Anti-initial-aging face cream composition with liquid crystal emulsification effect and preparation method of anti-initial-aging face cream composition
By using specific emulsifiers and natural active ingredients in the anti-aging face cream, a stable liquid crystal structure is formed, solving problems such as liquid crystal instability and high irritation, and achieving multi-target synergistic anti-aging effect and excellent skin feel.
Patent Information
- Application Number
- CN202511550919.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-10-28
- Publication Date
- 2025-12-12
AI Technical Summary
Existing anti-aging products often have unstable liquid crystal structures, high irritation, and limited efficacy, failing to effectively coordinate the skin's defense, repair, and regeneration functions. Furthermore, traditional emulsifiers can easily cause skin sensitivity and dryness.
Using emulsifiers such as polyglycerol-10 stearate and polyglycerol-5 oleate, combined with ingredients such as 7-dehydrocholesterol and cetearyl alcohol, a stable liquid crystal structure is formed through the PIT phase transition method. It is also formulated with natural active ingredients such as calendula extract and raspberry leaf extract to synergistically regulate skin function.
It achieves a stable liquid crystal structure, provides a refreshing and non-sticky skin feel, has a multi-target synergistic anti-aging effect, enhances the synergistic effect of active ingredients, reduces skin irritation, and is suitable for long-term use.
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Abstract
Description
Technical Field
[0001] This invention relates to the field of cosmetic technology, and in particular to an anti-aging face cream composition with liquid crystal emulsification effect and its preparation method. Background Technology
[0002] As average human lifespan increases, people's pursuit of healthy and youthful skin is growing, giving rise to the concept of "long-lasting skin." This concept emphasizes a systematic, long-term management strategy that intervenes in the aging process from multiple dimensions and targets. Early aging, as the initial sign of skin aging, specifically refers to the early self-perception of facial skin aging in Asian individuals aged 25-34, mainly manifested as rough, dull skin, uneven skin tone, and dryness with fine lines.
[0003] Traditional anti-aging products have the following problems: First, most products use high concentrations of a single active ingredient, such as high concentrations of niacinamide, peptides, or ergothioneine. This "intensive" approach is not suitable for young skin because young skin does not lack function, but rather has insufficient coordination of functions. Second, traditional emulsification systems use irritating emulsifiers such as PEG-40 stearate and glyceryl stearate, which can damage the lipid structure of the stratum corneum, leading to sensitivity and dryness with long-term use. Third, the addition of highly occlusive thickeners, such as behenol and C20-24 alkyl polydimethylsiloxane, not only fails to synergize with active ingredients but also reduces the effectiveness of the active ingredients and results in an unpleasant skin feel.
[0004] Liquid crystal emulsification technology, mimicking the lipid arrangement of cells in living organisms, significantly enhances skin compatibility. The multilayered gel network of lyotropic liquid crystals can bind a large amount of water, effectively reducing skin problems caused by long-term cosmetic use. Cubic and hexagonal liquid crystals simultaneously possess hydrophilic and lipophilic layers, providing a better skin feel and improved synergistic effects of water-soluble and oil-soluble active ingredients. However, the formation of liquid crystal structures is influenced by various factors and is difficult to maintain stable long-term existence in complex cosmetic systems; this remains a pressing technical challenge for the industry.
[0005] While some patents exist regarding liquid crystal emulsion compositions, such as CN103494714A which discloses an emulsifier composition capable of forming a liquid crystal structure, these primarily use hydrogenated lecithin, alkyl glycosides, and sucrose esters as emulsifiers. Furthermore, some patents, such as CN103494718B which discloses liquid crystal emulsifier compositions and preparation methods, along with their applications in cosmetics, while providing a basic liquid crystal structure, still fall short in terms of stability, skin feel, and synergistic effects with active ingredients. Particularly for the specific effect of anti-aging, existing technologies have failed to provide a comprehensive solution that can both form a stable liquid crystal structure and coordinate skin functions at multiple targets. Summary of the Invention
[0006] To address the shortcomings of existing technologies, the purpose of this invention is to provide an anti-aging face cream composition with liquid crystal emulsification effect and its preparation method, thereby solving problems such as unstable liquid crystal structure, high irritation, and limited efficacy in existing technologies.
[0007] The above-mentioned objective of this invention is achieved through the following technical solutions:
[0008] This invention provides an anti-aging face cream composition with liquid crystal emulsification effect, comprising the following components by weight percentage: 85-95% liquid crystal emulsification composition; 5-15% anti-aging active ingredient composition; wherein the liquid crystal emulsification composition includes emulsifier, thickener, oil, preservative and solvent.
[0009] According to one embodiment of the present invention, the liquid crystal emulsion composition comprises, by weight percentage: 1.5-2.5% polyglycerol-10 stearate and / or polyglycerol-5 oleate; 0.05-0.1% 7-dehydrocholesterol; 2-3% cetearyl alcohol; 1.0-1.2% hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer; 3.0% cetyl ethylhexanoate; 2.5% triglycerides; 2.0% isododecane; 2.0% polydimethylsiloxane; 0.2-1% jojoba seed oil; 3-6% glycerol; 68-82% water; and 0.6-1% preservative.
[0010] According to one embodiment of the present invention, the preservative is a mixture of capryloyl hydroxamic acid, ethylhexylglycerin, pentylene glycol and caprylyl glycol.
[0011] According to one embodiment of the present invention, the anti-aging active ingredient composition comprises, by weight percentage: 0.28-1.12% Calendula officinalis extract; 0.42-0.84% Raspberry leaf extract; 0.2-1% Laminaria japonica extract; 0.5-1% sodium DNase; 0.66-2% Kale leaf extract; 0.05-0.2% Laminaria japonica extract; 1-2% Lycopodium clavatum extract; and 2.0-5.0% Butylene glycol.
[0012] According to one embodiment of the present invention, the sodium DNA comprises wheat germ extract and carrageenan extract, forming a spherical DNA structure that facilitates skin penetration.
[0013] The present invention also provides a method for preparing the anti-aging face cream composition with liquid crystal emulsification effect according to the above embodiments, comprising the following steps:
[0014] Step S1: Preparation of Phase A: Mix water, glycerol and hydroxyethyl acrylate / sodium acryloyl dimethyl taurate copolymer, heat to 75°C, and homogenize at 5000-6000 rpm for 5 minutes;
[0015] Step S2, Preparation of Phase B: Polyglycerol-10 stearate and / or polyglycerol-5 oleate, cetyl ethylhexanoate, triglyceride, isododecane, polydimethylsiloxane, jojoba seed oil, cetearyl alcohol and 7-dehydrocholesterol are mixed and heated to 82°C until completely dissolved.
[0016] Step S3: Add phase B to phase A and homogenize at 80±2℃ and 5000-6000 rpm for 3 minutes. Then cool down to 70±2℃ and continue homogenizing at 5000-6000 rpm for 3 minutes.
[0017] Step S4: Cool to 45°C, add preservative, and homogenize at 3000-4000 rpm for 1 minute;
[0018] Step S5: Cool to room temperature and age to obtain liquid crystal emulsion composition.
[0019] The present invention also provides a method for preparing the anti-aging face cream composition with liquid crystal emulsification effect according to the above embodiments, comprising the following steps:
[0020] Step A1: Preparation of Phase A: Mix water, butanediol, glycerol and hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, heat to 75°C, and homogenize at 5000-6000 rpm for 5 minutes;
[0021] Step A2, Preparation of Phase B: Mix polyglycerol-10 stearate and / or polyglycerol-5 oleate, cetyl ethylhexanoate, triglyceride, isododecane, polydimethylsiloxane, jojoba seed oil, cetearyl alcohol and 7-dehydrocholesterol, and heat to 82°C until completely dissolved;
[0022] Step A3: Add phase B to phase A, and homogenize at 80±2℃ and 5000-6000 rpm for 3 minutes. Then cool down to 70±2℃ and continue homogenizing at 5000-6000 rpm for 3 minutes.
[0023] Step A4: Cool to 45°C, add anti-aging active ingredients and preservatives, and homogenize at 3000-4000 rpm for 1 minute;
[0024] Step A5: Cool to room temperature and age to obtain an anti-aging face cream composition with liquid crystal emulsification effect.
[0025] According to one embodiment of the present invention, the PIT phase transition method is used to form an O / W type liquid crystal emulsion structure below 72°C by utilizing the HLB value changes of polyglycerol-10 stearate and polyglycerol-5 oleate at different temperatures.
[0026] The present invention also provides the application of a liquid crystal emulsion composition in the preparation of anti-aging cosmetics, wherein the liquid crystal emulsion composition is formulated according to the above-mentioned proportions.
[0027] The present invention also provides the application of an anti-aging active ingredient composition in the preparation of anti-aging cosmetics, wherein the anti-aging active ingredient composition is formulated according to the above-mentioned proportions.
[0028] In summary, compared with the prior art, the present invention has at least one of the following beneficial technical effects:
[0029] 1. Stable liquid crystal structure: Through a special emulsifier ratio and PIT preparation process, the liquid crystal structure formed is stable for more than 6 months and exhibits a complete Maltese cross shape under a polarizing microscope.
[0030] 2. Multi-target anti-aging mechanism:
[0031] Regulation of intracellular defense functions: Calendula extract helps resist genomic instability and epigenetic changes by regulating epigenomic methylation, enhancing the expression of miR-199-5p and miR-424-5p, and limiting histone H3K9 methylation; Raspberry leaf extract assists in DNA damage repair and delays cell aging and mitochondrial dysfunction by scavenging free radicals in mitochondria and enhancing the activities of glutathione peroxidase, thioredoxin peroxidase and superoxide dismutase.
[0032] Regulation of extracellular repair function: Laminaria palmata extract increases Sirtuins protein expression, especially SIRT3 expression by 37%, which helps repair the low-quality extracellular matrix (ECM) secreted by fibroblast populations; Sodium DNA inhibits the expression of TNF-α, IL-6 and MMP-1 by suppressing the aging-associated secretory phenotype (SASP), enhances macrophage uptake capacity, repairs damage caused by chronic inflammation, and prevents the occurrence of potential wrinkles and fine lines.
[0033] Skin regeneration regulation: Kale leaf extract and bladderwort extract promote the self-renewal of epidermal and dermal cells, increase the synthesis of chondroitin sulfate and hyaluronic acid, improve dullness, roughness and dryness of the skin, and maintain the firmness and plumpness of the skin.
[0034] 3. Excellent skin feel and compatibility: The liquid crystal emulsion system provides a refreshing and non-sticky skin feel, reduces irritation, and avoids skin sensitivity and dryness caused by long-term use.
[0035] 4. Synergistic effect of active ingredients: The liquid crystal structure contains both hydrophilic and lipophilic layers, providing an ideal carrier for water-soluble and oil-soluble active ingredients and enhancing the synergistic effect of the ingredients.
[0036] This invention discloses an anti-aging face cream composition with liquid crystal emulsification effect and its preparation method. The composition includes emulsifiers (such as polyglycerol-10 stearate and / or polyglycerol-5 oleate, 7-dehydrocholesterol), thickeners, oils, solvents, and preservatives, as well as various natural active ingredients (such as calendula extract, raspberry leaf extract, sodium DNase, etc.). Prepared via the PIT phase transition method, it forms a stable and ordered liquid crystal structure with an effective shelf life exceeding 6 months. This face cream coordinates the skin's defense, repair, and regeneration functions, achieving anti-wrinkle, moisturizing, antioxidant, and skin brightening effects, while reducing irritation and improving skin feel, making it suitable for long-term use. The preparation method is simple, the face cream has a refreshing texture, and the active ingredients exhibit strong synergistic effects.
[0037] The key technology of this invention lies in the PIT (phase transition temperature) phase transition method, utilizing the changes in emulsifying properties of polyglycerol-10 stearate (higher HLB value) and polyglycerol-5 oleate (lower HLB value) at different temperatures. Above 72°C, the hydrogen bond network between the polyglycerol chains and water molecules in polyglycerol-10 stearate is disrupted, exposing hydrophobic regions and forming a W / O type emulsion. Below 72°C, the polyglycerol chains in polyglycerol-5 oleate fully extend, forming a dense hydrated layer and producing an O / W type emulsion. This phase transition process provides sufficient time and motive force for the emulsifier molecules to rearrange themselves in an orderly manner. Combined with the insertion of 7-dehydrocholesterol and cetearyl alcohol into the layered liquid crystal structure, this enhances the bending arrangement of the interfacial film, thereby spontaneously forming a regular, multilayered, and stable liquid crystal structure. Attached Figure Description
[0038] Figure 1 This is a flowchart of the test method for testing the antioxidant performance of Test Example 1 of the present invention.
[0039] Figure 2 This is a data analysis graph showing the test results of the moisturizing performance test of Experiment Example 1 of the present invention.
[0040] Figure 3 This is a comparison chart showing the liquid crystal content of the anti-aging face creams of three embodiments of the present invention after being placed at 40°C for 1 month and 6 months. Detailed Implementation
[0041] The technical solutions in the embodiments of this application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this application, and not all embodiments. All other embodiments obtained by those skilled in the art based on the embodiments of this application without creative effort are within the scope of protection of this application.
[0042] 1. The management strategy of "skin longevity" is related to anti-aging.
[0043] "Skin longevity" emphasizes a systematic, long-term management strategy. Its core lies in slowing down the aging process through multi-dimensional, multi-target scientific interventions, satisfying people's pursuit of youthful skin, and improving their quality of life. Early aging is the first sign of skin aging, especially referring to the early self-perception of facial skin aging among Asians aged 25-34. Anti-early aging specifically refers to the methods sought by younger people to maintain youthful skin and combat early aging due to unhealthy lifestyle habits (staying up late, stress, lack of daily sun protection, etc.) and the widespread adoption of the concept of early aging. Therefore, "skin longevity" and anti-early aging are naturally strongly related in their goals. Furthermore, the anti-early aging group is young people who are increasingly aware of the importance of self-management for facial aging and are gradually developing a willingness to implement it over a longer timescale. For example, 25-year-old women are more willing to use anti-early aging products long-term, even into their 35s or 40s, after their skin has matured. This trend aligns with the management strategy of "skin longevity."
[0044] 2. The "skin longevity" anti-aging strategy differs from traditional anti-aging and is more suitable for combating early signs of aging.
[0045] Regarding "skin longevity," L'Oréal and Estée Lauder's research has shifted from improving single signs of aging to systemic, root-cause intervention. Based on key mechanisms not yet apparent in the skin's deeper layers, such as aging markers, they have launched a series of long-term anti-aging products in order to proactively slow down the cellular aging process hidden beneath the skin.
[0046] Traditional cosmetic anti-aging strategies often focus on a single ingredient or mechanism, using high concentrations of active ingredients to achieve effects such as improving sagging, moisturizing, or reducing fine lines. This usually passively enhances skin functions, such as antioxidant function, thereby improving signs of aging. It lacks a systematic approach and does not address the root cause of aging.
[0047] It's important to understand that the skin problems faced by those experiencing early signs of aging are not severe. Supplementing with high concentrations of active ingredients can actually disrupt the skin's normal regulatory processes. Young skin's defense, repair, and regeneration functions are fully developed. The cause of early signs of aging is not a deficiency in skin function, but rather an insufficient ability to coordinate the skin's systematic processes of resisting irritation, repairing damage, and regenerating properly. The correct approach is to design multi-dimensional, multi-target ingredients based on aging markers and key skin mechanisms. This involves using smaller amounts of active ingredients to fully coordinate skin function, proactively maintaining the characteristics of youthful skin (thickness, firmness, and hydration) to achieve anti-aging effects (hydrated, smooth, radiant, and firm skin).
[0048] 3. Liquid crystal systems are better suited for anti-aging, achieving synergistic effects.
[0049] While products like the Han Shu Red Waist Cream contain high-efficacy ingredients such as cyclic peptides, vitamins, and ferulic acid, their emulsification system still uses PEG-40 stearate, glyceryl stearate, and octyl dodecyl myristate—all potentially acne-causing and irritating emulsifiers that can damage the lipid structure of the stratum corneum. Long-term use can easily lead to sensitivity and dryness. Furthermore, the formula contains multiple highly occlusive thickeners, such as behenol and C20-24 alkyl polydimethylsiloxane. These fail to synergize with the active ingredients, instead reducing their effectiveness and resulting in a poor skin feel, making them unsuitable for long-term use.
[0050] The multi-layered gel network of lyotropic liquid crystals can bind a large amount of water to achieve sustained release, effectively avoiding skin sensitivity and dryness that may be caused by long-term use of cosmetics. Furthermore, the cubic and hexagonal liquid crystal phases in lyotropic liquid crystals can coexist with both hydrophilic and lipophilic layers, resulting in a better skin feel and improved synergistic effects between water-soluble and oil-soluble active ingredients. This makes them more suitable for cosmetics intended for long-term use, allowing for the addition of lower concentrations of different active ingredients to achieve synergistic effects, making them ideal for anti-aging products.
[0051] 4. Problems with liquid crystal structures and the advantages of this invention
[0052] The formation of liquid crystals is influenced by emulsifiers, thickeners, oils, and active ingredients, and requires specific preparation processes to obtain a variety of liquid crystal structures. Furthermore, liquid crystal structures typically cannot persist long-term in complex cosmetic systems; their stability is significantly affected by ionic strength, pH, temperature, and storage time. This invention, through the rational combination of emulsifiers, thickeners, oils, and active ingredients, ensures the effectiveness of active ingredients while minimizing their impact on the liquid crystal structure. It also uses less irritating emulsifiers and fewer film-forming agents to reduce effects on the skin and efficacy. Most importantly, it achieves the long-term persistence of the liquid crystal structure within the product.
[0053] In addition, in order to maintain a stable liquid crystal structure, the usual practice is to add a large amount of glycerin to maintain the stacking of laminar liquid crystals, which often affects its skin feel and may even bring a certain stickiness.
[0054] Therefore, it is particularly important to develop an anti-aging product with a liquid crystal structure, suitable for long-term use by people with early signs of aging, that fully coordinates the skin's defense, repair and regeneration functions through the appropriate combination of water-soluble and oil-soluble active ingredients, and achieves smooth skin, brightened complexion, anti-wrinkle and firming, long-lasting moisturizing, and gentle and non-irritating effects.
[0055] This invention addresses the shortcomings of the prior art by providing an anti-aging composition and its preparation method that has a liquid crystal structure, fully coordinates the skin's defense, repair, and regeneration functions, and achieves smooth skin, brightens skin tone, reduces wrinkles and firms, provides long-lasting hydration, and is gentle and non-irritating.
[0056] The technical solution adopted by this invention to solve its technical problem is: a liquid crystal emulsion composition, comprising an emulsifier, a thickener, oils, preservatives, and a solvent. The emulsifier includes: polyglycerol-10 stearate and / or polyglycerol-5 oleate, 7-dehydrocholesterol; the thickener includes cetearyl alcohol, hydroxyethyl acrylate / sodium acryloyl dimethyl taurate copolymer; the oil includes cetyl ethylhexanoate, glyceryl tri(ethylhexanoate), isododecane, polydimethylsiloxane, and jojoba seed oil; the solvent includes glycerol and water; and the preservatives include capryloyl hydroxamic acid, ethylhexylglycerin, pentylene glycol, and caprylyl glycol.
[0057] Polyglycerol-10 stearate and / or polyglycerol-5 oleate were sourced from Sun Chemical Company.
[0058] Cetyl ethylhexanoate, glyceryl tri(ethylhexanoate), cetearyl alcohol and isododecane were sourced from BASF.
[0059] The polydimethylsiloxane was sourced from KCC Beauty.
[0060] Jojoba seed oil is sourced from Isabel Biotechnology Co., Ltd.
[0061] Dehydrocholesterol was sourced from EVONIK.
[0062] Glycerin and hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer were sourced from Seppic.
[0063] The water is produced in our own laboratory.
[0064] Polyglycerol-10 stearate (and / or) polyglycerol-5 oleate (1.5-2.5%): This is the primary emulsifier and the core of liquid crystal formation. Polyglycerol emulsifiers are nonionic emulsifiers with multiple hydrophilic hydroxyl heads and long-chain hydrophobic tails. Their molecules are relatively large and have significant steric hindrance. At the oil-water interface, they cannot arrange themselves tightly like traditional small-molecule emulsifiers. Instead, they spontaneously bend and entangle, forming complex layered, cubic, or hexagonal liquid crystal structures. This structure greatly improves the stability of the emulsion and provides a non-sticky feel.
[0065] 7-Dehydrocholesterol (0.05-0.1%): This is a co-emulsifier and liquid crystal promoter. 7-Dehydrocholesterol is a precursor to vitamin D and is also a sterol. Sterol molecules have a flat, rigid structure that can be inserted into the layered structure of liquid crystals along with the main emulsifier (polyglycerol ester) and higher alcohols (cetearyl alcohol), acting like "wedges" and oriented through a dipole effect. This helps distribute and consolidate the layered liquid crystal arrangement, resulting in a more abundant, denser, and more stable liquid crystal structure.
[0066] Cetyl ethylhexanoate, glyceryl tri(ethylhexanoate), and isododecane (7.5% total): These are moderately polar to non-polar emollients. They can be encapsulated in regions formed by the hydrophobic tails of the emulsifier. Their addition can regulate the fluidity and interlayer spacing of the liquid crystal layer, preventing the overall structure from becoming too rigid and brittle, maintaining appropriate flexibility, and thus achieving a smooth, non-sticky application feel.
[0067] Polydimethylsiloxane (2.0%): This is a non-polar, high molecular weight emollient. It is also present in the hydrophobic region, providing a refreshing, silky feel, reducing whitening after application, and helping to enhance the spreadability of the emulsion.
[0068] Jojoba (Simondia chinnsis) seed oil (0.2-1%): Jojoba oil is actually a liquid wax ester with a structure similar to human sebum, making it very stable. As an active emollient integrated into the liquid crystal structure, it effectively imparts a moisturizing feel to the emulsion, preventing dryness after water evaporation.
[0069] Cetearyl alcohol (2-3%): This is an important thickener and liquid crystal promoter. Higher alcohols (C16-C18) have a strong synergistic effect with the main emulsifier and sterols (7-dehydrocholesterol). Their long straight-chain alkane structures can be well inserted into and parallel to the hydrophobic layer of the emulsifier, greatly enhancing the thickness, strength, and stability of the liquid crystal structure, while providing the emulsion with consistency and a substantial texture.
[0070] Hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer (1.0-1.2%): This is a high-molecular-weight polymer thickener. In the aqueous phase, it forms a three-dimensional network structure through hydrogen bonding and other interactions. This network can "encapsulate" and "fix" the already formed liquid crystal particles, slowing down their aggregation or destruction due to Brownian motion. This significantly improves the static stability of the system macroscopically (preventing water and oil seepage), and it also exhibits extremely short rheological properties, high viscosity, high ionic resistance, and high shear resistance, making it ideal for increasing the stability of liquid crystal structures.
[0071] Water (70-80%) and glycerol (3-6%): Water is the continuous phase and the basis for constructing liquid crystal structures. Water molecules are sandwiched between each layer of the lamellar liquid crystal. Glycerol is an excellent co-solvent; it is soluble in water and can change the polarity of the aqueous phase, helping the emulsifier to hydrate better (dissolve and spread its hydrophilic head groups). This is crucial for the emulsifier to fully perform its function and form a stable liquid crystal structure. The presence of glycerol makes the aqueous phase more buffering against environmental changes (such as temperature and humidity), resulting in a more stable liquid crystal structure.
[0072] The technical solution adopted by the present invention to solve its technical problem based on the liquid crystal emulsion composition is: an anti-aging face cream composition, which is composed of active ingredients and excipients. The active ingredients include calendula extract, raspberry leaf extract, sodium DNA, palmate kelp extract, bladderwort extract, European schist extract, kale leaf extract, 7-dehydrocholesterol, and emollients.
[0073] Calendula flower extract is sourced from Silab and comprises 3.55 wt% calendula flower extract.
[0074] The raspberry leaf extract was sourced from Solabia and comprised 1.19 wt% raspberry leaf extract by weight.
[0075] The palmate kelp extract was harvested from Codif and contains 1 wt% palmate kelp extract by weight.
[0076] Sodium DNA is sourced from Dongfang Miaosen Company and comprises, by weight percentage, 0.5-3 wt% sodium DNA, 0.1-1.5 wt% wheat germ extract, and 0.1-1 wt% Carrageenan extract.
[0077] 7-Dehydrocholesterol was sourced from EVONIK and comprised 100 wt% 7-dehydrocholesterol.
[0078] The kale leaf extract is sourced from Solabia and comprises 3 wt% kale leaf extract by weight.
[0079] The extract of *Paecilomyces cerevisiae* was sourced from Solabia and comprised 100 wt% of *Paecilomyces cerevisiae* extract by weight.
[0080] The European schist extract was sourced from Codif and contains 0.5 wt% European schist extract.
[0081] As the body's first line of defense, the skin is constantly subjected to various levels of stimulation, yet rarely perceived. These stimuli mainly originate from external environmental factors and internal human factors. Among external environmental factors, solar radiation (accounting for 80%) and dietary intake have the greatest impact on the skin. When the skin is continuously exposed to UV radiation, the cellular defense mechanism—epignomic regulation—becomes ineffective in resisting the stimulation, leading to methylation changes. Among internal human factors, when the skin is exposed to high levels of endogenous ROS stimulation from neuroendocrine factors (staying up late, stress) or inflammation, the cellular defense mechanism—DNA damage response—becomes ineffective in resisting the stimulation, resulting in cell cycle arrest.
[0082] The failure of cellular defense mechanisms leads to genomic instability and epigenetic alterations, resulting in reduced expression of "longevity genes" and the onset of programmed cellular senescence. Mitochondria, as the core of cellular energy supply, are particularly susceptible to dysfunction when damaged, further exacerbating cellular senescence.
[0083] When cells age, they secrete large amounts of SASP (senescence-associated secretory phenotype) outside the cell, causing premature aging of adjacent cells. At this time, the normal communication function of the cell population is disrupted, and skin damage is difficult to repair.
[0084] The extracellular matrix (ECM), as the main substance secreted by cells, undergoes reactions such as collagen oxidation, glycation, and degradation, leading to ECM alterations. The secretion of pro-inflammatory factors increases significantly, while the immune response decreases, resulting in chronic inflammation. Ultimately, the skin suffers significant damage accompanied by impaired regeneration, leading to the formation of early signs of skin aging.
[0085] Therefore, by coordinating intrinsic cellular defense functions (epigome regulation, DNA damage repair), it helps resist basal instability and epigenetic changes, thereby delaying programmed aging and mitochondrial dysfunction; by coordinating extracellular repair functions, it helps metabolize low-quality extracellular matrix (glycated, hardened collagen) secreted by senescent cell populations, and the immune response clears the secreted SASP, thereby blocking the spread of senescent cells and inhibiting chronic inflammation and ECM changes; by coordinating skin regeneration functions, it promotes the self-renewal of epidermal and dermal cells, thereby delaying the formation of early signs of skin aging.
[0086] Calendula flower extract is rich in carotene and monosaccharides and oligosaccharides between DP1 and DP10. An addition of 0.85% enhances miR-199-5P (+31%) and miR-424-5p (+38%) expression and limits histone H3K9 methylation. 0.5% EPIGENOMYL significantly reduces miR-29a (-14%) and miR-29b (-20%), promotes matrix gene expression, and increases miR-22-5P (+18%), protecting the matrix from MMP1 degradation. This molecular-level regulation of epigenomic methylation enhances cellular resilience against genomic instability and epigenetic alterations. Under simulated solar radiation (SSR) conditions, it has also been shown to significantly promote type 1 procollagen synthesis, protect the structure of elastin and fibrin 1, and effectively resist the effects of photoaging on cells.
[0087] Raspberry leaf extract is rich in ellagitannins. Even a 0.5% addition can effectively scavenge free radicals in mitochondria and enhance the body's own antioxidant defense mechanisms: it strengthens the activities of glutathione peroxidase, thioredoxin peroxidase, and superoxide dismutase. Furthermore, it can assist in various DNA damage repair pathways, ultimately breaking cell cycle arrest and delaying cellular aging and mitochondrial dysfunction.
[0088] Sirtuins are a family of seven nicotinamide adenine dinucleotide (NAD+)-dependent enzymes distributed in the cell nucleus, mitochondria, and cytoplasm, and are essential for maintaining the stability of the extracellular environment.
[0089] Laminaria japonica extract is rich in iodine-free kelp polysaccharides (500-6000 ppm), mannitol, protein, minerals, and sugars. Even a 0.5% addition significantly increases the expression of five sirtuins, particularly SIRT3 expression by 37%, helping to stretch the low-quality extracellular matrix (ECM) secreted by aging fibroblast populations. It also protects mitochondrial morphology by reducing 38% of mitochondrial membrane cytochrome C leakage, improving mitochondrial function by 22%, enhancing cellular respiration and ATP production by 42%, repairing ECM damage, and re-strengthening the ECM.
[0090] Sodium DNA, derived from salmon testes, is combined with wheat germ extract and Carrageenan extract to form a more permeable spherical DNA structure, facilitating transdermal capture by cells via A2A receptors. In this combination, a 1% sodium DNA addition effectively inhibits the initiation of chronic inflammation and blocks the spread of aging-related damage in fibroblasts by suppressing the senescence-associated secretory phenotype (SASP) and inhibiting the expression of TNF-α, IL-6, and MMP-1. It also increases the uptake of inflammatory microspheres by M0 macrophages by 96%, thus preventing the spread of aging-related damage in fibroblasts. Furthermore, by activating ErbB tyrosine kinase receptors, it enhances cell division, thereby promoting fibroblast self-renewal and repairing damage caused by chronic inflammation.
[0091] 7-Dehydrocholesterol is a precursor to vitamin D and is converted into vitamin D in the body. An addition of 0.01% can significantly reduce the secretion of pro-inflammatory M1 macrophages and increase the secretion of anti-inflammatory M2 macrophages, effectively enhancing the skin's immunity and clearance capabilities and blocking the spread of chronic inflammation. Furthermore, it can reduce the degradation of the extracellular matrix by TIMP-1 by 49%, increase the expression of type III collagen fibers by 46%, and increase the expression of type XIV and XV collagen fibers by 45%, helping to reorganize fibrous and non-fibrous extracellular matrix proteins and effectively reducing ECM alterations.
[0092] The main components of kale leaf extract are omega-3, 6, and 9 and vitamin K (phylloquinone), while the main component of schistose pine extract is schistolin. By replenishing the skin with fatty acids, clotting vitamins, and anti-glycation alkaloids that are easily lacking, they can effectively enhance the skin's metabolic capacity under high sugar, high lipid, and high pro-inflammatory stress, restoring normal ECM structure. A 1% concentration of schistose pine extract can increase the survival rate of fibroblasts under oxidative stress by approximately 86%, reduce melanin AGEs expression by 36%, and RAGE expression by 25%, thereby combating ECM glycation. A 1% concentration of kale extract can actively regulate peroxisome proliferator-activated receptor α (PPARα) / retinoid X receptor-α (RXRα), thereby limiting the accumulation of dead skin cells by 41%, helping the epidermis regenerate smoothly, and maintaining skin firmness and plumpness.
[0093] The extract of *Leptochloa crus-galli* is rich in seaweed polysaccharides. Even a 0.1% concentration of *Leptochloa crus-galli* extract can increase the expression of chondroitin sulfate in the papillary dermis by 195%, and enhance hyaluronic acid synthesis in the dermis by 25% and in the epidermis by 109%. Furthermore, it can improve the appearance and texture of the skin, tighten the skin, and delay the appearance of fine lines due to dryness.
[0094] Example 1: Preparation of Liquid Crystal Emulsion Composition
[0095] The liquid crystal emulsion composition was prepared in the following proportions: polyglycerol-10 stearate 2.0%; 7-dehydrocholesterol 0.08%; cetearyl alcohol 2.5%; hydroxyethyl acrylate / sodium acryloyl dimethyl taurate copolymer 1.1%; cetyl ethylhexanoate 3.0%; triglyceride tri(ethylhexanoate) 2.5%; isododecane 2.0%; polydimethylsiloxane 2.0%; jojoba seed oil 0.5%; glycerol 4.5%; water 79.32%; capryloyl hydroxamic acid 0.2%; ethylhexylglycerin 0.3%; pentylene glycol 0.3%;
[0096] Octyl glycol 0.2%;
[0097] The preparation method is as follows:
[0098] Add phase A (water, glycerol, hydroxyethyl acrylate / sodium acryloyl dimethyl taurate copolymer) to a container and heat to 75°C. Then, homogenize and mix at 5500 rpm for 5 minutes.
[0099] Add phase B (polyglycerol-10 stearate, cetyl ethylhexanoate, triglyceride triethylhexanoate, isododecane, polydimethylsiloxane, jojoba seed oil, cetearyl alcohol, 7-dehydrocholesterol) to another container and heat to 82°C until completely dissolved;
[0100] Add phase B to phase A and homogenize at 80°C and 5500 rpm for 3 minutes, then cool to 70°C and continue homogenizing at 5500 rpm for 3 minutes.
[0101] Cool to 45°C, add phase C (capryloyl hydroxamic acid, ethylhexylglycerin, pentylene glycol, caprylyl glycol), and homogenize at 3500 rpm for 1 minute;
[0102] Cool to room temperature and age for 24 hours.
[0103] This invention fully utilizes the emulsifying properties of polyglycerol-10 stearate (high HLB value) and polyglycerol-5 oleate (low HLB value). At temperatures above 72°C, the hydrogen bond network between the polyglycerol chains and water molecules in the higher HLB value polyglycerol-10 stearate is disrupted, exposing hydrophobic regions, resulting in a w / o emulsion. Conversely, at temperatures below 72°C, the polyglycerol chains in the lower HLB value polyglycerol-5 oleate fully extend, forming a dense hydrated layer, resulting in an o / w emulsion. Therefore, the PIT phase transition method can help the interfacial film reassemble at lower temperatures, providing sufficient time and energy for the emulsifier molecules to rearrange in an orderly manner. Combined with the insertion of 7-dehydrocholesterol and cetearyl alcohol into the multilayer structure of the lamellar liquid crystal, this helps enhance the bending arrangement of the interfacial film, thereby spontaneously forming a regular, multilayered, and stable liquid crystal structure.
[0104] Example 2: Preparation of an anti-aging face cream
[0105] The anti-aging face cream was prepared according to the following proportions: 90% liquid crystal emulsion composition (prepared according to Example 1); 10% anti-aging active ingredient composition;
[0106] The anti-aging active ingredient composition includes: 0.85% calendula extract; 0.63% raspberry leaf extract; 0.6% palmate kelp extract; 0.8% sodium DNase (containing 0.3% wheat germ extract and 0.2% chondrus crispus extract); 1.33% kale leaf extract; 0.12% *Leptochloa crus-galli* extract; 1.5% *Lycopodium clavatum* extract; and 4.17% butylene glycol.
[0107] The preparation method is as follows: prepare the liquid crystal emulsion composition according to the method of Example 1; add the above anti-aging active ingredient composition when cooling to 45°C; homogenize and mix at 3500 rpm for 1 minute; cool to room temperature and age for 48 hours.
[0108] Example 3: Preparation of an anti-aging face cream
[0109] The anti-aging face cream was prepared according to the following proportions: 85% liquid crystal emulsion composition (prepared according to Example 1); 15% anti-aging active ingredient composition;
[0110] The anti-aging active ingredient composition includes: 0.85% calendula extract; 0.63% raspberry leaf extract; 0.6% palmate kelp extract; 0.8% sodium DNase (containing 0.3% wheat germ extract and 0.2% chondrus crispus extract); 1.33% kale leaf extract; 0.12% *Leptochloa crus-galli* extract; 1.5% *Lycopodium clavatum* extract; and 4.17% butylene glycol.
[0111] The preparation method is as follows: prepare the liquid crystal emulsion composition according to the method of Example 1; add the above anti-aging active ingredient composition when cooling to 45°C; homogenize and mix at 3500 rpm for 1 minute; cool to room temperature and age for 48 hours.
[0112] Example 4: Preparation of an anti-aging face cream
[0113] The anti-aging face cream was prepared according to the following proportions: 95% liquid crystal emulsion composition (prepared according to Example 1); 5% anti-aging active ingredient composition;
[0114] The anti-aging active ingredient composition includes: 0.85% calendula extract; 0.63% raspberry leaf extract; 0.6% palmate kelp extract; 0.8% sodium DNase (containing 0.3% wheat germ extract and 0.2% chondrus crispus extract); 1.33% kale leaf extract; 0.12% *Leptochloa crus-galli* extract; 1.5% *Lycopodium clavatum* extract; and 4.17% butylene glycol.
[0115] The preparation method is as follows: prepare the liquid crystal emulsion composition according to the method of Example 1; add the above anti-aging active ingredient composition when cooling to 45°C; homogenize and mix at 3500 rpm for 1 minute; cool to room temperature and age for 48 hours.
[0116] The anti-aging face creams prepared in Examples 2, 3, and 4 were placed at 40°C for 1 month and 6 months, respectively, and their liquid crystal content was observed. Figure 3 It can be seen that the liquid crystal in Example 2 (90% liquid crystal emulsion composition + 10% anti-aging composition) is the most abundant, the liquid crystal in Example 3 (85% liquid crystal emulsion composition + 15% anti-aging composition) is almost non-existent, and the liquid crystal in Example 4 (95% liquid crystal emulsion composition + 5% anti-aging composition) is significantly reduced.
[0117] Comparative Example 1: Face Cream with Traditional Emulsification System
[0118] The emulsification system of this invention is replaced by conventional emulsifiers PEG-40 stearate and glyceryl stearate, and the other components are the same as in Example 2.
[0119] Comparative Example 2: High-concentration single active ingredient face cream
[0120] A high concentration of nicotinamide (5%) was used instead of the multi-target active ingredient combination of the present invention, and the other ingredients were the same as in Example 2.
[0121] In this invention, the anti-aging face cream prepared in Example 2 is preferably used to conduct antioxidant performance tests, anti-wrinkle performance tests, and moisturizing performance tests on the face creams of Comparative Example 1 and Comparative Example 2, respectively.
[0122] Experimental Example 1: Antioxidant Performance Test
[0123] 1. Experimental objective and principle:
[0124] Antioxidant efficacy can be characterized by evaluating the inhibition rate of DPPH free radicals in test samples. DPPH analysis is a simple method for screening free radical scavengers and evaluating antioxidant activity. DPPH in ethanol is purple, with a maximum absorption wavelength of 517 nm. When a free radical scavenger is added to the DPPH solution, its lone pairs of electrons are paired, causing the absorption to disappear or weaken, resulting in a lighter solution color, appearing yellow or pale yellow, and a decrease in absorbance at 517 nm. The degree of change is linearly related to the free radical scavenging intensity, thus allowing for quantitative analysis using spectrophotometry. This method can be expressed as a scavenging rate; a higher scavenging rate indicates a stronger scavenging ability.
[0125] 2. Scope of application and relevance:
[0126] This experimental method is an in vitro method. DPPH, a stable free radical, is used to detect free radical scavenging activity, and is suitable for evaluating cosmetic products and raw materials that claim to achieve antioxidant effects through anti-free radical action. As a supplement to the subjective and objective human evaluation method, the in vitro method is one of the in vivo antioxidant pathways, and the results of in vivo method testing of antioxidant efficacy have a certain correlation.
[0127] Through experimental design, the DPPH radical scavenging rate results of the experimental sample group and the blank group were compared. Three replicates were performed for each gradient, and the scavenging rate was calculated to derive a linear equation for the scavenging rate.
[0128] 3. Test Indicators:
[0129] Table 1 Test Indicators
[0130] Experimental indicators Judgment criteria Free radical scavenging rate The higher the scavenging rate, the stronger the ability of the substance to scavenge free radicals.
[0131] Test methods such as Figure 1 As shown in Table 2, the experimental results are as follows:
[0132] Table 2. Experimental Results
[0133]
[0134] Experimental Conclusion: Antioxidant efficacy can be characterized by evaluating the inhibition rate of DPPH free radicals by the test samples. A higher scavenging rate indicates a stronger scavenging ability. The test results for the test samples are shown in Table 2. When the sample was diluted 10 times, the free radical scavenging rate was 65.31%, while comparative samples 1 and 2 were 32.3% and 48.5%, respectively. In summary, under the experimental conditions, the test samples exhibit better antioxidant efficacy compared to existing technologies.
[0135] Experimental Example 2: Anti-wrinkle performance test:
[0136] 1. Experimental objective and principle:
[0137] This test uses UVA irradiation of fibroblasts to evaluate the anti-wrinkle efficacy of the test samples by detecting changes in type I collagen content. UV irradiation leads to the production of numerous free radicals in the skin, further inducing the excessive generation of matrix metalloproteinases, thus promoting collagen degradation. Excessive collagen degradation results in skin atrophy and wrinkles. Collagen I is type I collagen, and collagen accounts for approximately 80% of the dermis, contributing to skin plumpness and fullness. Promoting an increase in Collagen I content can help resist wrinkle formation. Therefore, this test is based on an in vitro assessment model of UVA (long-wave ultraviolet) damage to fibroblasts (HSF), evaluating the anti-wrinkle and firming effects of the test products by detecting the expression of type I collagen.
[0138] Ultraviolet A (UVA) radiation is the most penetrating band of ultraviolet light in sunlight, capable of penetrating deep into the dermis and damaging skin cells, leading to photoaging. Human skin collagen is primarily composed of type I and type III collagen. Type I collagen is mainly distributed in the dermis, its main function being to provide skin elasticity, and its levels gradually decline with age. When skin cells are exposed to ultraviolet radiation, the synthesis of type I collagen decreases or its degradation increases, resulting in signs of aging such as sagging and wrinkles. Immunofluorescence staining utilizes the specific binding of antigens and antibodies and fluorescent labeling to display the expression and localization of target proteins within cells. The fluorescence intensity of the target protein can be used to indicate its relative expression level.
[0139] 2. Test materials:
[0140] Testing system: The cells used in this test were fibroblasts (HSF), provided by Guangdong Boxi Biotechnology Co., Ltd.
[0141] Sample information: The sample was prepared by the method of Example 2 of this invention.
[0142] Main reagents: high glucose DMEM medium, trypsin, phosphate-buffered saline (DPBS), double antibodies, fetal bovine serum, MTT, Col lagen I (COL1A1) antibody, secondary antibody, EGCG, 4% paraformaldehyde, anti-aging face cream.
[0143] Main equipment: CO2 cell incubator (Yamato), fluorescence inverted microscope (Olympus), fully automated cell counter (Countstar), biosafety cabinet (Thermo Fisher Scientific), multi-functional microplate reader (Tecan), constant temperature water bath (Yiheng), pipettes, ultraviolet crosslinker.
[0144] 3. Testing Method:
[0145] 1) Cell seeding: After cell resuscitation, when the cell plating rate reaches about 60%, seed the cells into 24-well plates and incubate overnight in a CO2 incubator (37°C, 5% CO2).
[0146] 2) Solution preparation: Prepare the working solution of the test substance according to the test group (Table 3).
[0147] Table 3 Test Groups
[0148]
[0149] 3) Drug administration: According to the test groups in Table 1, when the cell deposition rate in the 24-well plate reached 30%–50%, drug administration was performed in groups, with 3 replicates per group. 1 mL of culture medium was added to each well of the blank control group and negative control group; 1 mL of culture medium containing TGF-β1 was added to each well of the positive control group; and 1 mL of culture medium containing the corresponding concentration of the test sample was added to each well of the sample group. After drug administration, the 24-well plate was placed in an incubator (37℃, 5% CO2) and incubated for 24 h.
[0150] 4) UVA irradiation: According to the test groups, except for the blank control group, all other groups were subjected to UVA irradiation with an irradiation dose of 30 J / cm². 2 After irradiation, the samples were placed in a CO2 incubator (37℃, 5% CO2) and cultured for another 24 hours.
[0151] 5) Collagen I content assay: Cells were fixed with 4% paraformaldehyde for 30 minutes. Immunofluorescence was then performed, and the staining results were observed and photographed under a fluorescence microscope. Images were collected for later use. The analysis was performed using Plus software.
[0152] 6) Calculation of improvement rate: Improvement rate (%) = (sample group - negative control group) / negative control group × 100%.
[0153] 7) Statistical analysis of results: GraphPad Prism was used for plotting, and the results are expressed as Mean ± SD. t-tests were used for comparisons between groups. P < 0.05 was considered statistically significant, and P < 0.01 was considered highly statistically significant.
[0154] 4. Test Results:
[0155] Compared with BC, the content of Col lagen I in the NC group decreased significantly by 50.03% (p<0.05), indicating that the stimulation conditions in this test were effective.
[0156] Compared with NC, the content of Col lagen I in the PC group increased significantly by 163.66% (p<0.05), indicating that the positive control in this test was effective.
[0157] Compared with NC, after treatment with 0.03 mg / mL anti-aging cream for 72 h, the content of Collagen I significantly increased, and the content of type I collagen in HSF cells increased by 163.66% (p<0.05). In contrast, the content of type I collagen in HSF cells in comparative examples 1 and 2 increased by 88.7±4.25% and 95.6±5.12%, respectively (p<0.05). In conclusion, under the conditions of this experiment, the test sample exhibits better anti-wrinkle and firming effects compared to existing technologies.
[0158] Experiment 3: Moisturizing performance test:
[0159] 1. Purpose and principle of the experiment: To evaluate the efficacy claims of the sample by measuring the objective changes in the skin indicators of subjects before and after using the sample.
[0160] 2. Sample information is shown in Table 4:
[0161] Table 4
[0162]
[0163] 3. Experimental Design:
[0164] This randomized, blinded, controlled trial was conducted on the inner forearm. Skin parameters were measured in the sample and control areas before sample application (D0-BL) and 4 hours after sample application (D0-T4h). Statistical analysis was performed on the data to evaluate the efficacy claims of the sample. Trial type: randomized, single-blind, controlled trial; Control methods: self-controlled before-and-after, inter-group controlled; Control: blank control (no treatment was performed on the control area).
[0165] 4. Test Procedure:
[0166] 1) Upon arrival, participants complete check-in and basic information registration;
[0167] 2) Researchers conducted a medical history questionnaire survey on the subjects, explained the project to them, and guided the subjects to sign the "Informed Consent Form";
[0168] 3) Researchers screened eligible subjects based on the subject inclusion and exclusion criteria;
[0169] 4) Clean the inside of the forearms of the selected subjects by wiping them with a dry paper towel. The researchers marked the test area on the inside of the forearms. The sample area and control area were randomly distributed in the marked test area to ensure that the position of each area was statistically balanced. The subjects sat quietly in the rest and waiting area at a temperature of 21±1℃ and a relative humidity of 50±10% for at least 20 minutes, with the forearms exposed and kept relaxed to stabilize the skin condition of the test area.
[0170] 5) The researcher will conduct instrument testing and collect the baseline value (D0-BL) of the inner forearm;
[0171] 6) The researcher administered the solution at (2.0±0.1) mg / cm³. 2 The dosage was applied once to the sample area on the inner forearm of both hands of the subject.
[0172] 7) Subjects sat quietly in a resting and waiting area with a temperature of 21±1℃ and a relative humidity of 50±10% for 4 hours, with the inner sides of their forearms exposed and kept relaxed to stabilize the skin condition of the test area.
[0173] 8) The researcher will conduct instrument testing again and collect data 4 hours after sample use (D0-T4h);
[0174] 9) Subjects used the test samples under the guidance of researchers;
[0175] 10) Subjects complete the immediate survey questionnaire (DO-Tim).
[0176] 5. The test / evaluation items are shown in Table 5:
[0177] Table 5
[0178]
[0179]
[0180] 6. Subjects participating in the trial:
[0181] In accordance with the Declaration of Helsinki (2024) and its subsequent amendments, the Standards for Evaluating Cosmetic Efficacy Claims, and other relevant laws and regulations, this trial adheres to ethical principles. All participants voluntarily signed informed consent forms and underwent necessary medical protective measures to protect their interests to the greatest extent possible. Participants have the right to withdraw from the trial at any time for any reason. Eligible participants were screened and recruited according to inclusion and exclusion criteria.
[0182] 6.1. Inclusion criteria:
[0183] 1) Healthy female respondents aged 18-55 (excluding pregnant or lactating women); 2) Baseline values of the forearm test area using a capacitive skin moisture analyzer between 15-45 (Corneometer Unit, CU); 3) No obvious skin lesions or scars in the test area; 4) Able to cooperate well with the test according to the protocol requirements and maintain a regular lifestyle during the test; 5) Willing to participate in the test, able to read and understand all the contents of the informed consent form, and sign the informed consent form.
[0184] 6.2. Exclusion criteria:
[0185] 1) Individuals who have used antihistamines within the past week or immunosuppressants within the past month; 2) Individuals with a history of skin diseases such as psoriasis, eczema, atopic dermatitis, or severe acne, or other conditions that may affect the determination of experimental results; 3) Individuals with allergic diseases or a history of allergies to cosmetics or other topical preparations; 4) Individuals who have used anti-inflammatory drugs on the test site within the past two months; 5) Insulin-dependent diabetes mellitus patients; 6) Patients currently receiving treatment for asthma or other chronic respiratory diseases; 7) Individuals currently receiving dermatological treatment; 8) Individuals who have received anticancer chemotherapy within the past six months; 9) Patients with immunodeficiency or autoimmune diseases; 10) Breastfeeding or pregnant women, or those planning to conceive in the near future; 11) Individuals currently participating in or participating in other clinical trials within the past two months; 12) Individuals with highly sensitive constitutions; 13) Individuals who cannot complete the prescribed content according to the experimental requirements; 14) Individuals deemed unsuitable for efficacy trials by the researcher, in addition to the above.
[0186] 6.3. Restrictions:
[0187] 1) One month prior to and during the trial, participants must not use any topical medications or health products intended to improve skin that may affect the trial results, and are prohibited from undergoing massage, skin care at beauty salons, or medical treatments; 2) No special-effect products (cosmetics, skin care products) or topical medications should be used on the test site within two days prior to the test; 3) During the trial, participants should minimize intense outdoor sun exposure and avoid travel or vacations. If outdoor activities are necessary, necessary sun protection measures should be taken, such as wearing a hat, using an umbrella, and wearing sun-protective clothing; 4) During the trial, this sample should replace the same type of skin care products used daily, while other daily skin care products and habits should remain unchanged; 5) During the trial, participants should maintain good sleep habits and avoid excessive late nights.
[0188] 7. Test environment: Temperature: 20℃~22℃, Relative humidity: 40%~60%;
[0189] 8. Statistical analysis methods for experimental data:
[0190] 1) Descriptive statistics of the experimental data were performed using Excel software, including quantity, mean, standard deviation, minimum, and maximum values. 2) The differences in the experimental data were statistically analyzed using SPSS software. The Shapiro-Wilk Test was used to determine the significance of the normality of the data. If Sig.(two-tailed) > 0.05, the data were considered normally distributed, and a t-test was used for statistical analysis. If Sig.(two-tailed) < 0.05, the data were considered non-normally distributed, and a nonparametric test was used for statistical analysis. A two-tailed test was used with a significance level of α = 0.05. 3) A binomial test was used in SPSS software to analyze whether the population from which the sample came followed a binomial distribution with a specified probability p. A 2-point agreement questionnaire was used: 1 point was "agree," with a probability of p; 0 points were "disagree," with a probability of 1-p. A one-tailed test was used with a significance level of α = 0.05 and a proportion of 9.
[0191] 9. Criteria for determining the conclusion:
[0192] Moisturizing efficacy: If the change in stratum corneum moisture content in the sample area is significantly better than that in the control area after 4 hours of use (P<0.05), the test sample is judged to have a 4-hour moisturizing efficacy; otherwise, the test sample is judged not to have a 4-hour moisturizing efficacy.
[0193] 10. Experimental Results:
[0194] 10.1. Sample Completion Status
[0195] The trial was completed by 33 participants. The final statistics of the 33 participants showed that all 33 were female, aged 21 to 45 years, with a mean age of 36.1 ± 7.4 years.
[0196] 10.2. Sample usage and tolerability feedback:
[0197] Each subject used the test sample as required within the specified time. In accordance with the "Administrative Measures for Monitoring Adverse Reactions to Cosmetics" and the "Technical Specifications for Cosmetic Safety (2015 Edition)" and other relevant guidance documents, no adverse reactions were found during the test.
[0198] 10.3. Instrument test results: See Table 6; data analysis is shown in [link to table]. Figure 2 .
[0199] Table 6 Instrument Test Results
[0200]
[0201] 10.4. Questionnaire Survey Results:
[0202] The results of the questionnaire survey are shown in Tables 7 and 8:
[0203] Table 7. Statistical Table of Approval Rating Results (2-point scale)
[0204]
[0205] Table 8. Statistical Table of Approval Rating Results (out of 5 points)
[0206]
[0207]
[0208] 11. Experimental Conclusion: During the experimental period, the anti-aging face cream of the test sample had moisturizing effect. The skin moisture content was measured by a skin moisture content tester. After using the product of Example 2 for 4 hours, the skin moisture content increased by 58.7%, and after 24 hours, it still maintained an increase of 36.2%, which was significantly better than the comparative product.
[0209] Liquid crystal structure stability test: The liquid crystal emulsion composition prepared in Example 1 was observed using a polarizing microscope, showing a complete Maltese cross structure, indicating the formation of a good liquid crystal system. In an accelerated stability test at 40°C, the complete liquid crystal structure was maintained after 6 months.
[0210] Skin irritation test: Through patch test, the irritation score of the product in Example 2 was 0.32 (almost no irritation), while that of Comparative Example 1 was 1.85 (mild irritation).
[0211] The above experimental results demonstrate that the anti-aging face cream composition with liquid crystal emulsification effect provided by this invention has significant technical and market competitive advantages. The anti-aging face cream composition and its preparation method provided by this invention have clear industrial applicability, with readily available raw materials and a simple process, making them suitable for large-scale industrial production. The product exhibits good stability, excellent skin feel, and a clear anti-aging effect, meeting market demands and possessing broad application prospects.
[0212] This invention, based on a liquid crystal emulsified composition, adds an anti-aging composition to prepare an anti-aging face cream with liquid crystal emulsification effects. While ensuring the long-term existence of the liquid crystal structure, it provides a better skin feel and improved synergistic effects of water-soluble and oil-soluble active ingredients; it is less irritating and avoids skin sensitivity and dryness problems that may occur with long-term use of cosmetics. The preparation process of this invention is simple, the face cream has a refreshing and easily absorbed texture, enhances the sustained release and penetration of active ingredients, and has clear anti-wrinkle and moisturizing effects.
[0213] This invention utilizes the PIT phase transition method to prepare a stable liquid crystal structure, resulting in an effective lifespan exceeding 6 months. The liquid crystal structure is ordered and uniform, exhibiting a complete Maltese cross under a polarizing microscope. The liquid crystal emulsion structure reduces the irritation of emulsifiers and active ingredients, avoiding skin sensitivity and dryness issues that may arise from long-term cosmetic use. It provides a better skin feel and improved synergistic effects between water-soluble and oil-soluble active ingredients.
[0214] In terms of regulating the skin's defense function, calendula extract and raspberry leaf extract are added as natural active ingredients. Even with low dosage, they can restore the epigenome and repair DNA damage, which are the two inherent defense mechanisms of the skin, thereby helping cells to better resist internal and external stimuli and relieve cell cycle arrest.
[0215] In terms of regulating the skin's defense function, the addition of palmate kelp extract as a natural active ingredient can increase sirtuins protein expression at a low dosage, reduce the two major aging markers of genomic instability and epigenetic changes, thereby delaying cellular aging and mitochondrial dysfunction.
[0216] In terms of regulating skin repair function, the addition of spherical DNA sodium, 7-dehydrocholesterol and European pine extract as active ingredients can help the skin metabolize low-quality extracellular matrix at low dosages, regulate the clearance of secreted SASP by M0, M1, and M2 macrophages, block the spread of senescent cells, and thus inhibit chronic inflammation and ECM changes.
[0217] To regulate skin regeneration, kale leaf extract and bladderwort extract are added as natural active ingredients, rather than highly irritating retinol. Even at lower concentrations, these ingredients can enhance the self-renewal of epidermal and dermal cells under high pro-inflammatory stress, thereby delaying the formation of early signs of skin aging.
[0218] This invention addresses the problems caused by high concentrations of single active ingredients, irritating emulsifiers, and highly occlusive thickeners in existing anti-aging products, and proposes a novel solution—achieving multi-target coordinated skin function through liquid crystal emulsification technology. This is a problem that has not been fully recognized or technically solved in the field.
[0219] This invention employs a specific combination of emulsifiers (a blend of polyglycerol-10 stearate and / or polyglycerol-5 oleate with 7-dehydrocholesterol), combined with a PIT phase transition process, successfully solving the technical challenge of maintaining the long-term stability of liquid crystal structures in complex cosmetic systems. This specific combination and process are not conventional choices in the field, and no corresponding technical inspiration is provided in the prior art.
[0220] The face cream composition provided by this invention not only has a stable liquid crystal structure (maintained for more than 6 months), but also exhibits significantly better effects than the comparative ratio in terms of anti-oxidation, anti-wrinkle and moisturizing, while having extremely low skin irritation. These synergistic effects are beyond the expectations of those skilled in the art.
[0221] This invention achieves multi-target regulation of skin function through a carefully designed combination of active ingredients: calendula extract and raspberry leaf extract synergistically enhance the skin's defense function; kelp extract and sodium DNA synergistically enhance the repair function; and kale leaf extract and *Leptochloa crus-galli* extract synergistically enhance the regeneration function. This multi-component synergistic effect is not a simple additive effect of the individual components, but rather produces an unexpected synergistic enhancement.
[0222] The principle of this invention is as follows: This invention relates to the field of cosmetic technology, specifically to an anti-aging face cream composition with liquid crystal emulsification effect and its preparation method. The composition includes emulsifiers (such as polyglycerol-10 stearate and / or polyglycerol-5 oleate, 7-dehydrocholesterol), thickeners, oils, solvents, and preservatives, as well as various natural active ingredients (such as calendula extract, raspberry leaf extract, sodium DNase, etc.). Prepared via the PIT phase transition method, it forms a stable and ordered liquid crystal structure with an effective shelf life exceeding 6 months. This face cream can coordinate the skin's defense, repair, and regeneration functions, achieving anti-wrinkle, moisturizing, antioxidant, and skin brightening effects, while reducing irritation, improving skin feel, and making it suitable for long-term use. The preparation method is simple, the face cream has a refreshing texture, and the active ingredients have a strong synergistic effect.
[0223] The embodiments described herein are preferred embodiments of the present invention and are not intended to limit the scope of protection of the present invention. Therefore, all equivalent changes made in accordance with the structure, shape, and principle of the present invention should be covered within the scope of protection of the present invention.
Claims
1. A face cream composition with liquid crystal emulsification effect for anti-aging, characterized in that, It includes the following components by weight percentage: Liquid crystal emulsion composition 85-95%; Anti-aging active ingredient composition 5-15%; The liquid crystal emulsion composition includes an emulsifier, a thickener, an oil, a preservative, and a solvent.
2. The anti-aging face cream composition according to claim 1, characterized in that, The liquid crystal emulsion composition comprises the following components by weight percentage: 1.5-2.5% polyglycerol-10 stearate and / or polyglycerol-5 oleate; 7-Dehydrocholesterol 0.05-0.1%; Cetearyl alcohol 2-3%; Hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer 1.0-1.2%; Cetyl ethylhexanoate 3.0%; 2.5% triglyceride (ethylhexanoate); Isododecane 2.0%; Polydimethylsiloxane 2.0%; Jojoba seed oil 0.2-1%; Glycerin 3-6%; Water content: 68-82%; Preservatives: 0.6-1%.
3. The anti-aging face cream composition according to claim 2, characterized in that, The preservative is a mixture of capryloyl hydroxamic acid, ethylhexylglycerin, pentylene glycol and caprylyl glycol.
4. The anti-aging face cream composition according to claim 1, characterized in that, The anti-aging active ingredient composition comprises the following components by weight percentage: Calendula extract 0.28-1.12%; Raspberry leaf extract 0.42-0.84%; 0.2-1% of palmate kelp extract; Sodium DNA 0.5-1%; Kale leaf extract 0.66-2%; Extract of *Leptochloa crus-galli* 0.05-0.2%; 1-2% European lycopodium extract; Butanediol 2.0-5.0%.
5. The anti-aging face cream composition according to claim 4, characterized in that, The sodium DNA contains wheat germ extract and carrageenan extract, forming a spherical DNA structure that helps it penetrate the skin.
6. A method for preparing an anti-aging face cream composition with liquid crystal emulsification effect according to any one of claims 1-5, characterized in that, Includes the following steps: Step S1: Preparation of Phase A: Mix water, glycerol and hydroxyethyl acrylate / sodium acryloyl dimethyl taurate copolymer, heat to 75°C, and homogenize at 5000-6000 rpm for 5 minutes; Step S2, Preparation of Phase B: Polyglycerol-10 stearate and / or polyglycerol-5 oleate, cetyl ethylhexanoate, triglyceride (ethylhexanoate), isododecane, polydimethylsiloxane, jojoba seed oil, cetearyl alcohol and 7-dehydrocholesterol are mixed and heated to 82°C until completely dissolved. Step S3: Add phase B to phase A and homogenize at 80±2℃ and 5000-6000 rpm for 3 minutes. Then cool down to 70±2℃ and continue homogenizing at 5000-6000 rpm for 3 minutes. Step S4: Cool to 45°C, add preservative, and homogenize at 3000-4000 rpm for 1 minute; Step S5: Cool to room temperature and age to obtain liquid crystal emulsion composition.
7. A method for preparing an anti-aging face cream composition with liquid crystal emulsification effect according to any one of claims 1-5, characterized in that, Includes the following steps: Step A1: Preparation of Phase A: Mix water, butanediol, glycerol and hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, heat to 75°C, and homogenize at 5000-6000 rpm for 5 minutes; Step A2, Preparation of Phase B: Mix polyglycerol-10 stearate and / or polyglycerol-5 oleate, cetyl ethylhexanoate, triglyceride (ethylhexanoate), isododecane, polydimethylsiloxane, jojoba seed oil, cetearyl alcohol and 7-dehydrocholesterol, and heat to 82°C until completely dissolved. Step A3: Add phase B to phase A, and homogenize at 80±2℃ and 5000-6000 rpm for 3 minutes. Then cool down to 70±2℃ and continue homogenizing at 5000-6000 rpm for 3 minutes. Step A4: Cool to 45°C, add anti-aging active ingredients and preservatives, and homogenize at 3000-4000 rpm for 1 minute; Step A5: Cool to room temperature and age to obtain an anti-aging face cream composition with liquid crystal emulsification effect.
8. The preparation method according to claim 6 or 7, characterized in that, Using the PIT phase transition method, the HLB values of polyglycerol-10 stearate and polyglycerol-5 oleate at different temperatures are utilized to form an O / W type liquid crystal emulsion structure below 72°C.
9. The application of a liquid crystal emulsion composition in the preparation of anti-aging cosmetics, characterized in that, The liquid crystal emulsion composition is formulated according to the proportions described in claim 2 or 3.
10. The application of an anti-aging active ingredient composition in the preparation of anti-aging cosmetics, characterized in that, The anti-aging active ingredient composition is formulated according to the proportions described in claim 4 or 5.
Citation Information
Patent Citations
Emulsifier composition capable of forming liquid crystal structure and application of emulsifier composition
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Liquid crystal emulsifier composition, and preparation method and application thereof in cosmetics
CN103494718B
