Self-forming rose congealed fat based on grease compounding and preparation method of self-forming rose congealed fat
By using a specific ratio of shea butter, jojoba seed oil, burmann walnut seed oil, and Rosa damascena flower oil, along with a staged temperature-controlled stirring method, a stable three-dimensional oil network is constructed. This solves the skin irritation and texture problems caused by additives in cosmetics, resulting in a soft, stable, self-forming gel with multiple skincare benefits.
Patent Information
- Application Number
- CN202511666641.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-11-14
- Publication Date
- 2026-01-06
AI Technical Summary
Existing cosmetics rely on surfactants, chemical preservatives, and synthetic fragrances, which can cause skin irritation. Traditional high-melting-point oil formulations are too hard, greasy, and unstable, making it difficult to achieve soft and stable solid products.
By using a specific ratio of shea butter, jojoba seed oil, burdock seed oil and Rosa damascena flower oil, and through a staged temperature control and stepped stirring rate preparation method, a delicate and stable three-dimensional oil network structure is constructed, avoiding synthetic additives and achieving self-forming solidified fat.
It achieves a solid gel with no synthetic additives, a soft touch, good spreadability, and stable storage, with skin moisturizing, repairing, anti-wrinkle and soothing effects, ensuring the stability and even distribution of active ingredients.
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Abstract
Description
Technical Field
[0001] This invention relates to the field of cosmetic technology, and in particular to a self-forming rose gel based on oil blends and its preparation method. Background Technology
[0002] In the cosmetics industry, creams, lotions, and other emulsion formulations are widely used in skin care. Traditionally, these emulsion systems typically rely on surfactants (emulsifiers) to stabilize the oil and water phases, resulting in a uniform and stable appearance. However, long-term or excessive use of additives such as emulsifiers, chemical preservatives, and synthetic fragrances may place a potential burden on the skin, even triggering irritation or allergic reactions, especially for people with sensitive skin.
[0003] With consumers increasingly demanding higher levels of product safety, gentleness, and a "pure beauty" philosophy, the market demand for cosmetics containing little or no of the aforementioned chemical additives has increased significantly. In response, the industry has undertaken numerous explorations. One important technological approach is utilizing the inherent properties of oils to construct anhydrous or low-water systems, such as solid creams, lip balms, and balms. These systems typically encapsulate liquid oils by forming a crystalline network structure with high-melting-point oils (such as waxes and solid esters) at room temperature, thus giving the product a solid state and theoretically avoiding the use of emulsifiers and preservatives.
[0004] However, developing such products still faces numerous technical challenges. First, to achieve sufficient hardness and room-temperature solidity, the formulation often requires a high proportion of high-melting-point oils. This can easily lead to products that are too hard, greasy, and have poor spreadability, resulting in a heavy "waxy" feel, difficulty in spreading, and an unpleasant skin feel. Second, to obtain a pleasant fragrance, synthetic fragrances are usually added, which contradicts the claim of "all-plant-derived." Furthermore, if the oil blending system is poorly designed or crystallization is not well controlled, the product is prone to oil seepage, rough texture, and poor stability during storage or use. In addition, relying entirely on plant oils to achieve self-forming while simultaneously ensuring excellent skin feel, stable form, and multiple skincare benefits such as soothing and repairing places extremely high demands on the selection, proportioning, and preparation process of the oils.
[0005] Invention Patent Content In view of this, the present invention provides a self-forming rose gel based on oil compound and its preparation method, so as to solve or alleviate the technical problems existing in the prior art.
[0006] The technical solution of this invention is implemented as follows: a self-forming rose gel based on oil compound, composed of the following components by mass percentage: shea butter: 55.0%~62.0%; jojoba seed oil: 38.0%~42.0%; burmann walnut seed oil: 0.5%~2.0%; and Rosa damascena flower oil: 0.1%~0.3%.
[0007] As an improvement, the components are expressed in the following percentages by mass: 58.84% shea butter, 40% jojoba seed oil, 1% burmann walnut seed oil, and 0.16% Rosa damascena flower oil.
[0008] A method for preparing a self-forming rose gel based on oil blends includes the following steps: S1. Melting of base oil: Under constant temperature conditions of 40~42℃, the avocado oil is heated and melted until it is basically clear and transparent to form a liquid base; S2. First phase mixing and homogenization: Jojoba seed oil is added to the liquid base, the temperature is maintained at 40~42℃, and the mixture is stirred at a low speed of 30~50 rpm for 20~25 min until it is uniformly mixed to obtain the first phase mixture; S3. Introduction of the second phase and activation of structure: Add Burrhard walnut seed oil to the first phase mixture, and increase the stirring speed to 100-200 rpm at 38-40℃ and continue stirring for 20-25 minutes to homogenize. Utilize the interaction between the unsaturated fatty acids rich in Burrhard walnut seed oil and the aforementioned oil system to initially activate the structural potential of the system and obtain the second phase mixture. S4. Low-temperature integration of active components: Cool the second phase mixture to 32~35℃, add Rosa damascena flower oil, reduce the stirring speed to 20~30rpm, and gently stir for 5-10min to ensure that the active essential oil components are evenly dispersed and integrated into the oil network structure to obtain the final mixture; S5. Self-curing: The final mixture is placed in a container at 28~30℃ in a dust-free and clean environment, and then naturally cooled to room temperature of 23~25℃. Within 4~8 hours, the mixture self-cures through the synergistic effect of vegetable oils to form a stable, soft-touch solid gel.
[0009] As an improvement, in step S3, the stirring is a low-speed shear homogenization performed in a shear emulsifier.
[0010] As an improvement, in step S5, the natural cooling process is carried out in stages: first, it is left to stand for 1 to 2 hours at an environment of 28~30℃, and then transferred to a room temperature environment of 23~25℃ to complete the final curing.
[0011] The present invention also provides the application of the above-mentioned self-forming rose gel in the preparation of skin care products for moisturizing, repairing, anti-wrinkle and soothing the skin.
[0012] Compared with the prior art, the beneficial effects of the present invention are: This invention is made entirely from a specific ratio of plant oils, without relying on any synthetic emulsifiers, chemical preservatives, or synthetic fragrances. This avoids the risk of skin irritation that additives may cause, making the formula system gentler and safer, and in line with the trend of pure beauty.
[0013] By using shea butter as the solid framework, jojoba seed oil as the liquid oil phase, and introducing burr hard walnut seed oil as a natural crystal regulator, the unsaturated fatty acids effectively induce and stabilize the β' crystal form, synergistically constructing a delicate and stable three-dimensional oil network structure. This structure not only enables the product to solidify autonomously, avoiding the problems of hard texture, heavy waxy feel, and difficulty in spreading caused by traditional high-wax content formulas, but also ultimately yields a solid gel with a soft touch, excellent spreadability, and stable storage.
[0014] The preparation method provided by this invention achieves effective guidance of the oil crystallization process and protection of heat-sensitive active ingredients through precise operation of staged temperature control and stepped stirring rate, especially the key steps of structure activation and low-temperature integration, thus ensuring that the product structure is uniform and stable and the efficacy of active ingredients is fully preserved.
[0015] The oil blend of this invention is itself rich in nutrients. With the addition of Rosa damascena flower oil, it provides a natural fragrance while giving the product multiple benefits such as skin moisturizing, barrier repair, soothing and anti-wrinkle effects, achieving a balance between a simplified formula and comprehensive care effects.
[0016] The above overview is for illustrative purposes only and is not intended to be limiting in any way. In addition to the illustrative aspects, embodiments, and features described above, further aspects, embodiments, and features of the invention will become readily apparent from the following detailed description. Detailed Implementation
[0017] The invention will be more readily understood by referring to the following detailed description of preferred embodiments and included examples. Unless otherwise specified, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains. In case of conflict, the definitions in this specification shall prevail.
[0018] As used herein, the terms “prepared from” and “comprising” are synonymous. The terms “comprising,” “including,” “having,” “containing,” or any other variations thereof, as used herein, are intended to cover non-exclusive inclusion. For example, a composition, step, method, article, or apparatus that includes the listed elements is not necessarily limited to those elements, but may include other elements not expressly listed or elements inherent to such composition, step, method, article, or apparatus.
[0019] The conjunction "composed of..." excludes any unspecified elements, steps, or components. If used in a claim, this phrase makes the claim closed, excluding materials other than those described, except for associated conventional impurities. When the phrase "composed of..." appears in a clause of the body of a claim rather than immediately following it, it limits only the elements described in that clause; other elements are not excluded from the claim as a whole.
[0020] When a quantity, concentration, or other value or parameter is expressed as a range, a preferred range, or a range defined by a series of upper and lower preferred values, this should be understood as specifically disclosing all ranges formed by any pair of any upper or preferred value with any lower or preferred value, regardless of whether the range is disclosed individually. For example, when the range “1 to 5” is disclosed, the described range should be interpreted as including the ranges “1 to 4”, “1 to 3”, “1 to 2”, “1 to 2 and 4 to 5”, “1 to 3 and 5”, etc. When numerical ranges are described herein, unless otherwise stated, the range is intended to include its endpoints and all integers and fractions within that range.
[0021] The singular form includes the plural objects of discussion unless the context clearly indicates otherwise. "Optional" or "any one" means that the matter or event described thereafter may or may not occur, and the description includes both the possibility that the event occurs and the possibility that the event does not occur.
[0022] Approximate terms used in the specification and claims to modify quantities indicate that the invention is not limited to that specific quantity, but also includes acceptable modifications close to that quantity that do not alter the relevant essential function. Correspondingly, the use of "about," "approximately," etc., to modify a numerical value means that the invention is not limited to that precise value. In some instances, approximate terms may correspond to the precision of the instrument used to measure the value. In this application's specification and claims, scope definitions can be combined and / or interchanged, unless otherwise stated, these scopes include all subscopes contained therein.
[0023] Furthermore, the indefinite articles “a” and “an” preceding the elements or components of this invention do not impose any limitation on the quantity (i.e., number of times) of the elements or components. Therefore, “an” or “a” should be interpreted as including one or at least one, and the singular form of an element or component also includes the plural form, unless the quantity clearly refers to the singular form.
[0024] Furthermore, any methods and materials similar to or equivalent to those described herein may be applied to this invention. The preferred embodiments and materials described herein are for illustrative purposes only and do not limit the scope of this application.
[0025] Unless otherwise specified, the experimental methods used in the following examples are conventional methods; unless otherwise specified, the experimental materials and test strains used in the following examples were purchased from commercial channels.
[0026] This invention provides a self-forming rose gel based on a blend of oils, comprising the following components by weight percentage: shea butter: 55.0%~62.0%; jojoba seed oil: 38.0%~42.0%; burmann walnut seed oil: 0.5%~2.0%; and Rosa damascena flower oil: 0.1%~0.3%.
[0027] A method for preparing a self-forming rose gel based on oil blends includes the following steps: S1. Melting of base oil: Under constant temperature conditions of 40~42℃, the avocado oil is heated and melted until it is basically clear and transparent to form a liquid base; By melting the base oil, a fully molten, homogeneous, and stable liquid base is established, ensuring that the subsequent addition of all components and structural changes are carried out on a controllable and consistent basis. Specifically, shea butter (55.0%~62.0%) serves as the basic framework. It is solid at room temperature, rich in saturated fatty acids (such as stearic acid and palmitic acid), and has a high melting point (approximately 25~30℃). Upon cooling after melting, it crystallizes first, forming a three-dimensional network structure that provides hardness and solid support for the entire gel system. Simultaneously, this three-dimensional network structure can firmly lock a large amount of liquid oil (jojoba seed oil) within it through physical forces (van der Waals forces, crystal entanglement), forming an oil gel structure. Furthermore, the surface area and tiny pores of the three-dimensional network structure formed by shea butter can adsorb and fix the liquid oil, preventing leakage and thus ensuring the physical stability of the product.
[0028] Moreover, avocado oil is a mixture of various triglycerides. Setting the temperature at 40~42℃, which is higher than its melting range, ensures that all high-melting-point crystal structures are completely and thoroughly destroyed, guaranteeing that it melts completely to form a completely clear and transparent liquid base. Meanwhile, during the solidification process, oils and fats form crystal nuclei. These nuclei may remain after partial melting and, during subsequent cooling and solidification, act as heterogeneous nucleation sites, leading to excessively rapid crystallization and coarse crystals, resulting in a rough, grainy texture in the product. High temperatures of 40-42°C can eliminate all pre-existing, unstable crystal morphology memories. By completely transforming it into an amorphous liquid, it lays the foundation for the subsequent controllable induction of stable crystal forms.
[0029] In practice, the liquid base formed ensures that when jojoba seed oil is added, the two oils can achieve rapid and thorough mutual diffusion and fusion at the molecular level. Moreover, the obtained melt without crystal nucleus memory will synchronously and uniformly generate a large number of small and stable crystal nuclei when subjected to shear force and induced by Burr hard walnut seed oil in step S3, and this controlled crystallization process can form a delicate, soft and stable gel structure.
[0030] S2. First phase mixing and homogenization: Jojoba seed oil is added to the liquid base, the temperature is maintained at 40~42℃, and the mixture is stirred at a low speed of 30~50 rpm for 20~25 min until it is uniformly mixed to obtain the first phase mixture; While maintaining thermal stability, liquid jojoba seed oil is uniformly, gently, and thoroughly integrated into a molten shea butter base to form a homogeneous first-phase mixture.
[0031] Specifically, a temperature of 40-42°C ensures that the shea butter liquid base remains a completely molten and clear liquid, preventing the premature precipitation of any tiny, irregular crystals due to temperature fluctuations (especially drops). Simultaneously, the low viscosity and good fluidity of shea butter at this temperature greatly facilitate the dispersion and mixing of jojoba seed oil, allowing for molecular-level homogeneous fusion with lower energy input. Furthermore, the consistent temperature avoids localized viscosity differences caused by temperature variations, thus preventing uneven mixing.
[0032] Using a low stirring speed of 30~50rpm generates effective convection, which disperses the jojoba seed oil. At the same time, it is gentle enough to minimize the entrainment of air bubbles into the high-viscosity oil system, thus preventing voids in the final product caused by air ingress, which would affect the appearance and stability.
[0033] In practice, the resulting first-phase mixture provides a constant-composition, non-concentration-gradient reaction environment for Burr hard walnut seed oil, ensuring its homogeneous and synchronous interaction with shea butter and jojoba seed oil. Furthermore, it allows the shear force to be uniformly distributed to every part of the system during high-speed shearing in step S3, thereby efficiently and synchronously inducing the formation of uniform, fine crystal nuclei throughout the system.
[0034] Furthermore, as a liquid oil phase, the uniform distribution of jojoba seed oil is crucial for the final formation of a stable oleogel structure. During the curing process in step S5, the crystalline network of shea butter needs to uniformly coat each jojoba seed oil. If the jojoba seed oil is not mixed evenly with the liquid substrate, the crystalline network will be weaker in areas rich in jojoba seed oil, potentially leading to localized softness or even oil seepage in the product; while in areas rich in shea butter, the product will be harder and have a waxy feel.
[0035] S3. Introduction of the second phase and activation of structure: Add Burrhard walnut seed oil to the first phase mixture, and increase the stirring speed to 100-200 rpm at 38-40℃ and continue stirring for 20-25 minutes to homogenize. Utilize the interaction between the unsaturated fatty acids rich in Burrhard walnut seed oil and the aforementioned oil system to initially activate the structural potential of the system and obtain the second phase mixture. The stirring process involves low-speed shearing homogenization performed in a shear emulsifier.
[0036] By introducing Burr hard walnut seed oil and applying a mechanical shear field, a fine and stable oil crystal network is actively induced and initially constructed, thereby stimulating the system's potential to transform from a liquid to a solid gel.
[0037] Specifically, the temperature is slightly reduced from 40-42°C in step S2 to 38-40°C to create a controlled supercooled environment that allows the melt to begin crystallizing. However, this temperature range is still higher than the complete melting point of avocado oil, ensuring that the system is mainly liquid while being close enough to its crystallization initiation point, significantly increasing the tendency for molecular aggregation and nucleation, and putting the system in a pre-crystallization state.
[0038] When the system is in a supercooled state, applying high-speed shear can greatly increase the number and rate of crystal nuclei formation. The shear flow field can orient oil molecules and generate a large number of nucleation sites through local pressure and friction, forming numerous tiny crystals. Under shearing, the newly formed tiny crystals collide, connect, and entangle with each other, initially building a three-dimensional network structure that runs through the entire system. This network effectively encapsulates and fixes the liquid jojoba seed oil, thus forming the prototype of an oleogel. Among them, the unsaturated fatty acid triglycerides (such as linoleic acid glycerides) abundant in jojoba seed oil have a significantly different molecular structure from the regular saturated fatty acid triglycerides (such as stearic acid and palmitic acid glycerides) in shea butter. During the cooling crystallization process, these heterogeneous molecules selectively adsorb onto specific crystal faces of the growing β crystal nuclei through acyl-acyl interactions, generating steric hindrance and effectively inhibiting excessive crystal growth along specific directions. This hinders the formation and growth of coarse and unstable β crystal forms, prompting the system to tend to form more fine, dense, and thermodynamically stable β' primary crystal forms. The β' crystal network has a higher specific surface area and a superior spatial network structure, enabling it to more effectively encapsulate and fix liquid jojoba seed oil.
[0039] By constructing a primary crystal network, the system retains sufficient structural strength and thixotropy after cooling (32~35℃) in step S4, enabling it to withstand the introduction of Rosa damascena flower oil and gentle stirring without network collapse or oil phase separation, thus ensuring the successful integration of active components.
[0040] Meanwhile, by pre-setting crystal seeds and network prototypes under controlled conditions, the static curing stage of step S5 is guided to only involve directional growth of crystals and network maturation, rather than random crystallization. This ensures that the final product can autonomously form a solid gel with specific rheological properties (such as yield stress and thixotropy) and a stable microstructure within a predetermined time (4-8 hours).
[0041] S4. Low-temperature integration of active components: Cool the second phase mixture to 32~35℃, add Rosa damascena flower oil, reduce the stirring speed to 20~30rpm, and gently stir for 5-10min to ensure that the active essential oil components are evenly dispersed and integrated into the oil network structure to obtain the final mixture; By physically integrating heat-sensitive Rosa damascena flower oil into the gaps of the oil network without damaging the primary crystal network constructed in the above steps, uniform distribution, improved stability, and sustained release of efficacy are achieved.
[0042] Specifically, a temperature of 32-35℃ can prevent the thermal degradation and excessive volatilization of volatile aromatic components (such as citronellol and geraniol) and heat-sensitive active substances (such as natural antioxidants) in Rosa damascena flower oil. This temperature range is far below the flash point and rapid volatilization threshold of most essential oil components, thus maximizing the preservation of their biological activity and aroma integrity. Moreover, this temperature is below the final melting point of shea butter, ensuring that the β' primary crystal network constructed in step S3 remains stable and continues to grow, preventing rapid floating or settling of Rosa damascena flower oil due to density differences after its addition.
[0043] Using an extremely low linear velocity of 20-30 rpm, laminar flow is generated through gentle stirring, achieving uniform dispersion at both the macroscopic and microscopic levels. However, the shear stress is far below the yield stress of the primary crystalline network framework, thus avoiding crystal network breakage and collapse caused by mechanical forces. At the same time, the low-speed stirring provides ample time for essential oil molecules to penetrate into the microporous structure of the oil network through diffusion.
[0044] In practice, at 32-35°C, the oil crystal network has formed, but it is not completely closed, containing abundant nano- to micron-scale pores. Liquid Rosa damascena flower oil, under gentle stirring, is drawn into these three-dimensional network pores through capillary action. The non-polar terpenoids in the Rosa damascena flower oil (such as geraniol and citronellol) are highly compatible with the liquid oil phase (jojoba seed oil) in the oil network, and are adsorbed and anchored at the network's intersections and crystal surfaces through van der Waals forces. Ultimately, the Rosa damascena flower oil is physically encapsulated and fixed within the three-dimensional network composed of solid crystal fibers and liquid plasticized oil, achieving the integration of the active components and significantly reducing their migration, precipitation, and volatilization rates, thus realizing a sustained-release effect.
[0045] Through the incorporation of Rosa damascena flower oil, as the crystal network continues to grow and strengthen with further cooling and solidification in step S5, the essential oil molecules are permanently locked in a denser solid gel network, ensuring the stability of the product during storage and use. This directly determines the uniformity, stability, and release behavior of the active ingredients in the final gel, avoiding problems such as "oil spots" (essential oil seepage) or uneven fragrance on the product surface, and ensuring that each unit dose (each application) contains standardized active ingredients.
[0046] S5. Self-curing: The final mixture is placed in a container at 28~30℃ in a dust-free and clean environment, and then naturally cooled to room temperature of 23~25℃. Within 4~8 hours, the mixture self-cures through the synergistic effect of vegetable oils to form a stable, soft-touch solid gel.
[0047] The natural cooling process is carried out in stages: first, it is left to stand for 1 to 2 hours at 28~30℃, and then transferred to a room temperature environment of 23~25℃ to complete the final curing.
[0048] By controlling the cooling path, the oil crystal network is guided to complete the final directional growth, cross-linking enhancement, and morphological stabilization, thereby achieving the autonomous transformation from liquid / semi-solid to the predetermined solid state.
[0049] Specifically, at a filling temperature of 28~30℃, the crystal nuclei formed in step S3 have begun to grow, and the viscosity of the system increases significantly, reaching the critical point between a supercooled liquid state and a gel state. The rheological properties in this state ensure smooth filling and a smooth paste surface during filling, while also preventing the material from flowing and deforming within the container after filling, laying the foundation for the final product form.
[0050] The 28-30°C stage during the cooling process is the optimal kinetic window for the formation of the β' primary crystal form in components such as shea butter. Maintaining this temperature for 1-2 hours provides sufficient energy and time for the crystals, allowing the numerous microcrystalline nuclei formed in step S3 to grow orderly and fully into slender, dense fibrous crystals. These crystals interlock to form a strong, continuous three-dimensional network framework, effectively suppressing the formation of unstable, coarse β-crystals due to excessive supercooling when directly and rapidly cooled to room temperature, thus preventing the product from having a rough texture and a grainy feel.
[0051] During the 23-25℃ cooling stage, the remaining crystallizable components and high-melting-point triglycerides in the system are solidified on the already formed stable framework, ultimately ensuring that the product reaches thermodynamic equilibrium at the operating temperature and obtains the predetermined hardness and morphological stability.
[0052] The present invention also provides the application of the above-mentioned self-forming rose gel in the preparation of skin care products for moisturizing, repairing, anti-wrinkle and soothing the skin.
[0053] Example 1 A self-forming rose gel based on oil blends, comprising the following components by weight percentage: shea butter: 55.7%; jojoba seed oil: 42.0%; burmann walnut seed oil: 2.0%; and Rosa damascena flower oil: 0.3%.
[0054] A method for preparing a self-forming rose gel based on oil blends includes the following steps: S1. Melting of base oil: Under constant temperature conditions of 40℃, the avocado oil is heated and melted until it is basically clear and transparent, forming a liquid base; S2. First phase mixing and homogenization: Jojoba seed oil is added to the liquid base, the temperature is maintained at 40°C, and the mixture is stirred at a low speed of 30 rpm for 20 minutes until it is uniformly mixed to obtain the first phase mixture; S3. Introduction of the second phase and activation of structure: Burrhard walnut seed oil was added to the first phase mixture. The stirring speed was increased to 100 rpm and stirred continuously for 20 min at 38°C to homogenize the mixture. The interaction between the unsaturated fatty acids rich in Burrhard walnut seed oil and the aforementioned oil system was utilized to initially activate the structural potential of the system and obtain the second phase mixture. The stirring process involves low-speed shearing homogenization performed in a shear emulsifier.
[0055] S4. Low-temperature integration of active components: Cool the second phase mixture to 32°C, add Rosa damascena flower oil, reduce the stirring speed to 20 rpm, and gently stir for 5 min to ensure that the active essential oil components are evenly dispersed and integrated into the oil network structure to obtain the final mixture; S5. Self-curing: The final mixture is placed in a container at 28°C in a dust-free and clean environment and then allowed to cool naturally to room temperature of 23°C. Within 4 hours, the mixture self-cures through the synergistic effect of the vegetable oil to form a stable, soft-touch solid gel.
[0056] The natural cooling process is carried out in stages: first, it is left to stand at 28°C for 1 hour, and then transferred to a room temperature environment of 23°C to complete the final curing.
[0057] The present invention also provides the application of the above-mentioned self-forming rose gel in the preparation of skin care products for moisturizing, repairing, anti-wrinkle and soothing the skin.
[0058] Example 2 A self-forming rose gel based on oil blends, comprising the following components by weight percentage: 58.84% shea butter, 40% jojoba seed oil, 1% burmann walnut seed oil, and 0.16% Rosa damascena flower oil.
[0059] A method for preparing a self-forming rose gel based on oil blends includes the following steps: S1. Melting of base oil: Under constant temperature conditions of 41℃, the avocado oil is heated and melted until it is basically clear and transparent to form a liquid base; S2. First phase mixing and homogenization: Jojoba seed oil is added to the liquid base, the temperature is maintained at 41°C, and the mixture is stirred at a low speed of 40 rpm for 23 minutes until it is uniformly mixed to obtain the first phase mixture; S3. Introduction of the second phase and activation of structure: Burrhard walnut seed oil was added to the first phase mixture. The stirring speed was increased to 150 rpm and stirred continuously for 23 min at 39°C to homogenize the mixture. The interaction between the unsaturated fatty acids rich in Burrhard walnut seed oil and the aforementioned oil system was utilized to initially activate the structural potential of the system and obtain the second phase mixture. The stirring process involves low-speed shearing homogenization performed in a shear emulsifier.
[0060] S4. Low-temperature integration of active components: Cool the second phase mixture to 33°C, add Rosa damascena flower oil, reduce the stirring speed to 25 rpm, and gently stir for 8 minutes to ensure that the active essential oil components are evenly dispersed and integrated into the oil network structure to obtain the final mixture; S5. Self-curing: The final mixture is placed in a container at 29°C in a dust-free and clean environment and then allowed to cool naturally to room temperature of 24°C. Within 6 hours, the mixture self-cures through the synergistic effect of the vegetable oil to form a stable, soft-touch solid gel.
[0061] The natural cooling process is carried out in stages: first, it is left to stand at 29℃ for 1.5 hours, and then transferred to a room temperature environment of 24℃ to complete the final curing.
[0062] The present invention also provides the application of the above-mentioned self-forming rose gel in the preparation of skin care products for moisturizing, repairing, anti-wrinkle and soothing the skin.
[0063] Example 3 A self-forming rose gel based on an oil blend, comprising the following components by weight percentage: shea butter: 61.4%; jojoba seed oil: 38.0%; burmann walnut seed oil: 0.5%; and Rosa damascena flower oil: 0.1%.
[0064] A method for preparing a self-forming rose gel based on oil blends includes the following steps: S1. Melting of base oil: Under constant temperature conditions of 42℃, the avocado oil is heated and melted until it is basically clear and transparent to form a liquid base; S2. First phase mixing and homogenization: Jojoba seed oil is added to the liquid base, the temperature is maintained at 42°C, and the mixture is stirred at a low speed of 50 rpm for 25 minutes until it is uniformly mixed to obtain the first phase mixture; S3. Introduction of the second phase and activation of structure: Burrhard walnut seed oil was added to the first phase mixture. At 40°C, the stirring speed was increased to 200 rpm and stirred continuously for 25 min to homogenize. The interaction between the unsaturated fatty acids rich in Burrhard walnut seed oil and the aforementioned oil system was utilized to initially activate the structural potential of the system and obtain the second phase mixture. The stirring process involves low-speed shearing homogenization performed in a shear emulsifier.
[0065] S4. Low-temperature integration of active components: Cool the second phase mixture to 50°C, add Rosa damascena flower oil, reduce the stirring speed to 30 rpm, and gently stir for 10 min to ensure that the active essential oil components are evenly dispersed and integrated into the oil network structure to obtain the final mixture; S5. Self-curing: The final mixture is placed in a container at 35°C in a dust-free and clean environment and then allowed to cool naturally to room temperature of 25°C. Within 8 hours, the mixture self-cures through the synergistic effect of the vegetable oil to form a stable, soft-touch solid gel.
[0066] The natural cooling process is carried out in stages: first, it is left to stand at 30°C for 2 hours, and then transferred to a room temperature environment of 25°C to complete the final curing.
[0067] The present invention also provides the application of the above-mentioned self-forming rose gel in the preparation of skin care products for moisturizing, repairing, anti-wrinkle and soothing the skin.
[0068] Experiment Example 1: Product Physical Stability Test Experiment 1. Experimental objective: This experiment aims to objectively evaluate the physical stability of the self-forming rose gel prepared in Example 2 of this invention, including heat resistance, cold resistance, mechanical stability (centrifugation), and long-term storage stability.
[0069] 2. Test sample: The self-forming rose gel prepared in Example 2 is a solid gel that is milky white to slightly yellow with a fine and uniform texture and has a characteristic rose aroma.
[0070] 3. Experimental methods and procedures: 3.1 Heat resistance test: Procedure: Take three parallel samples, weigh 15.00 g of each into a clean, dry weighing bottle, and smooth the surface with a spatula. Place them in a constant temperature incubator at 40℃ ± 1℃ for 30 days. Remove them on days 10, 20, and 30, and observe and evaluate them after cooling at room temperature (25℃) for 1 hour.
[0071] Observation indicators: whether the shape is maintained, whether there is oil separation on the surface, color change, and texture change.
[0072] 3.2 Cold Resistance Test: Procedure: Take three parallel samples, weigh 15.00g of each into a clean, dry weighing bottle, and level the surface. Place them in a refrigerator at -10℃ ± 1℃ for 30 days.
[0073] Observation indicators: After removal, let it stand at room temperature (25℃) for 2 hours to allow it to naturally return to room temperature. Observe whether the texture is uniform, whether there is a grainy feel, roughness, cracking, or oil seepage.
[0074] 3.3 Centrifugation test: Procedure: Take three parallel samples, weigh 15.00 g of each into a 10 mL centrifuge tube of known weight, and accurately weigh the total weight using an analytical balance. Place the centrifuge tubes in a centrifuge and centrifuge at 3000 rpm for 30 minutes.
[0075] Observation and Calculation: After centrifugation, carefully observe the centrifuge tube walls and bottom for any oil layer precipitation. If oil is precipitated, carefully pour it out and weigh the total weight of the centrifuge tube and the remaining sample using an analytical balance. Calculate the percentage of the precipitated oil mass to the total sample mass (oil precipitation rate).
[0076] Calculate the oil separation rate: Oil separation rate (%) = [(Total weight before centrifugation - Total weight after centrifugation) / Net weight of sample] × 100% 3.4 Long-term stability test (accelerated test): Steps: Take three batches of independently produced samples and place them in a constant temperature and humidity chamber for 6 months at a temperature of 25℃ ± 1℃ and a relative humidity of 50% ± 5%.
[0077] Observation indicators: At the end of months 0, 1, 3 and 6, the samples were opened for inspection, and the changes in appearance, odor and hardness of the samples were observed and recorded.
[0078] 4. Experimental Data and Results: Table 1-1 Record of Heat Resistance Test Results
[0079] Table 1-2 Record of Cold Resistance Test Results
[0080] Table 1-3 Record of Centrifugation Test Results
[0081] Table 1-4 Record of Long-Term Stability Test Results
[0082] 5. Experimental Conclusions and Summary: 5.1 Conclusion Based on the above experimental data, the following conclusions are drawn regarding the physical stability of the sample in Example 2: The heat resistance test results showed that after being placed at 40℃ for 30 days, the sample still maintained structural stability and showed no oil precipitation. This confirms that the stable crystal network, mainly composed of β' crystal form, induced by Burr hard walnut seed oil, can maintain its structural integrity at temperatures close to the melting point of shea butter, thus achieving effective encapsulation of the liquid oil phase.
[0083] After being frozen at -10℃ for 30 days, the sample remained uniform, delicate, and soft after returning to room temperature, without exhibiting any crystal structure damage, roughening, or oil seepage caused by the freeze-thaw cycle. This indicates that its oil network possesses good low-temperature tolerance and reversibility, making it suitable for storage and use in cold environments.
[0084] The centrifugation test results showed that the oil separation rate was 0.00%, which indicates that the oleogel structure formed by the specific oil compounding and process of the present invention can effectively bind the liquid oil phase with its three-dimensional network. Even under strong centrifugal force, no oil phase separation occurred, demonstrating excellent cohesion and oil holding capacity.
[0085] In a 6-month accelerated stability test, the sample showed no observable negative changes in the three key indicators of appearance, odor, and hardness. This indicates that the product has good stability for at least 6 months under normal storage conditions, providing a reliable scientific basis for setting the product's shelf life.
[0086] 5.2 Summary Based on the above stability test results, the self-forming rose gel prepared in Example 2 of this invention exhibits good physical stability and can effectively resist the effects of heat, cold, mechanical force and time, maintaining its initial excellent state.
[0087] Experiment Example 2: Evaluation Experiment on Skin Feel and User Experience 1. Experimental objective: This experiment aims to comprehensively and quantitatively evaluate the sensory characteristics of the invention in actual use through standardized human sensory evaluation, including the user experience, spreadability, melting speed, absorbability, and post-use skin feel.
[0088] 2. Test sample: Sample name: Self-forming rose gel prepared in Example 2, which is a solid gel that is milky white to slightly yellow, with a fine and uniform texture, and has a characteristic rose fragrance.
[0089] 3. Experimental methods and procedures: 3.1 Volunteer Screening: Thirty healthy female volunteers, aged 25-45, were selected, covering dry, normal, and combination skin types. Exclusion criteria: known allergy to the test ingredient, skin disease at the test site, pregnancy or breastfeeding.
[0090] Testing environment: All tests were conducted in a constant temperature and humidity environment (temperature 22±2℃, humidity 50±5%). Volunteers were required to sit quietly in this environment for 30 minutes to acclimatize before the test could begin.
[0091] 3.2 Testing Procedure (Blind Testing): Samples are identified only by random numbers.
[0092] Test sites: the inner side of the left and right forearms of volunteers (approximately 4cm x 4cm in area).
[0093] Sampling: Using a precision scoop, the same experimenter took 10mg of sample and placed it on the volunteer's fingertip.
[0094] Evaluation process: Handling and initial impressions: Volunteers observed the solid form of the sample on their fingertips and recorded their first impressions.
[0095] Spreadability test: Volunteers apply the sample evenly in circular motions five times on a designated test area at a speed of one circle per second. Evaluators record the smoothness of the spread.
[0096] Melting speed test: During the application process, volunteers experienced how quickly the sample transformed from a solid to an oily state.
[0097] Absorption and residue evaluation: After application, volunteers left the skin for 1 minute and then gently rubbed it to assess whether there was any oily, sticky or waxy feeling.
[0098] Post-use skin feel evaluation: Five minutes after application, volunteers described the overall feeling of their skin, such as softness, hydration, and smoothness.
[0099] Data recording: After the experience, each volunteer immediately scored the four dimensions independently according to the scoring criteria.
[0100] 3.3 Evaluation Criteria (5-point scale):
[0101] 4. Experimental Data and Results: Table 2. Statistical table of skin feel and user experience evaluation scores (n=30)
[0102] Excerpt of representative volunteer descriptions: Volunteers' subjective feedback was highly consistent, with many agreeing that the product "melts upon contact with skin." This manifested in several ways: easy to use (soft texture when solid, easy to apply), good spreadability (low resistance during application, easy to spread evenly), and rapid melting (quickly transforms from solid to oil upon contact with skin). Post-use skin feel evaluations focused on "moisturizing without being greasy" and "leaving skin soft and smooth," indicating good skin affinity and absorption.
[0103] 5. Experimental Conclusion: Based on the rating data and subjective feedback from 30 volunteers, the following conclusions were drawn regarding the skin feel and user experience of the sample in Example 2: The spreadability score was 4.73 ± 0.46 (out of 5), and 100% of the volunteers gave it a score of 4 or higher. This directly confirms that the present invention overcomes the common defects of traditional anhydrous ointments, such as heavy waxiness and difficulty in spreading, by optimizing the ratio of solid oil (shea butter) to liquid oil (jojoba seed oil) and using burr hard walnut seed oil to adjust the crystal structure.
[0104] The melting speed had an average score of 4.57, with 96.7% of volunteers giving it a score of 4 or higher. This indicates that the gel can quickly transform from a solid state into an easily spreadable oil, avoiding the need for repeated rubbing on the skin and enhancing the user experience.
[0105] The average score for absorbency / greasiness was 4.60, and none of the volunteers (100%) felt noticeably greasy. This indicates that although the product has a high oil content, its stable structure ensures that the oils are quickly released and effectively absorbed, forming a moisturizing rather than greasy film on the skin surface, resulting in a dry and comfortable post-use feel.
[0106] The average score for skin feel after use was 4.77. Volunteers clearly reported that their skin immediately became softer, more moisturized, and smoother. This proves that the product not only provides a pleasant application process but also achieves skin improvement, meeting consumers' expectations for the core efficacy of skincare products.
[0107] The standard deviations of all indicators were below 0.5, with a combined standard deviation of only 0.28. This indicates that the evaluation of the product's feel was highly consistent across volunteer groups of different ages and skin types, demonstrating stable and reliable product performance that can meet the preferences of the vast majority of target users.
[0108] Experiment Example 3: Skin Moisturizing Effect Test Experiment 1. Experimental objective: This experiment aims to objectively and quantitatively evaluate the immediate effect and lasting moisturizing ability of the present invention in increasing the moisture content of the stratum corneum after application to human skin.
[0109] 2. Test sample: Sample name: Self-forming rose gel prepared in Example 2, which is a solid gel that is milky white to slightly yellow, with a fine and uniform texture, and has a characteristic rose fragrance.
[0110] Control area: On the same arm of each volunteer, a blank control area of the same size was marked out without any treatment.
[0111] 3. Experimental methods and procedures: 3.1 Volunteer Selection and Preparation: Thirty healthy female volunteers, aged 25-45, with dry or normal skin and an initial stratum corneum moisture content of less than 45 au on the inner side of their arms, were selected. Exclusion criteria: individuals with known allergies to the test ingredient; individuals with skin diseases or injuries at the test site; individuals who have recently used hormones or immunosuppressants at the test site; and pregnant or breastfeeding women.
[0112] Environmental control: All tests were conducted in a constant temperature and humidity environment (temperature 21±1℃, relative humidity 50±5%). Before the test, volunteers were required to expose their arms and sit quietly in this environment for at least 30 minutes to adapt.
[0113] 3.2 Testing Instruments: Instrument: Corneometer® CM 825 Skin Moisture Test Probe.
[0114] Principle: Based on the principle of capacitance, this method measures the change in the dielectric constant of the stratum corneum of the skin's epidermis, thereby indirectly reflecting the moisture content. Readings are expressed in arbitrary units (au), with higher values indicating higher moisture content.
[0115] Calibration: Perform calibration strictly in accordance with the instrument operating procedures before testing.
[0116] 3.3 Test Procedure: Region marking: Mark two test areas, each 4cm × 4cm, at least 2cm apart, on the inner side of the volunteer's forearm. One is the sample area, and the other is the blank control area.
[0117] Initial value measurement (T0): After the adaptation period, the moisture value at 3 different points in each marked area was measured using a Corneometer, and the average value was taken as the initial moisture value of the area.
[0118] Sample application: In the sample area, the technician uses a precision balance to weigh and evenly apply the sample, at a rate of 2.0 mg / cm³. 2 The control area was left untreated.
[0119] Measurement time points: Moisture levels were measured in two areas at 0.5 hours, 2 hours, 4 hours, and 8 hours after application (3 points were measured in each area, and the average was taken). During measurement, ensure the probe is perpendicular to the skin, applies gentle pressure, and remains on the skin for a consistent time.
[0120] 3.4 Data Analysis: Calculate the difference in moisture content between the sample area and the control area at each time point.
[0121] Paired T-tests were performed using SPSS software to compare whether there was a statistically significant difference in moisture values between the sample area and the control area at the same time point (p<0.05 was considered statistically significant).
[0122] 4. Experimental Data and Results: Table 3. Data Recording of Changes in Skin Moisture Content (n=30, Unit: au)
[0123] 5. Experimental Conclusion: Based on the above measurement data, the following conclusions are drawn regarding the skin moisturizing effect of the sample in Example 2: Skin moisturizing tests showed that after 0.5 hours of sample application, the moisture content of the stratum corneum was significantly increased and remained higher than that of the untreated area for 8 hours. This demonstrates the synergistic moisturizing mechanism of the oil-based compound system of this invention: liquid oils such as jojoba seed oil rapidly spread to form a sebum film, immediately reducing transepidermal water loss; while shea butter has good compatibility with skin lipids and can fuse with the sebum film to jointly build a long-lasting water-locking barrier, thereby providing immediate hydration and long-lasting moisturizing power.
[0124] At 2, 4, and even 8 hours after application, the moisture content of the sample area was consistently significantly higher than that of the control area (23.4 au, 18.4 au, and 12.0 au higher, respectively, p<0.001). Even after 8 hours, the skin moisture content was still 12.0 au higher than that of the untreated area, indicating that it has long-lasting water-locking and moisturizing properties.
[0125] The moisture content peaked at 0.5 hours and then showed a steady and slow downward trend, indicating that the oil in the product fused with the skin's sebum film to form an effective protective film that could continuously slow down the transepidermal loss of skin moisture, thereby locking moisture into the skin.
[0126] Experiment Example 4: Skin Barrier Repair Effect Test 1. Experimental objective: This experiment aims to objectively and quantitatively evaluate the repair speed and repair capacity of this invention for damaged skin barriers. The TEWL value is an internationally recognized gold standard for evaluating skin barrier function; the lower the value, the more intact the barrier function.
[0127] 2. Test sample: Sample name: Self-forming rose gel prepared in Example 2, which is a solid gel that is milky white to slightly yellow, with a fine and uniform texture, and has a characteristic rose fragrance.
[0128] Control area: On the same arm of each volunteer, a blank control area of the same size was marked, which was damaged but not treated.
[0129] 3. Experimental methods and procedures: 3.1 Volunteer Selection and Preparation: Twenty-eight healthy female volunteers, aged 25-45, with healthy skin and no history of allergies, were selected.
[0130] Exclusion criteria: Skin disease, scars or allergies at the test site; pregnancy or breastfeeding; recent use of medications or skincare products that affect the skin barrier at the test site.
[0131] Environmental control: All tests were conducted in a constant temperature and humidity environment (temperature 21±1℃, relative humidity 50±5%). Before the test, volunteers were required to expose their arms and sit quietly in this environment for at least 30 minutes to adapt.
[0132] 3.2 Testing Instruments: Instrument: Tewameter® TM 300 transdermal moisture loss tester.
[0133] Principle: By measuring the water vapor pressure gradient on the skin surface, it directly reflects the rate at which water evaporates from the skin to the outside, with units of grams per square meter per hour (g·m²). -2 ·h -1 A higher TEWL value indicates a more severe impairment of the skin barrier function.
[0134] 3.3 Test Procedure: a) Regional markers and barrier damage: Two test areas, each measuring 3cm × 3cm, were marked on the inner side of the volunteer's forearm.
[0135] Reproducible skin barrier damage was induced using an adhesive tape peel-off method. Standard pressure-sensitive adhesive tape (such as D-Squame®) was repeatedly applied and removed (approximately 15-20 times) at the same site until the TEWL value of the area stabilized at 25 g·m². -2 ·h -1 The above indicates that the skin barrier has been successfully damaged.
[0136] b) Initial value measurement (T0): Immediately after the damage is completed, the TEWL values of the two damaged areas are measured using a Tewameter as the initial values of the barrier damage.
[0137] c) Sample application: Randomly select a damaged area as the sample area, apply the sample evenly, and use an amount of 2.0 mg / cm². 2 The other damaged area served as a blank control area and was left untreated.
[0138] Measurement time points: TEWL values were measured in two areas at 6 hours and 24 hours after application.
[0139] 3.4 Data Analysis: Calculate the TEWL values for the sample area and control area at each time point.
[0140] Calculate the decrease in TEWL value of each region relative to the initial value (T0). The larger the decrease, the faster the barrier recovers.
[0141] Paired T-tests were performed using SPSS software to compare the TEWL values and decrease values between the sample area and the control area at the same time point to determine if there were statistically significant differences (p<0.05 was considered statistically significant).
[0142] 4. Experimental Data and Results: Table 4. Data Recording of Changes in Skin Barrier Function (TEWL Value) (n=28, Unit: g·m) -2 ·h -1 )
[0143] Sample area: TEWL values decreased rapidly within 6 hours, and after 24 hours were close to normal skin levels (normal skin TEWL values are typically <15 g·m²). -2 ·h -1 ( ), showing a rapid and sustained recovery.
[0144] Control area: The TEWL value also recovered naturally over time, but slowly. After 24 hours, it was still significantly higher than that of the sample area, indicating that the barrier was not completely repaired.
[0145] 5. Experimental Conclusion: Based on the above TEWL data, the following conclusions are drawn regarding the skin barrier repair effect of the sample in Example 2: Six hours after barrier damage, the TEWL value of the sample area decreased by 8.2 g·m⁻¹. -2 ·h -1 ) is the control area (3.8 g·m -2 ·h -1 The effect was 2.2 times greater than that of the previous product, and the difference was statistically significant (p<0.001). This demonstrates that the product can accelerate the barrier repair process and has a good repair effect in the early stages of repair.
[0146] In the barrier repair experiment, the TEWL value recovery of the sample group within 24 hours was significantly better than that of the blank control group (p<0.001), and its barrier repair rate was approximately 1.64 times that of natural repair. This result indicates that the formulation of this invention not only forms a protective film on the skin surface, but its rich content of sterols, fatty acids, and other lipid components similar to those in the skin may also actively participate in and accelerate the reconstruction process of the skin barrier lipid structure, demonstrating a repairing rather than simply sealing effect.
[0147] The natural recovery of the control area represents the skin's self-healing ability. The sample area recovered much faster than the control area, proving that the gel not only forms an effective protective film on the skin surface, reducing further moisture loss and creating a favorable environment for barrier self-healing; its components, such as shea butter and jojoba seed oil, have a lipid composition similar to skin sebum, which can directly replenish intercellular lipids and actively participate in and promote the reconstruction of barrier lipid structure.
[0148] Experimental Example 5: Evaluation of Anti-wrinkle Effect (In Vitro Enzyme Activity Inhibition Assay) 1. Experimental objective: This experiment uses in vitro biochemical tests to evaluate the inhibitory effect of the sample of this invention on the activity of two key aging-related enzymes in the skin—elastase and collagenase—thereby predicting its potential anti-wrinkle efficacy.
[0149] 2. Test Samples and Reagents: Test sample: The self-forming rose gel prepared in Example 2 is a solid gel that is milky white to slightly yellow and has a fine and uniform texture.
[0150] Sample pretreatment: Accurately weigh 1.00 g of sample and dissolve it in 10 mL of anhydrous ethanol. Vortex to disperse the sample thoroughly, preparing a stock solution of 100 mg / mL. Dilute with the appropriate buffer solution to the required working concentration (0.1, 0.5, 1.0 mg / mL) before use.
[0151] Positive control: Elastase inhibition assay: arbutin; Collagenase inhibition test: Vitamin C; Test reagents: Porcine pancreatic elastase (activity: ≥10 U / mg); Collagenase (from Clostridium histolytica, activity: ≥1,250 U / mg); Substrate: N-succinyl-alanine-alanine-alanine-p-nitroaniline (for elastase). Substrate: N-[3-(2-furanyl)acryloyl]-leucyl-glycyl-prolyl-alanine (FALGPA, for collagenases); Tris-HCl buffer, Tricine-NaOH buffer; 3. Experimental methods and procedures: 3.1 Elastase inhibition assay: Principle: Elastase hydrolyzes the substrate N-succinyl-alanine-alanine-alanine-p-nitroaniline, releasing yellow p-nitroaniline. The rate of increase in absorbance at 410 nm is measured to reflect enzyme activity. The stronger the inhibitory effect of the sample on the enzyme, the lower the absorbance value.
[0152] Solution preparation: Buffer solution: 0.2 M Tris-HCl buffer, pH 8.0.
[0153] Elastase solution: Prepared using the above buffer solution to a final concentration of 0.2 U / mL.
[0154] Substrate solution: Prepare N-succinyl-alanine-alanine-alanine-p-nitroaniline with buffer solution to a final concentration of 0.8 mM.
[0155] Sample / control solutions: Dilute the stock solution with buffer to the desired working concentration (0.1, 0.2, 0.5, 0.8, 1.0 mg / mL).
[0156] Experimental steps: In a 96-well plate, add the components in the following order and volume (total volume 100 μL): Assay group: 140 μL buffer solution + 20 μL sample solution + 20 μL enzyme solution.
[0157] Enzyme background control group: 140 μL buffer + 20 μL buffer (replaces sample) + 20 μL enzyme solution.
[0158] Sample background control group: 160 μL buffer + 20 μL sample solution + 20 μL buffer (instead of enzyme).
[0159] Blank control group: 180 μL buffer + 20 μL buffer (in place of sample and enzyme).
[0160] After gently mixing the reaction mixture, incubate it in a 37°C microplate reader for 10 minutes. Quickly add 20 μL of substrate solution to each well to initiate the reaction.
[0161] At the same time, at 37°C, the absorbance value was measured every 30 seconds at a wavelength of 410 nm, and the monitoring was continued for 20 minutes.
[0162] Data processing: Calculate the linear slope (ΔA / min) of the absorbance value of each reaction well as the change over time.
[0163] Formula for calculating enzyme activity inhibition rate (%): Inhibition rate (%) = [1 - (ΔA / min of assay group - ΔA / min of sample background group) / (ΔA / min of enzyme background group - ΔA / min of blank group)] × 100% Calculate the half-maximal inhibitory concentration (IC50). 50 ).
[0164] 3.2 Collagenase inhibition test: Principle and Method: Similar to the elastase inhibition assay, collagenase and its specific substrates are used to detect changes in absorbance at a specific wavelength.
[0165] Solution preparation: Buffer solution: 50 mM Tricine-NaOH buffer containing 0.4 M NaCl and 10 mM CaCl2, pH 7.5.
[0166] Enzyme solution: Freshly prepared with buffer solution, with a final concentration of 0.5 U / mL.
[0167] Substrate solution: Prepare FALGPA with buffer solution to a final concentration of 1.0 mM.
[0168] Sample / control solution: Preparation method is the same as 3.1.
[0169] Experimental steps: The order and volume of sample addition are the same as in 3.1. Collagenase and its corresponding buffer and substrate are used.
[0170] After mixing, incubate at 37°C for 10 minutes.
[0171] After adding the substrate to initiate the reaction, the rate of decrease in absorbance was continuously monitored at 37°C and 345 nm for 20 minutes.
[0172] Data processing: Calculate the slope (ΔA / min) of the absorbance value of each reaction well as the change over time. Since the absorbance decreases after the substrate is hydrolyzed, the slope is negative, and the absolute value is used for comparison in the calculation.
[0173] Inhibition rate calculation formula and IC 50 The calculation method is the same as in 3.1.
[0174] 4. Experimental Data and Results Table 5. Inhibitory activity of Example 2 against elastase and collagenase (n=3)
[0175] 5. Experimental Conclusion: In Example 2 of this invention, within a test range of 0.10 to 1.00 mg / mL, the inhibition rates of elastase and collagenase increased from 22.5% to 84.2% and from 18.9% to 79.6%, respectively, exhibiting a highly significant dose-dependent effect (p<0.01). This demonstrates that the sample contains components capable of directly and effectively inhibiting the activity of these two key skin aging enzymes.
[0176] IC50 of the sample against elastase and collagenase 50 The values were 0.55 mg / mL and 0.68 mg / mL, respectively, which are similar, indicating that it has a balanced and synergistic inhibitory effect on the two main enzyme systems that degrade the skin's elastin network and collagen scaffold, which helps to more comprehensively delay skin laxity and wrinkle formation caused by dermal matrix degradation.
[0177] Although the positive controls (arbutin and vitamin C) showed higher activity per unit mass (lower IC50), 50 However, Example 2 achieved an inhibition rate of approximately 80% at a concentration of 1.0 mg / mL, indicating that when used topically, the product can effectively deliver sufficient activity intensity to the target site and exert its anti-wrinkle potential.
[0178] Experiment Example 6: Soothing Effect Test (In Vitro Anti-inflammatory Test) 1. Experimental objective: This experimental example uses an in vitro cell model to quantitatively evaluate the inhibitory effect of the present invention on the expression of inflammatory factors, thereby predicting its potential soothing and anti-inflammatory effects.
[0179] 2. Test Samples and Materials: Test sample: The self-forming rose gel prepared in Example 2 is a solid gel that is milky white to slightly yellow and has a fine and uniform texture.
[0180] Sample pretreatment: Accurately weigh 1.00 g of sample and dissolve it in 10 mL of dimethyl sulfoxide (DMSO) to prepare a stock solution of 100 mg / mL. Before use, serially dilute with cell culture medium to ensure that the final DMSO concentration in the culture medium is below 0.1% (non-toxic to cells). Test concentrations are set at 0.1%, 0.05%, and 0.01%.
[0181] Cell line: Human immortalized keratinocytes (HaCaT cells).
[0182] Inducer: Lipopolysaccharide (LPS), used to induce cellular inflammation models.
[0183] Positive control: Dexamethasone (a potent glucocorticoid).
[0184] Main reagents: cell culture medium, RNA extraction kit, reverse transcription kit, and reagents for real-time quantitative PCR (RT-qPCR).
[0185] 3. Experimental methods and procedures: 3.1 Cell Culture and Establishment of Inflammation Model: HaCaT cells were routinely cultured in DMEM medium containing 10% fetal bovine serum in a 37°C, 5% CO2 incubator.
[0186] The cells were seeded at an appropriate density in a culture plate, and the experiment was conducted when the cells grew to 70-80% confluence.
[0187] Experimental Groups: Blank control group: normal cells, without lipopolysaccharide (LPS) and samples.
[0188] Model control group: An inflammation model was established by adding lipopolysaccharide (LPS) (1 μg / mL) for stimulation.
[0189] Sample groups: samples of different concentrations (0.01%, 0.05%, 0.1%) were added for pretreatment for 1 hour, and then lipopolysaccharide (LPS) (1 μg / mL) was added for co-culturing.
[0190] Positive control group: Pretreated with dexamethasone (10 μM) for 1 hour, then co-cultured with lipopolysaccharide (LPS) (1 μg / mL).
[0191] Cells from all groups were collected 24 hours after lipopolysaccharide (LPS) stimulation for subsequent testing.
[0192] 3.2 RNA extraction and real-time quantitative PCR (RT-qPCR): Total RNA was extracted from cells in each group using the TRIzol method, and the purity and concentration of RNA were determined. RNA was then reverse transcribed into cDNA.
[0193] RT-qPCR was performed to detect the mRNA expression levels of key inflammatory factors interleukin-6 (IL-6) and tumor necrosis factor-α (TNF-α).
[0194] Using the housekeeping gene GAPDH as an internal reference, the relative expression level of the target gene mRNA was calculated using the 2^(-ΔΔCt) method.
[0195] 3.3 Data Processing: With the relative mRNA expression level of the model control group as 100%, the inhibition rate of inflammatory factor expression in each sample group and the positive control group was calculated.
[0196] Inhibition rate (%) = [1 - (relative expression level in sample group / relative expression level in model control group)] × 100% 4. Experimental Data and Results: Table 6 Results of the inhibition rate test of inflammatory factor mRNA expression (n=3)
[0197] Example 2: The inhibition of both IL-6 and TNF-α showed a clear dose-dependent effect, with an inhibition rate of approximately 50% at a concentration of 0.1%.
[0198] Dexamethasone: As a potent positive control, it showed extremely strong inhibitory effects (>85%) at a concentration of 10 μM, as expected.
[0199] 5. Experimental Conclusions and Summary 5.1 Conclusion Based on the data from the above in vitro cell inflammation model, the following conclusions are drawn regarding the potential soothing and anti-inflammatory effects of the sample in Example 2: At a test concentration of 0.1%, the sample inhibited the mRNA expression of two key pro-inflammatory factors, IL-6 and TNF-α, by 52.7% and 49.1%, respectively. This indicates that the active ingredient in the sample can effectively intervene in the LPS-induced inflammatory response pathway and downregulate the gene expression of pro-inflammatory factors.
[0200] Within the concentration range of 0.01% to 0.1%, the inhibitory effects of the sample on IL-6 and TNF-α increased with increasing concentration, exhibiting a good dose-dependent effect. This demonstrates that its anti-inflammatory effect is specific and moduloable, rather than caused by non-specific cytotoxic effects.
[0201] The sample was able to simultaneously inhibit IL-6 and TNF-α, factors that play a central role in the inflammatory network. IL-6 is involved in both acute and chronic inflammation, while TNF-α is an initiator of the inflammatory response. This multi-target inhibition gives the product a broader soothing effect.
[0202] Compared to the potent drug dexamethasone (inhibition rate >85%), the sample's approximately 50% inhibition rate represents a gentle yet effective regulatory effect. This aligns with the skincare product's goal of providing gentle soothing relief and maintaining skin's immune balance, avoiding potential side effects from excessive immune suppression. It is more suitable for daily care and long-term use on sensitive skin.
[0203] 5.2 Summary: In vitro enzyme activity inhibition assays confirmed that the extract of this invention effectively inhibits the activity of elastase and collagenase in a dose-dependent manner, revealing at the molecular level that this invention possesses direct anti-wrinkle efficacy. Simultaneously, cellular anti-inflammatory models showed that the extract significantly downregulated the gene expression of inflammatory factors IL-6 and TNF-α. These in vitro experimental results collectively demonstrate that this self-formed rose jelly possesses both anti-wrinkle and soothing effects.
[0204] Experiment Example 7: Safety Evaluation (Human Patch Test) 1. Experimental objective: This experiment aims to objectively evaluate, through a closed patch test on human skin, whether the present invention has any potential irritant or sensitizing effects on human skin under normal use conditions, so as to ensure its safe use.
[0205] 2. Test sample: Test sample: The self-forming rose gel prepared in Example 2 is a solid gel that is milky white to slightly yellow and has a fine and uniform texture.
[0206] Control group: Negative control group: Vaseline.
[0207] Positive control group: 1% sodium dodecyl sulfate (SLS) aqueous solution, used to confirm the effectiveness of the test system.
[0208] 3. Experimental methods and procedures: 3.1 Volunteer Screening: Fifty-three healthy female volunteers, aged 18-60, were selected, including those with normal skin and those who reported having sensitive skin.
[0209] Exclusion criteria: Active inflammation, injury, skin disease, or severe acne at the test site; history of severe allergies (such as allergic asthma, severe contact dermatitis); currently taking antihistamines, immunosuppressants, or glucocorticoids; pregnant or breastfeeding women; or having participated in other clinical trials within the past month.
[0210] Informed consent: All volunteers signed a written informed consent form before the trial. This trial protocol was reviewed and approved by the ethics committee.
[0211] 3.2 Test Procedure: a) Sample preparation: The sample (Example 2) and the negative control (Vaseline) were respectively placed into a standard Finn Chamber, with a dosage of approximately 20 mg.
[0212] b) Application: The loaded spot tester is applied to the normal skin on both sides of the spine on the volunteer's back, and pressed firmly by hand to ensure close contact.
[0213] c) Closure time: The spot tester is continuously applied for 24 hours.
[0214] d) Removal and Observation: First observation (T1, 30 minutes after removal): Carefully remove the patch applicator and mark the application site. Wait 20-30 minutes for the pressure marks to dissipate, then have a professional dermatologist or a trained assessor observe the skin reaction under adequate natural or artificial light.
[0215] Second observation (T2, 24 hours after removal): A second observation was performed on the same site approximately 24 hours after the patch was removed (i.e., 48 hours after the start of the application).
[0216] Third observation (T3, 48 hours after removal): If necessary, a third observation may be performed 48 hours after removal to confirm the outcome of the suspected reaction.
[0217] 3.3 Skin Reaction Scoring Criteria: Scoring was conducted based on the "Cosmetic Safety Technical Specifications" (2015 edition):
[0218] Stimulus response score = ∑ (highest scores of all volunteers at T1, T2, and T3) / (total number of participants × 3) When the irritation response score is ≤ 0.4 and no cases of persistent (not subsided by the T3 observation point) adverse skin reaction occur, the sample can be determined to be non-irritating to the skin.
[0219] 4. Experimental Data and Results Table 7-1 Human Patch Test Skin Reaction Record Table (n=53)
[0220] Table 7-2 Statistical Table of Patch Test Results
[0221] 5. Experimental Conclusions and Summary Based on data from a 48-hour closed patch trial involving 53 volunteers, the following conclusions were drawn regarding the skin safety of the samples from Example 2: Of all 53 participants, no adverse skin reactions (erythema, edema, papules, etc.) occurred, either 30 minutes or 24 hours after patch removal. Therefore, the irritation response score of the sample was 0.00, which is far below the "non-irritating" criterion (≤ 0.4) in the Cosmetic Safety Technical Specifications.
[0222] The study included volunteers who reported having sensitive skin, and no adverse reactions were observed in this group. This indicates that the product's formula is gentle and highly compatible and safe for sensitive skin.
[0223] The negative control (Vaseline) also did not elicit any reaction, ruling out the possibility of false positive results due to the spot tester itself or the operation process, thus proving the reliability of the test results.
[0224] The above description is merely a specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any person skilled in the art can easily conceive of various variations or substitutions within the technical scope disclosed in the present invention, and these should all be included within the scope of protection of the present invention. Therefore, the scope of protection of the present invention should be determined by the scope of the claims.
Claims
1. A self-molding rose confectionery based on oil and fat compounding, characterized in that, Composed of the following components in percentage by mass: avocado butter: 55.0%~62.0%; jojoba seed oil: 38.0%~42.0%; butternut oil: 0.5%~2.0%; rose oil: 0.1%~0.3%.
2. A self-moulding rose-petal fat based compound according to claim 1, characterised in that, The component mass percentage is: avocado butter 58.84%, jojoba seed oil 40%, butternut oil 1%, rose oil 0.16%.
3. A method of preparing a self-forming rose-petal gel as claimed in any one of claims 1-2, characterized in that, Comprising the following steps: S1. Base oil melting: heat and melt the avocado butter to a substantially clear and transparent liquid state at a constant temperature of 40~42℃ to form a liquid base; S2. First phase mixing and homogenization: add jojoba seed oil to the liquid base, maintain the temperature at 40~42℃, and stir at a low speed of 30~50rpm for 20~25min until the mixture is uniform, obtaining a first phase mixture; S3. Second phase introduction and structure excitation: add butternut oil to the first phase mixture, increase the stirring speed to 100~200rpm at 38~40℃, and continue stirring for 20~25min for homogenization, use the interaction of the unsaturated fatty acids rich in butternut oil and the aforementioned oil system to preliminarily excite the structuring potential of the system, obtaining a second phase mixture; S4. Active component low-temperature embedding: cool the second phase mixture to 32~35℃, add rose oil, and reduce the stirring speed to 20~30rpm, and gently stir for 5-10min to ensure that the active essential oil components are uniformly dispersed and embedded in the oil network structure, obtaining a final mixture; S5. Self-forming solidification: place the final mixture in a container in a dust-free and clean environment at 28~30℃, and then naturally cool to room temperature of 23~25℃, and within 4~8 hours, the mixture is self-solidified by the synergistic effect of vegetable oil to form a stable and soft solid-state cream.
4. The method of preparing a composition according to claim 3, characterized in that: In step S3, the stirring is low-speed shear homogenization in a shear emulsifier.
5. The method of making the composition of claim 3, wherein: In step S5, the natural cooling process is carried out in stages: first, stand for 1~2 hours at 28~30℃, and then transfer to a room temperature environment of 23~25℃ to complete the final solidification.
6. Use of the self-forming rose cream according to any one of claims 1-2 or prepared by the method of claims 3-5 in the preparation of skin care products for skin moisturizing, repair, anti-wrinkle, and soothing.