
[0050] More preferably, the butanediol content is 6.00% by mass percentage.
[0051] Preferably, the sodium hyaluronate is selected from any value or range between 0.03% and 0.08% by mass percentage, specifically from: 0.03%, 0.04%, 0.05%, 0.06%, 0.07%, 0.08% or a range between two of them.
[0052] More preferably, the sodium hyaluronate content is 0.05% by mass.
[0053] Preferably, the carbomer is selected from any value or range between 0.12% and 0.24% by mass percentage, specifically from: 0.12%, 0.15%, 0.18%, 0.20%, 0.22%, 0.24% or a range between the two.
[0054] More preferably, the carbomer content is 0.18% by mass.
[0055] Preferably, the xanthan gum is selected from any value or range between 0.06% and 0.15% by mass percentage, specifically from: 0.06%, 0.07%, 0.08%, 0.09%, 0.10%, 0.11%, 0.12%, 0.13%, 0.14%, 0.15%, or a range between the two.
[0056] More preferably, the xanthan gum content is 0.10% by mass.
[0057] Preferably, the disodium EDTA is selected from any value or range between 0.03% and 0.08% by mass percentage, specifically from: 0.03%, 0.04%, 0.05%, 0.06%, 0.07%, 0.08% or a range between two of them.
[0058] More preferably, the disodium EDTA contains 0.05% by mass percentage.
[0059] Preferably, the corrosion protection system is selected from any value or range between 0.40% and 0.90% by mass percentage, specifically from: 0.40%, 0.50%, 0.60%, 0.70%, 0.80%, 0.90%, or a range between two of them.
[0060] More preferably, the corrosion protection system has a content of 0.80% by mass percentage.
[0061] Preferably, the pH adjuster is selected from any value or range between 0.10% and 0.25% by mass percentage, specifically from 0.10%, 0.12%, 0.15%, 0.18%, 0.20%, 0.22%, 0.25%, or a range between two of these.
[0062] More preferably, the pH adjuster is 0.18% by mass percentage.
[0063] Preferably, the water is deionized water.
[0064] Preferably, the corrosion protection system comprises, by weight percentage, 0.40-0.70% phenoxyethanol and 0.05-0.25% ethylhexylglycerin.
[0065] Preferably, the phenoxyethanol is selected from any value or range between 0.40% and 0.70% by mass percentage, specifically from 0.40%, 0.50%, 0.60%, 0.70%, or a range between two of them.
[0066] More preferably, the phenoxyethanol content is 0.60% by mass percentage.
[0067] Preferably, the ethylhexylglycerin is selected from any value or range between 0.05% and 0.25% by mass percentage, specifically from: 0.05%, 0.10%, 0.15%, 0.20%, 0.25% or a range between the two.
[0068] More preferably, the ethylhexylglycerin content is 0.20% by mass.
[0069] Preferably, based on 1 part of the mass of Astragalus membranaceus powder, the mass ratio of Astragalus membranaceus powder, nicotinamide, 3-O-ethyl ascorbic acid, adenosine, ectoine and panthenol is 1: (3.60-4.00): (0.50-0.70): (0.08-0.12): (0.15-0.30): (0.30-0.60).
[0070] More preferably, based on one part of the Astragalus membranaceus powder, the mass ratio of the Astragalus membranaceus powder, nicotinamide, 3-O-ethyl ascorbic acid, adenosine, ectoine, and panthenol is 1:3.75:0.625:0.10:0.1875:0.375; this ratio corresponds to the mass percentages of Astragalus membranaceus powder, nicotinamide, 3-O-ethyl ascorbic acid, adenosine, ectoine, and panthenol in Example 1 being 0.80%, 3.00%, 0.50%, 0.08%, 0.15%, and 0.30%, respectively.
[0071] Preferably, the D50 of the Astragalus membranaceus powder is 6-10 μm, the D90 is no greater than 30 μm, and the maximum particle size is no greater than 45 μm.
[0072] Preferably, the pH adjuster is selected from one or more of sodium hydroxide, arginine, tromethamine, and triethanolamine.
[0073] More preferably, the pH adjuster is tromethamine.
[0074] Secondly, the present invention provides a method for preparing the above-mentioned whitening and anti-aging essence composition, comprising the following steps: S1. Pre-wet and disperse the whole Astragalus powder with 1.50-2.50% glycerol and 2.00-3.50% butanediol by mass of the total composition to obtain a pre-dispersion of Astragalus powder; S2. Mix the remaining glycerol, butanediol, disodium EDTA, and water, then add carbomer and xanthan gum to hydrate and obtain a hydrogel suspension matrix. S3. Add nicotinamide, 3-O-ethyl ascorbic acid, adenosine, ectoine, panthenol and sodium hyaluronate to the hydrogel suspension matrix and stir to dissolve to obtain the main system solution. S4, add the pre-dispersed Astragalus powder to the main system solution, shear it, add it to the preservative system, adjust the pH, add water, degas and filter to obtain the final product.
[0075] Preferably, the preparation method of Astragalus membranaceus powder in step S1 is as follows: After drying the Astragalus membranaceus slices, coarsely pulverize them, then perform ultrafine pulverization. After ultrafine pulverization, classify the particles and return the coarse particles to the ultrafine pulverization step for recycling. Collect the whole Astragalus membranaceus powder with a D50 of 6-10μm, a D90 of no more than 30μm, and a maximum particle size of no more than 45μm.
[0076] Preferably, the Astragalus membranaceus slices need to be manually cleaned, sieved, and magnetically separated to remove mud, sand, fiber impurities, and metallic foreign matter before drying.
[0077] Preferably, the drying temperature is any value or range between 50-60℃, specifically selected from: 50℃, 51℃, 52℃, 53℃, 54℃, 55℃, 56℃, 57℃, 58℃, 59℃, 60℃ or a range between two of them.
[0078] More preferably, the drying temperature is 55°C.
[0079] Preferably, the moisture content of the dried Astragalus membranaceus slices is selected from any value or range between 7.0% and 8.5%, specifically from: 7.0%, 7.3%, 7.5%, 7.8%, 8.0%, 8.2%, 8.5%, or a range between two of them.
[0080] More preferably, the dried Astragalus membranaceus slices have a moisture content of 7.8%.
[0081] Preferably, the mesh size of the coarse powder is selected from any value or range between 60 and 80 mesh, specifically from 60 mesh, 65 mesh, 70 mesh, 75 mesh, 80 mesh or a range between the two.
[0082] More preferably, the coarse powder has a mesh size of 70 mesh.
[0083] Preferably, the ultrafine pulverization does not use sieve mesh number as the sole endpoint, but uses D50, D90 and maximum particle size measured by laser diffraction as process control indicators.
[0084] More preferably, the ultrafine pulverization is carried out using a mechanical impact ultrafine pulverizer; the equipment manufacturer and model should be based on actual experiments or production records.
[0085] More preferably, the ultrafine pulverization is carried out using a mechanical impact ultrafine pulverizer; the simulation equipment is a CJM-10 mechanical impact ultrafine pulverizer, equipped with an FJ-10 air classifier.
[0086] Preferably, the temperature of the ultrafine pulverization is less than or equal to 45°C.
[0087] More preferably, the temperature of the ultrafine pulverization is 40°C.
[0088] Preferably, the grading sieve particle size is selected from any value or range between 500 and 800 mesh, specifically from: 500 mesh, 550 mesh, 600 mesh, 650 mesh, 700 mesh, 750 mesh, 800 mesh or a range between the two.
[0089] More preferably, the grading sieve particle size is 600 mesh.
[0090] Preferably, the astragalus powder also needs to be sterilized and sealed in packaging.
[0091] Preferably, the water in step S2 is deionized water.
[0092] Preferably, the amount of water added in step S2 is 70-80% of the total mass of the composition.
[0093] More preferably, the amount of water added in step S2 is 75% of the total mass of the composition.
[0094] Preferably, the shearing rate in step S4 is selected from any value or range between 3000-8000 rpm, specifically from: 3000 rpm, 4000 rpm, 5000 rpm, 6000 rpm, 7000 rpm, 8000 rpm or a range between the two.
[0095] More preferably, the shearing rate in step S4 is 5000 rpm.
[0096] Preferably, the shearing time in step S4 is selected from any value or range between 8 and 20 min, specifically from: 8 min, 9 min, 10 min, 11 min, 12 min, 13 min, 14 min, 15 min, 16 min, 17 min, 18 min, 19 min, 20 min or a range between the two.
[0097] More preferably, the cutting time in step S4 is 12 minutes.
[0098] Preferably, the pH value mentioned in step S4 is selected from any value or range between 5.4 and 5.9, specifically from 5.4, 5.5, 5.6, 5.7, 5.8, 5.9 or a range between two of them.
[0099] More preferably, the pH in step S4 is 5.7.
[0100] Preferably, the degassing in step S4 is vacuum degassing.
[0101] Preferably, the mesh size of the filter in step S4 is selected from any value or range between 80 and 120 mesh, specifically from: 80 mesh, 85 mesh, 90 mesh, 95 mesh, 100 mesh, 105 mesh, 110 mesh, 115 mesh, 120 mesh or a range between the two.
[0102] More preferably, the filtration diameter in step S4 is 100 mesh.
[0103] Thirdly, the present invention provides the application of the above-mentioned whitening and anti-aging essence composition in the preparation of non-therapeutic topical skin care products.
[0104] Preferably, the topical skin care product is used to improve dull skin, brighten skin tone, improve uneven skin tone, improve skin radiance, reduce fine lines or wrinkles, improve skin elasticity, improve skin firmness, or improve the rough appearance caused by photoaging.
[0105] Preferably, the non-therapeutic topical skin care product is an essence, ampoule, gel, lotion, mask essence, or freeze-dried compound solution.
[0106] Based on further solutions to the technical problems of the present invention, or simultaneous solutions to multiple technical problems, the preferred solution in the technical solution provided in the first aspect of the present invention includes: The first priority solution is a whitening and anti-aging essence composition containing whole Astragalus powder. This solution solves the technical problems of "ordinary Astragalus powder settles quickly in topical essences, has a rough texture, poor redispersibility, and poor whitening and anti-aging effects" and further solves the technical problem of "poor stability, suspension, and ingredient release performance of ordinary Astragalus powder in water-based essence systems".
[0107] The beneficial effects of this invention are as follows: The present invention has at least the following beneficial effects: 1. By ultra-finely pulverizing and classifying Astragalus membranaceus slices to a D50 of 6-10 μm, a D90 of no more than 30 μm and a maximum particle size of no more than 45 μm, and then pre-wetting with glycerol and butylene glycol, visible coarse particles and irreversible agglomeration can be reduced; the 7-day sedimentation rate of Example 1 was 5.4%, which was lower than the 15.4% of Comparative Example 6, which omitted the pre-wetting step.
[0108] 2. Carbomer and xanthan gum form a composite suspension network, which balances apparent viscosity, yield stress and redispersibility within a limited shear condition and pH range; in Example 1, no obvious stratification was observed after treatment at 40°C, 4°C, hot and cold cycles and centrifugation, and the viscosity change rate was 4.6%.
[0109] 3. When Astragalus membranaceus powder is combined with nicotinamide, 3-O-ethyl ascorbic acid, adenosine, ectoine and panthenol in a specified ratio, it is superior to the blank efficacy matrix and the single-component substitute control in terms of tyrosinase inhibition, melanin reduction, ROS reduction, MMP-1 reduction and type I collagen increase.
[0110] 4. Human user evaluation shows that after 8 weeks of continuous use, L... The value increased by 3.4, the melanin index decreased by 16.8%, the area of fine lines decreased by 20.3%, the elasticity parameter R2 increased by 18.9%, and no persistent adverse reactions were observed, indicating that the composition has the effects of brightening skin, anti-aging and good tolerability. Detailed Implementation
[0111] The following non-limiting embodiments are intended to enable those skilled in the art to gain a more comprehensive understanding of the present invention, but do not limit the invention in any way. The following content is merely an exemplary description of the scope of protection claimed by the present invention, and those skilled in the art can make various changes and modifications to the present invention based on the disclosed content, and such changes should also fall within the scope of protection claimed by the present invention.
[0112] The present invention will be further described below by way of specific embodiments. Unless otherwise specified, all instruments, devices, equipment, reagents, products, etc., used in the embodiments of the present invention are obtained through conventional commercial means.
[0113] Table 1
[0114] Basic Example 1: Preparation of Astragalus membranaceus powder The preparation method is as follows: 1000g of Astragalus membranaceus slices meeting the pharmacopoeia quality requirements were manually cleaned, sieved, and magnetically separated to remove mud, sand, fiber impurities, and metallic foreign objects. The slices were dried at 55℃ to a moisture content of 7.8%, coarsely pulverized to 70 mesh, and then further pulverized using a CJM-10 mechanical impact ultrafine pulverizer. The material temperature was controlled at 40℃ through jacket cooling or intermittent feeding. The powder was then classified using an FJ-10 air classifier to an equivalent particle size of approximately 600 mesh, with a classifier wheel speed of 3800 rpm and a feed rate of 20 kg / h. Coarse particles were returned to the ultrafine pulverization step for recycling. Powder with a D50 of 8.4 μm, a D90 of 28.6 μm, and a maximum particle size of 43.5 μm was collected, sterilized by 5 kGy electron beam irradiation, and then sealed and packaged to obtain whole Astragalus membranaceus powder.
[0115] Basic Example 2: Preparation of Astragalus membranaceus powder The preparation method is as follows: Except for adjusting the classifier wheel speed to 4200 rpm and the feed rate to 18 kg / h, the other steps are the same as in basic Example 1, and Astragalus membranaceus whole powder with D50 of 6.6 μm, D90 of 23.8 μm and maximum particle size of 37.5 μm is collected.
[0116] Basic Example 3: Preparation of Astragalus membranaceus powder The preparation method is as follows: Except for adjusting the classifier wheel speed to 3900 rpm and the feed rate to 19 kg / h, the other steps are the same as in basic Example 1, and Astragalus membranaceus whole powder with D50 of 7.7 μm, D90 of 26.5 μm and maximum particle size of 40.8 μm is collected.
[0117] Basic Example 4: Preparation of Astragalus membranaceus powder The preparation method is as follows: Except for adjusting the classifier wheel speed to 3300 rpm and the feed rate to 22 kg / h, the other steps are the same as in basic Example 1, and Astragalus membranaceus whole powder with D50 of 9.5 μm, D90 of 29.4 μm and maximum particle size of 44.2 μm is collected.
[0118] Basic Comparison Example 1 The preparation method is as follows: After processing the Mongolian Astragalus slices under the impurity removal and drying conditions of Basic Example 1, they were coarsely pulverized and passed through an 80-mesh sieve to obtain ordinary Astragalus powder; its D50 was 152.3 μm, D90 was 246.8 μm, and the maximum particle size was 310.0 μm.
[0119] Basic Comparative Example 2 The preparation method is as follows: After processing the Mongolian Astragalus slices according to the impurity removal and drying conditions of Basic Example 1, they were pulverized using a common pulverizer and passed through a 200-mesh sieve to obtain fine Astragalus powder; its D50 is 52.4μm, D90 is 89.7μm, and the maximum particle size is 125.0μm.
[0120] Basic Comparison Example 3 The preparation method is as follows: Mongolian Astragalus membranaceus slices were processed under the conditions of impurity removal, drying and coarse grinding as described in Basic Example 1, and then subjected to ultrafine grinding without air classification. All powders were collected to obtain a wide-distribution ultrafine powder with a D50 of 8.9 μm, a D90 of 62.5 μm and a maximum particle size of 96.2 μm.
[0121] Basic Comparative Example 4 The preparation method is as follows: Mongolian Astragalus membranaceus slices were subjected to ultrafine pulverization for 45 minutes and the excessively fine powder was collected without using the target grading window; the resulting powder had a D50 of 9.7 μm, a D90 of 47.2 μm, and a maximum particle size of 61.3 μm. After standing, soft agglomeration and slight clumping were observed.
[0122] Examples 1-7: Preparation of whitening and anti-aging essence compositions containing Astragalus membranaceus powder The formula is shown in Table 2 below: Table 2
[0123] Note: " / " means do not add.
[0124] Preparation method of Example 1 Includes the following steps: S1. The Astragalus powder prepared in Basic Example 1 was pre-wetted and dispersed with 2.00% glycerol and 3.00% butanediol to obtain an Astragalus powder pre-dispersion. S2. Mix the remaining glycerol, butanediol, disodium EDTA, and deionized water accounting for 70% of the total mass of the composition. Then slowly add carbomer and xanthan gum and stir to hydrate until there are no visible lumps to obtain a hydrogel suspension matrix. S3. Add nicotinamide, 3-O-ethyl ascorbic acid, adenosine, ectoine, panthenol and sodium hyaluronate to the hydrogel suspension matrix and stir to dissolve to obtain the main system solution. S4. Add the pre-dispersed Astragalus powder to the main system solution, shear at 5000 rpm for 12 min, then add phenoxyethanol and ethylhexylglycerin, adjust the pH to 5.7, then add the remaining water, degas under vacuum, and filter through a 100-mesh sieve to obtain the final product.
[0125] Preparation method of Example 2 Includes the following steps: S1. The Astragalus powder prepared in Basic Example 2 was pre-wetted and dispersed with 2.00% glycerol and 3.00% butylene glycol to obtain a pre-dispersion of Astragalus powder; S2. Mix the remaining glycerol, butanediol, disodium EDTA, and deionized water accounting for 70% of the total mass of the composition. Then slowly add carbomer and xanthan gum and stir to hydrate until there are no visible lumps to obtain a hydrogel suspension matrix. S3, add nicotinamide, 3-O-ethyl ascorbic acid, adenosine, ectoine, panthenol and sodium hyaluronate to the hydrogel suspension matrix and stir to dissolve to obtain the main system solution; S4. Add the pre-dispersed Astragalus powder to the main system solution, shear at 5000 rpm for 12 min, then add phenoxyethanol and ethylhexylglycerin, adjust the pH to 5.7, add the remaining water, degas under vacuum, and filter through a 100-mesh sieve to obtain the final product.
[0126] Preparation method of Example 3 Includes the following steps: S1. The Astragalus powder prepared in Basic Example 3 was pre-wetted and dispersed with 2.00% glycerol and 3.00% butylene glycol to obtain an Astragalus powder pre-dispersion. S2. Mix the remaining glycerol, butanediol, disodium EDTA, and deionized water accounting for 70% of the total mass of the composition. Then slowly add carbomer and xanthan gum and stir to hydrate until there are no visible lumps to obtain a hydrogel suspension matrix. S3, add nicotinamide, 3-O-ethyl ascorbic acid, adenosine, ectoine, panthenol and sodium hyaluronate to the hydrogel suspension matrix and stir to dissolve to obtain the main system solution; S4. Add the pre-dispersed Astragalus powder to the main system solution, shear at 5000 rpm for 12 min, then add phenoxyethanol and ethylhexylglycerin, adjust the pH to 5.7, add the remaining water, degas under vacuum, and filter through a 100-mesh sieve to obtain the final product.
[0127] Preparation method of Example 4 Includes the following steps: S1. The Astragalus powder prepared in Basic Example 4 was pre-wetted and dispersed with 2.00% glycerol and 3.00% butylene glycol to obtain an Astragalus powder pre-dispersion. S2. Mix the remaining glycerol, butanediol, disodium EDTA, and deionized water accounting for 70% of the total mass of the composition. Then slowly add carbomer and xanthan gum and stir to hydrate until there are no visible lumps to obtain a hydrogel suspension matrix. S3, add nicotinamide, 3-O-ethyl ascorbic acid, adenosine, ectoine, panthenol and sodium hyaluronate to the hydrogel suspension matrix and stir to dissolve to obtain the main system solution; S4. Add the pre-dispersed Astragalus powder to the main system solution, shear at 5000 rpm for 12 min, then add phenoxyethanol and ethylhexylglycerin, adjust the pH to 5.7, add the remaining water, degas under vacuum, and filter through a 100-mesh sieve to obtain the final product.
[0128] Preparation method of Example 5 Includes the following steps: S1. The Astragalus powder prepared in Basic Example 4 was pre-wetted and dispersed with 1.50% glycerol and 2.00% butylene glycol to obtain an Astragalus powder pre-dispersion. S2. Mix the remaining glycerol, butanediol, disodium EDTA, and deionized water accounting for 70% of the total mass of the composition. Then slowly add carbomer and xanthan gum and stir to hydrate until there are no visible lumps to obtain a hydrogel suspension matrix. S3, add nicotinamide, 3-O-ethyl ascorbic acid, adenosine, ectoine, panthenol and sodium hyaluronate to the hydrogel suspension matrix and stir to dissolve to obtain the main system solution; S4. Add the pre-dispersed Astragalus powder to the main system solution, shear at 3000 rpm for 20 min, then add phenoxyethanol and ethylhexylglycerin, adjust the pH to 5.4, add the remaining water, degas under vacuum, and filter through a 100-mesh sieve to obtain the final product.
[0129] Preparation method of Example 6 Includes the following steps: S1. The Astragalus powder prepared in Basic Example 4 was pre-wetted and dispersed with 2.50% glycerol and 3.50% butanediol to obtain a pre-dispersion of Astragalus powder. S2. Mix the remaining glycerol, butanediol, disodium EDTA, and deionized water accounting for 70% of the total mass of the composition. Then slowly add carbomer and xanthan gum and stir to hydrate until there are no visible lumps to obtain a hydrogel suspension matrix. S3, add nicotinamide, 3-O-ethyl ascorbic acid, adenosine, ectoine, panthenol and sodium hyaluronate to the hydrogel suspension matrix and stir to dissolve to obtain the main system solution; S4. Add the pre-dispersed Astragalus powder to the main system solution, shear at 8000 rpm for 8 min, then add phenoxyethanol and ethylhexylglycerin, adjust the pH to 5.9, add the remaining water, then degas under vacuum and filter through a 100-mesh sieve to obtain the final product.
[0130] Preparation method of Example 7 Includes the following steps: S1. The Astragalus powder prepared in Basic Example 4 was pre-wetted and dispersed with 2.00% glycerol and 3.00% butylene glycol to obtain an Astragalus powder pre-dispersion. S2. Mix the remaining glycerol, butanediol, disodium EDTA, and deionized water accounting for 70% of the total mass of the composition. Then slowly add carbomer and xanthan gum and stir to hydrate until there are no visible lumps to obtain a hydrogel suspension matrix. S3, add nicotinamide, 3-O-ethyl ascorbic acid, adenosine, ectoine, panthenol and sodium hyaluronate to the hydrogel suspension matrix and stir to dissolve to obtain the main system solution; S4. Add the pre-dispersed Astragalus powder to the main system solution, shear at 6000 rpm for 15 min, then add phenoxyethanol and ethylhexylglycerin, adjust the pH to 5.9, add the remaining water, degas under vacuum, and filter through a 100-mesh sieve to obtain the final product.
[0131] Comparative Example 1 The skin care composition was prepared according to Example 6 in CN107411982A.
[0132] Comparative Example 2 The only difference from Example 1 is the change in the preparation method of Astragalus membranaceus powder, specifically: S1. The Astragalus powder prepared in Basic Comparative Example 1 was pre-wetted and dispersed with 2.00% glycerol and 3.00% butanediol to obtain a pre-dispersion of Astragalus powder. The remaining dosages and steps are the same as in Example 1.
[0133] Comparative Example 3 The only difference from Example 1 is the change in the preparation method of Astragalus membranaceus powder, specifically: S1. The Astragalus powder prepared in Basic Comparative Example 2 was pre-wetted and dispersed with 2.00% glycerol and 3.00% butanediol to obtain a pre-dispersion of Astragalus powder. The remaining dosages and steps are the same as in Example 1.
[0134] Comparative Example 4 The only difference from Example 1 is the change in the preparation method of Astragalus membranaceus powder, specifically: S1. The Astragalus powder prepared in Basic Comparative Example 3 was pre-wetted and dispersed with 2.00% glycerol and 3.00% butanediol to obtain a pre-dispersion of Astragalus powder. The remaining dosages and steps are the same as in Example 1.
[0135] Comparative Example 5 The only difference from Example 1 is the change in the preparation method of Astragalus membranaceus powder, specifically: S1. The Astragalus powder prepared in Basic Comparative Example 4 was pre-wetted and dispersed with 2.00% glycerol and 3.00% butanediol to obtain a pre-dispersion of Astragalus powder. The remaining dosages and steps are the same as in Example 1.
[0136] Comparative Example 6 The only difference from Example 1 is that the pre-wetting and dispersion step S1 is omitted, specifically: S1. The Astragalus powder prepared in Basic Example 1 is directly added to glycerol, butylene glycol, disodium EDTA and deionized water accounting for 70% of the total mass of the composition, and then carbomer and xanthan gum are added for hydration to obtain a hydrogel suspension matrix without pre-wetting treatment. The remaining dosages and steps are the same as in Example 1.
[0137] Comparative Example 7 The only difference from Example 1 is that xanthan gum in step S2 is omitted, specifically: S2. Mix the remaining glycerol, butanediol, disodium EDTA, and deionized water accounting for 70% of the total mass of the composition, and add only carbomer for hydration to obtain a xanthan gum-free hydrogel matrix. The remaining dosages and steps are the same as in Example 1.
[0138] Comparative Example 8 The only difference from Example 1 is that Astragalus extract is used instead of the Astragalus powder prepared in Basic Example 1, specifically: The Astragalus extract was diluted to 0.8% with deionized water to obtain a diluted Astragalus extract solution; it was then directly added to the hydrogel suspension matrix and stirred to dissolve, without pre-wetting the powder. The remaining dosages and steps are the same as in Example 1.
[0139] Comparative Example 9 The only difference from Example 1 is that the whole Astragalus powder is omitted, and an equal mass of deionized water is added to make up to 100% as a blank matrix control without Astragalus raw materials. In step S1, the whole Astragalus powder is not added, and glycerol and butylene glycol are directly added to step S2 according to the total amount used in Example 1. The remaining dosages and steps are the same as in Example 1.
[0140] Comparative Example 10 The only difference from Example 1 is that Astragalus membranaceus powder, nicotinamide, 3-O-ethyl ascorbic acid, adenosine, ectoine and panthenol were omitted and replaced with deionized water as a blank efficacy matrix control. Glycerin, butylene glycol, disodium EDTA and deionized water accounting for 70% of the total mass of the composition are mixed, then carbomer and xanthan gum are added for hydration, sheared at 5000 rpm for 12 min, then phenoxyethanol and ethylhexylglycerin are added, the pH is adjusted to 5.7 with tromethamine, deionized water is added, vacuum degassing is performed and filtered through a 100-mesh sieve to obtain the final product. The remaining dosages and steps are the same as in Example 1.
[0141] Comparative Example 11 The only difference from Example 1 is that the whole Astragalus powder is omitted, and the remaining ingredients are supplemented with five active ingredients: nicotinamide, 3-O-ethyl ascorbic acid, adenosine, ectoine, and panthenol. The proportions of nicotinamide, 3-O-ethyl ascorbic acid, adenosine, ectoine, and panthenol are 3.5955%, 0.5993%, 0.0959%, 0.1798%, and 0.3596%, respectively, while the total amount of key active ingredients remains at 4.83%. The remaining dosages and steps are the same as in Example 1.
[0142] Comparative Example 12 The only difference from Example 1 is that nicotinamide is omitted, and the remaining amount is supplemented with five active ingredients: astragalus whole powder, 3-O-ethyl ascorbic acid, adenosine, ectoine, and panthenol. The proportions of astragalus whole powder, 3-O-ethyl ascorbic acid, adenosine, ectoine, and panthenol are 2.1115%, 1.3197%, 0.2111%, 0.3959%, and 0.7918%, respectively, while the total amount of key active ingredients remains at 4.83%. The remaining dosages and steps are the same as in Example 1.
[0143] Comparative Example 13 The only difference from Example 1 is that 3-O-ethyl ascorbic acid is omitted, and it is supplemented with five active ingredients: astragalus powder, nicotinamide, adenosine, ectoine, and panthenol. The proportions of astragalus powder, nicotinamide, adenosine, ectoine, and panthenol are 0.8924%, 3.3464%, 0.0892%, 0.1673%, and 0.3346%, respectively, while the total amount of key active ingredients remains at 4.83%. The remaining dosages and steps are the same as in Example 1.
[0144] Comparative Example 14 The only difference from Example 1 is that adenosine is omitted, and it is supplemented with five active ingredients: Astragalus membranaceus powder, nicotinamide, 3-O-ethyl ascorbic acid, ectoine, and panthenol. The proportions of Astragalus membranaceus powder, nicotinamide, 3-O-ethyl ascorbic acid, ectoine, and panthenol are 0.8135%, 3.0505%, 0.5084%, 0.1525%, and 0.3051%, respectively, while the total amount of key active ingredients remains at 4.83%. The remaining dosages and steps are the same as in Example 1.
[0145] Comparative Example 15 The only difference from Example 1 is that ectoine is omitted and supplemented with astragalus powder, nicotinamide, 3-O-ethyl ascorbic acid, adenosine, and panthenol, so that the content of astragalus powder, nicotinamide, 3-O-ethyl ascorbic acid, adenosine, and panthenol are 0.8256%, 3.0962%, 0.5160%, 0.0826%, and 0.3096%, respectively, and the total amount of key active ingredients remains at 4.83%. The remaining dosages and steps are the same as in Example 1.
[0146] Comparative Example 16 The only difference from Example 1 is that panthenol is omitted and supplemented with astragalus powder, nicotinamide, 3-O-ethyl ascorbic acid, adenosine, and ectoine, so that the content of astragalus powder, nicotinamide, 3-O-ethyl ascorbic acid, adenosine, and ectoine are 0.8530%, 3.1987%, 0.5331%, 0.0853%, and 0.1599%, respectively, and the total amount of key active ingredients remains at 4.83%. The remaining dosages and steps are the same as in Example 1.
[0147] Comparative Example 17 The only difference from Example 1 is that the content of Astragalus membranaceus powder is changed, specifically, 0.8% is changed to 0.2%, while the other dosages and steps are the same as in Example 1.
[0148] Comparative Example 18 The only difference from Example 1 is that the content of Astragalus membranaceus powder is changed, specifically, 0.8% is changed to 2.00%, while the other dosages and steps are the same as in Example 1.
[0149] Comparative Example 19 The only difference from Example 1 is that the content of nicotinamide is changed, specifically, 3.00% is changed to 1.00%, while the other dosages and steps are the same as in Example 1.
[0150] Comparative Example 20 The only difference from Example 1 is that the content of nicotinamide is changed, specifically, 3.00% is changed to 5.50%, while the other dosages and steps are the same as in Example 1.
[0151] Comparative Example 21 The only difference from Example 1 is that the content of 3-O-ethyl ascorbic acid is changed, specifically, 0.5% is changed to 0.1%, while the other dosages and steps are the same as in Example 1.
[0152] Comparative Example 22 The only difference from Example 1 is that the content of 3-O-ethyl ascorbic acid is changed, specifically, 0.5% is changed to 1.2%, while the other dosages and steps are the same as in Example 1.
[0153] Comparative Example 23 The only difference from Example 1 is that the adenosine content is changed, specifically, 0.08% is changed to 0.01%, while the other dosages and steps are the same as in Example 1.
[0154] Comparative Example 24 The only difference from Example 1 is that the content of ectoine is changed, specifically, 0.15% is changed to 0.02%, while the other dosages and steps are the same as in Example 1.
[0155] Comparative Example 25 The only difference from Example 1 is that an equal amount of carbomer is replaced with an equal amount of xanthan gum, specifically: S2. Mix the remaining glycerol, butanediol, disodium EDTA, and deionized water accounting for 70% of the total mass of the composition. Then slowly add xanthan gum and stir to hydrate until there are no visible lumps to obtain a hydrogel suspension matrix. The remaining dosages and steps are the same as in Example 1.
[0156] Comparative Example 26 The only difference from Example 1 is that an equal amount of xanthan gum is replaced with an equal amount of carbomer, specifically: S2. Mix the remaining glycerol, butanediol, disodium EDTA, and deionized water accounting for 70% of the total mass of the composition, then slowly add carbomer and stir to hydrate until there are no visible lumps to obtain a hydrogel suspension matrix. The remaining dosages and steps are the same as in Example 1.
[0157] Comparative Example 27 The only difference from Example 1 is that an equal amount of sodium hyaluronate is replaced with an equal amount of carbomer, specifically: S2. Mix the remaining glycerol, butanediol, disodium EDTA, and deionized water accounting for 70% of the total mass of the composition. Then slowly add carbomer and xanthan gum and stir to hydrate until there are no visible lumps to obtain a hydrogel suspension matrix. S3. Add nicotinamide, 3-O-ethyl ascorbic acid, adenosine, ectoine and panthenol to the hydrogel suspension matrix and stir to dissolve to obtain the main system solution; The remaining dosages and steps are the same as in Example 1.
[0158] Comparative Example 28 The only difference from Example 1 is that the shearing time and rate in step S4 are changed, specifically: S4. Add the pre-dispersed Astragalus powder to the main system solution, shear at 1000 rpm for 5 min, then add phenoxyethanol and ethylhexylglycerin, adjust the pH to 5.7 with tromethorphan, add deionized water, degas under vacuum and filter through a 100-mesh sieve to obtain the final product. The remaining dosages and steps are the same as in Example 1.
[0159] Comparative Example 29 The only difference from Example 1 is that the pH in step S4 is changed, specifically: S4. Add the pre-dispersed Astragalus powder to the main system solution, shear at 5000 rpm for 12 min, then add phenoxyethanol and ethylhexylglycerin, adjust the pH to 4.8, add deionized water, degas under vacuum and filter through a 100-mesh sieve to obtain the final product. The remaining dosages and steps are the same as in Example 1.
[0160] Test Example 1: Effects on appearance, skin feel, sedimentation, redispersion, and active ingredient release 1. Detection method: (1) Particle size: The powders obtained from the whitening and anti-aging essence compositions prepared in Examples 1-7 and Comparative Examples 1-5 were separated, and 0.05% polysorbate 80 was added to deionized water as the dispersion medium. The mixtures were ultrasonically dispersed for 60 s to obtain the whitening and anti-aging essence composition solutions prepared in Examples 1-7 and Comparative Examples 1-5. The particle size was measured using a laser diffractometer, and the opacity was controlled within the instrument's recommended range. Each group was measured in parallel three times, and the average values of the volume references D50 and D90 were reported. Comparative Example 1 did not contain Astragalus powder, and its particle size was marked as "not applicable".
[0161] (2) Sedimentation rate: 50 mL of the whitening and anti-aging essence compositions prepared in Examples 1-7 and Comparative Examples 1-5 were respectively placed into stoppered graduated cylinders and allowed to stand at 25±2℃. The height Ht of the upper clear layer and the total height H0 of the sample were measured at 24h and 7d respectively. Sedimentation rate (%) = Ht / H0 × 100%. If there is no obvious clear layer, it is recorded as 0.
[0162] (3) Number of redispersions: After 7 days of settling, the graduated cylinder is inverted at a frequency of about 1 time / s. Each inversion is recorded as 1 time until the bottom sediment is completely gone and visually uniform. Record the number of inversions required. If the sediment cannot be evenly dispersed after more than 20 times, it is recorded as ">20 times".
[0163] (4) Skin feel evaluation: 10 trained evaluators applied 0.10g of sample to the inner side of the forearm and evaluated it on a scale of 1-5 based on the texture, uniformity, stringiness and stickiness. The lower the score for texture and stickiness, the better, and the higher the score for uniformity, the better. The description in the table is the consensus of most evaluators.
[0164] (5) Release rate of astragalus marker components: Using astragaloside A as the marker component, 1.00 g of the whitening and anti-aging essence compositions prepared in Examples 1-7 and Comparative Examples 1-5 were weighed and placed in dialysis bags with a molecular weight cutoff of 3500 Da. The bags were immersed in 100 mL of aqueous release medium containing 20% ethanol and shaken at 32±0.5℃ and 100 rpm. Samples were taken at specified times and replenished with an equal volume of liquid. The concentration of astragaloside A was determined by HPLC. The cumulative release amount Qn at the nth sampling was Qn = CnV0 + VsΣCi; the release rate (%) was Qn / M0×100%, where Cn was the concentration of the nth sample, V0 was the total volume of the release medium, Vs was the volume of a single sampling, ΣCi was the sum of the concentrations of the previous n-1 samples, and M0 was the theoretical total amount of astragaloside A in the sample. Each group was divided into 3 parallel samples.
[0165] 2. Experimental Results Compared to Comparative Examples 1-5, the 24-hour and 7-day sedimentation rates of Examples 1-7 were both lower, with the 24-hour sedimentation rate below 2.5% and the 7-day sedimentation rate below 7.1%. The number of redispersions in Examples 1-7 was less than 10, and the release rate of the Astragalus membranaceus marker component was above 75%.
[0166] Table 3
[0167] Test Example 2: Evaluation under high temperature, low temperature, thermal cycling, centrifugation, and long-term static conditions. 1. Experimental Methods Three independent batches were prepared for each sample group. The high-temperature test involved placing the sample at 40±2℃ for 4 weeks; the low-temperature test involved placing it at 4±2℃ for 4 weeks; the thermal cycling test involved placing the sample at 4℃ for 24 hours, then transferring it to 40℃ for 24 hours, constituting one cycle, for a total of 5 cycles; the centrifugation test involved centrifugation at 25℃ and 3000 rpm for 30 minutes; and the long-term static test involved placing the sample at 25±2℃ in the dark for 12 weeks. Color, odor, precipitation, aggregation, layering, and redispersion were observed at each time point.
[0168] Viscosity was measured using a rotational viscometer after equilibration at 25±0.5℃ for 30 min, with the same rotor and rotation speed used and measured in parallel three times.
[0169] Viscosity change rate (%) = |ηt - η0| / η0 × 100%, where η0 is the initial viscosity and ηt is the viscosity after treatment. pH was measured using a calibrated pH meter, and pH change = |pHt - pH0|.
[0170] Stability determination: Stable when there is no irreversible stratification, no obvious precipitation or agglomeration, viscosity change rate not greater than 10%, and pH change not greater than 0.20; basically stable when fine sedimentation occurs but other indicators are within acceptable limits; unstable when irreversible stratification occurs, obvious coarse particles occur, or viscosity change rate is greater than 20%.
[0171] 2. Experimental Results The whitening and anti-aging essence compositions prepared in Examples 1-7 of this invention can maintain uniformity in both high-temperature and low-temperature tests, without obvious discoloration or irreversible stratification, with viscosity change rate controlled within 10% and pH change controlled within 0.10.
[0172] Table 4
[0173] Example 3: Detection of tyrosinase inhibition rate, B16 cell melanin reduction rate, ROS, MMP-1, and type I collagen content. 1. Experimental Methods Sample working solution: Weigh 1.00 g of the whitening and anti-aging essence composition prepared in Examples 1-7 and Comparative Examples 1-2, 8, 10-16 respectively, add 9.00 mL of phosphate buffer, shake at 37℃ for 2 h, centrifuge at 10000 rpm for 10 min, and sterilize the supernatant through a 0.22 μm filter membrane. For cell experiments, first determine the highest concentration with no significant cytotoxicity (cell viability not less than 90%) using the CCK-8 assay, and then conduct subsequent experiments at this concentration. Each experiment included a blank control group, a model control group, a sample group, and a positive control group, with at least 3 replicates per group, each independently repeated 3 times. The blank control group was not induced; only an equal volume of culture medium or buffer was added. The sample group was induced under the corresponding model induction conditions.
[0174] Model control group: In the tyrosinase assay, mushroom tyrosinase, L-DOPA, and an equal volume of PBS were added without adding the sample; in the B16 cell melanin assay, cells were induced with 100 nmol / L α-MSH for 48 h and then an equal volume of culture medium was added; in the ROS assay, cells were treated with 200 μmol / L H2O2 for 2 h, and then cultured for another 24 h after changing the culture medium; in the MMP-1 and type I collagen assays, human skin fibroblasts were irradiated with UVB at 20 mJ / cm² and then cultured for another 24 h after adding an equal volume of culture medium.
[0175] Positive control group: 100 μg / mL kojic acid was added for the tyrosinase test; 1 mmol / L arbutin was added for the B16 cell melanin test; 5 mmol / L N-acetylcysteine was added for the ROS test; and 1 μmol / L all-trans retinoic acid was added for the MMP-1 and type I collagen tests. All positive controls and samples were tested under the same model induction conditions and treatment time.
[0176] (1) Tyrosinase inhibition rate: Using L-DOPA as a substrate, mushroom tyrosinase and sample working solution were added, and the mixture was reacted at 37℃ for 20 min. The absorbance was measured at 475 nm. Inhibition rate (%) = [1-(A 样品 -A 样品空白 ) / (A 模型 -A 模型空白 )]×100%.
[0177] (2) Melanin reduction rate in B16 cells: B16-F10 cells were induced with α-MSH and treated with the sample for 48 h. Cells were collected, and melanin was dissolved in 1 mol / L NaOH at 80 °C. The absorbance was measured at 405 nm and corrected for total protein content. Melanin reduction rate (%) = (Mc-Ms) / Mc×100%, where Mc is the melanin content per unit protein in the model group and Ms is the melanin content per unit protein in the sample group.
[0178] (3) ROS reduction rate: Keratinocytes or fibroblasts were subjected to oxidative stress or UV induction, and DCFH-DA probe was added after sample treatment. The fluorescence intensity was measured. ROS reduction rate (%) = (Fc-Fs) / Fc×100%, where Fc is the fluorescence intensity of the model group and Fs is the fluorescence intensity of the sample group.
[0179] (4) MMP-1 reduction rate and type I collagen increase rate: Human skin fibroblasts were induced by UVB and cultured in the sample for 24-48 h. The contents of MMP-1 and type I collagen in the culture supernatant were measured by ELISA. MMP-1 reduction rate (%) = (Cc-Cs) / Cc×100%; type I collagen increase rate (%) = (Cs-Cc) / Cc×100%, where Cc is the content of the model group and Cs is the content of the sample group.
[0180] 2. Experimental Results Table 5
[0181] Test Example 4: Comprehensive evaluation of skin brightening index, anti-aging index, and stability. 1. Experimental Methods To eliminate dimensional differences among different test items, the corresponding test value of Comparative Example 10 (blank efficacy matrix) was set to 0 points, and a preset target value of 100 points was used for linear dimensionless normalization. The preset target values for each item were: tyrosinase inhibition rate 80%, melanin reduction rate 60%, ROS reduction rate 70%, MMP-1 reduction rate 60%, and type I collagen increase rate 60%. For the above positive indicators, the single-item standardized score S_i = (X_i - X_0) / (X_t - X_0) × 100%, where X_i is the test result of the sample to be evaluated, X_0 is the test result of Comparative Example 10, and X_t is the corresponding preset target value; S_i is counted as 0 when it is less than 0 and as 100 when it is greater than 100. In this paper, Si only represents the single-item standardized score and is not the same parameter as the stability comprehensive score S.
[0182] Skin brightening index B = 0.50 × S_i (tyrosinase) + 0.50 × S_i (melanin); Anti-aging index A = 0.34 × S_i (ROS) + 0.33 × S_i (MMP-1) + 0.33 × S_i (type I collagen).
[0183] The overall stability score S consists of six components: appearance, thermal cycling, centrifugation, viscosity, pH, and redispersibility. S = (Sappearance + Sthermal cycling + Scentrifugation + Sviscosity + SpH + Sredispersibility) / 6. Appearance, thermal cycling, and centrifugation are scored as follows: no abnormalities, reversible minor abnormalities, obvious but recoverable abnormalities, and irreversible stratification or obvious agglomeration, respectively, at 100, 70, 40, and 0 points. Viscosity change rate ≤10% is scored at 100 points, >10%-20% at 70 points, and >20% at 0 points. pH change ≤0.20 is scored at 100 points, >0.20-0.40 at 70 points, and >0.40 at 0 points. Redispersibility count ≤5 times is scored at 100 points, 6-10 times at 70 points, 11-20 times at 40 points, and >20 times at 0 points. Samples without powder and without precipitation receive 100 points for redispersibility. S≥95 indicates "excellent stability", 85≤S<95 indicates "good stability", 70≤S<85 indicates "basically stable", and S<70 indicates "poor stability".
[0184] 2. Experimental Results Table 6
[0185] Test Example 5: Stability Test 1. Experimental Methods Three independent batches were prepared for each sample group. After sample preparation, the initial appearance was observed after standing at 25±2℃ for 24 hours. The sedimentation rate, redispersion times, and release rate of Astragalus marker components were determined according to the method of Test Example 1. The samples were placed at 40±2℃ for 4 weeks and centrifuged at 25℃ and 3000rpm for 30 min according to the method of Test Example 2. The sedimentation rate after 4 weeks of placement at 40℃ and the stratification after centrifugation were recorded. The D90 was measured by laser diffractometer before and after treatment. The D90 change rate (%) = |D90t-D900| / D900×100%, where D900 is the initial D90 and D90t is the D90 after treatment. The average value of the three independent batches was taken as the result.
[0186] The comprehensive score W for process stability is calculated as the arithmetic mean of the scores of seven items: initial appearance, 7-day sedimentation rate, sedimentation rate after 4 weeks of storage at 40℃, stratification after centrifugation, number of redispersions, D90 change rate, and release rate of marker components. That is, W = (S initial appearance + S 7-day sedimentation + S 40℃ sedimentation + S centrifugation + S redispersion + D90 + S release) / 7. Initial appearance is scored as follows: uniform and fine (100 points); slight powdery texture or slight viscosity / change in color and odor (70 points); poor uniformity or visible slight coarse particles (40 points); irreversible stratification (0 points). 7-day sedimentation rates are scored as follows: ≤7%, >7%-10%, >10%-15%, >15%-20%, >20% (100, 80, 60, 40, 0 points respectively). Sedimentation rates after 4 weeks at 40℃ are scored as follows: ≤10%, >10%-15%, >15%-20%, >20%-30%, >30% (100, 80, 60, 40, 0 points respectively). No stratification after centrifugation (100 points); no obvious stratification or a small amount that can be shaken (100 points). 70 points for fine sedimentation, 40 points for slight stratification, and 0 points for obvious or irreversible stratification; 100 points for redispersion times ≤5, 70, 40, and 0 points for 6-10, 11-20, and >20 respectively, and 100 points for no powder and no sediment; 100 points for D90 change rate ≤5%, >5%-10%, >10%-15%, >15%-20%, and >20% respectively; 100 points for marker component release rate ≥80%, 70%-<80%, 60%-<70%, 40%-<60%, and <40% respectively.
[0187] This test does not consider the feeding temperature as an independent variable; all samples were added with the active ingredient at 35±2℃ and stirred until completely dissolved, and the astragalus powder pre-dispersion was incorporated into the main system at 30±2℃ to reduce the risk of 3-O-ethyl ascorbic acid discoloration and powder agglomeration due to heat.
[0188] 2. Experimental Results Table 7
[0189] Test Case 6: Human Efficacy Evaluation 1. Experimental Methods (1) Subjects and Usage Method: Thirty subjects with dull skin tone, uneven skin tone, mild fine lines, roughness, or decreased elasticity were selected. A self-controlled evaluation of the whitening and anti-aging essence composition prepared in Example 1 was conducted before and after use. Subjects used approximately 0.50g of the whitening and anti-aging essence prepared in Example 1 twice daily, morning and evening, after cleansing their faces, for 8 consecutive weeks. Other functional skincare products were discontinued 24 hours before the test. Testing was conducted before use, at 2 weeks, 4 weeks, and 8 weeks.
[0190] (2) Test environment: After cleaning their face, the subjects sat quietly for 30 minutes in an environment with a temperature of 20±2℃ and a relative humidity of 50±10%, and then measured the same fixed area of the face. Each instrument measured the same subject and the same area three times in a row and took the average value.
[0191] (3) Skin brightness and melanin: L was measured using a skin colorimeter. Value, L Change = Lt - L0; MI is measured using a melanin testing probe, and the MI change rate (%) = (MIt - MI0) / MI0 × 100%.
[0192] (4) Skin tone uniformity: L was measured at 5 fixed points on the cheek. Value and calculate the standard deviation SD. Evenness improvement rate (%) = (SD0 - SD0) t ) / SD0×100%. Skin gloss was measured using a gloss meter, and the change rate (%) = (G) / SD0×100%. t -G0) / G0×100%.
[0193] (5) Fine lines and roughness: The area of fine lines and roughness parameters of a fixed area were analyzed using standardized facial images or skin contour imaging systems; the rate of change of fine line area (%) = (A t -A0) / A0×100%.
[0194] (6) Skin elasticity: R2 (Ua / Uf, representing the overall elasticity of the skin) was measured using a skin elasticity tester, and R2 was used as the only elasticity evaluation parameter in this test; R2 change rate (%) = (R2t-R20) / R20×100%, where R20 is the R2 before use and R2t is the R2 at the corresponding follow-up time point.
[0195] (7) Subjective satisfaction and safety: Satisfaction was rated on a 5-point scale, with 1 point being very dissatisfied, 2 points being dissatisfied, 3 points being neutral, 4 points being satisfied, and 5 points being very satisfied; Satisfaction (%) = Number of people who scored 4-5 points / Total number of people × 100%. Each follow-up visit recorded adverse reactions such as stinging, itching, erythema, and papules, as well as their duration, severity, and correlation with the sample.
[0196] The subjects, usage methods, testing environment, detection indicators, and calculation methods described above shall be implemented in accordance with the protocol described in this test example.
[0197] The detection indicators include skin brightness (L). Values, melanin index (MI), skin tone evenness, skin radiance, fine line area, skin roughness, elasticity parameter (R2), subjective satisfaction, and adverse reactions.
[0198] For specific testing methods and calculation formulas, see items (2)-(7) above.
[0199] 2. Experimental Results Table 8
[0200] Test Example 7: Mildness and Safety Evaluation 1. Experimental Methods The sample dosage, application time, observation time points, scoring criteria, and overall irritation index calculation methods for human closed patch testing shall be implemented in accordance with the above-mentioned scheme.
[0201] 2. Experimental Results Thirty healthy subjects were selected for a human patch test. 0.020 g of the whitening and anti-aging essence composition prepared in Example 1 was placed in a patch applicator with a diameter of approximately 8 mm and applied to the back or inner forearm for 24 hours; a blank white patch applicator was also used as a control. Erythema, edema, papules, itching, and burning sensation were observed at 0.5 h, 24 h, and 48 h after removal.
[0202] Objective skin reactions are rated on a scale of 0-4: 0 points, no reaction; 1 point, barely visible mild erythema or edema; 2 points, clearly visible erythema, edema, or a few papules; 3 points, obvious erythema and edema with dense papules or vesicles; 4 points, severe erythema, edema, vesicles, or erosion. Subjective itching / burning sensation is rated on a scale of 0-3: 0 points, none; 1 point, mild; 2 points, moderate; 3 points, obvious.
[0203] The overall stimulation index is calculated as Σ (highest objective response score for each subject at each observation time point) / number of subjects. An overall stimulation index ≤ 0.20 is considered essentially no stimulation, > 0.20-0.50 is considered mild stimulation, > 0.50-1.00 is considered moderate stimulation, and > 1.00 is considered significant stimulation.
[0204] Table 9
[0205] Finally, it should be noted that the above content is only used to illustrate the technical solution of the present invention, and is not intended to limit the scope of protection of the present invention. Simple modifications or equivalent substitutions made by those skilled in the art to the technical solution of the present invention do not depart from the essence and scope of the technical solution of the present invention.
Claims
1. A whitening and anti-aging essence composition containing whole Astragalus membranaceus powder, characterized in that, The composition, by weight percentage, includes the following components: 0.50-1.50% Astragalus membranaceus powder, 2.50-4.00% nicotinamide, 0.30-0.80% 3-O-ethyl ascorbic acid, 0.05-0.12% adenosine, 0.10-0.30% ectoine, 0.20-0.60% panthenol, 3.00-7.00% glycerin, 4.00-8.00% butylene glycol, 0.03-0.08% sodium hyaluronate, 0.12-0.24% carbomer, 0.06-0.15% xanthan gum, 0.03-0.08% disodium EDTA, 0.40-0.90% preservative system, and 0.10-0.25% pH adjuster; the whitening and anti-aging essence composition also requires the addition of water to bring the total to 100%.
2. The whitening and anti-aging essence composition according to claim 1, characterized in that, The Astragalus membranaceus powder has a D50 of 6-10 μm, a D90 of no more than 30 μm, and a maximum particle size of no more than 45 μm.
3. The whitening and anti-aging essence composition according to claim 1, characterized in that, The corrosion protection system, by mass percentage, includes 0.40-0.70% phenoxyethanol and 0.05-0.25% ethylhexylglycerin.
4. The whitening and anti-aging essence composition according to claim 1, characterized in that, Based on the mass of Astragalus membranaceus powder as 1 part, the mass ratio of Astragalus membranaceus powder, nicotinamide, 3-O-ethyl ascorbic acid, adenosine, ectoine and panthenol is 1:(3.60-4.00):(0.50-0.70):(0.08-0.12):(0.15-0.30):(0.30-0.60).
5. The whitening and anti-aging essence composition according to claim 1, characterized in that, The pH adjuster is selected from one or more of sodium hydroxide, arginine, tromethamine, and triethanolamine.
6. A method for preparing the whitening and anti-aging essence composition according to any one of claims 1-5, characterized in that, Includes the following steps: S1. Pre-wet and disperse the whole Astragalus powder with 1.50-2.50% glycerol and 2.00-3.50% butanediol by mass of the total composition to obtain a pre-dispersion of Astragalus powder; S2. Mix the remaining glycerol, butanediol, disodium EDTA, and water, then add carbomer and xanthan gum to hydrate and obtain a hydrogel suspension matrix. S3. Add nicotinamide, 3-O-ethyl ascorbic acid, adenosine, ectoine, panthenol and sodium hyaluronate to the hydrogel suspension matrix and stir to dissolve to obtain the main system solution. S4, add the pre-dispersed Astragalus powder to the main system solution, shear it, add it to the preservative system, adjust the pH, add water, degas and filter to obtain the final product.
7. The preparation method according to claim 6, characterized in that, The preparation method of Astragalus membranaceus powder in step S1 is as follows: After drying the Astragalus membranaceus slices, coarsely pulverize them, then perform ultrafine pulverization. After ultrafine pulverization, classify the particles and return the coarse particles to the ultrafine pulverization step for recycling. Collect the whole Astragalus membranaceus powder with a D50 of 6-10μm, a D90 of no more than 30μm, and a maximum particle size of no more than 45μm.
8. The preparation method according to claim 6, characterized in that, The shearing rate in step S4 is 3000-8000 rpm, and the shearing time is 8-20 min.
9. The preparation method according to claim 6, characterized in that, The pH value mentioned in step S4 is 5.4-5.
9.
10. The use of the whitening and anti-aging essence composition according to any one of claims 1-5 in the preparation of a non-therapeutic topical skin care product, characterized in that, The topical skin care products are serums, ampoules, gels, lotions, mask essences, or freeze-dried compound solutions, and are used to improve dull skin, brighten skin tone, improve uneven skin tone, improve skin radiance, reduce fine lines or wrinkles, improve skin elasticity, improve skin firmness, or improve the rough appearance caused by photoaging.
Citation Information
Patent Citations
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CN107411982A
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