Composition based on circadian rhythm regulation effect, freeze-dried functional liquid, freeze-dried facial mask and preparation methods of composition, freeze-dried functional liquid and freeze-dried facial mask

By using circadian rhythm adjustment compositions and freeze-drying technology in the facial mask, rice fermentation broth, bean seed extract and drought-yrup extract were fixed on a biofiber membrane cloth, solving the poor skin care effect and environmental protection of existing facial masks. The problem has achieved multi-dimensional improvement of the skin and the use of environmentally friendly materials.

CN119139198APending Publication Date: 2024-12-17MAGELINE BIOLOGY TECH CO LTD
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Patent Information

Application Number
CN202411150358.2
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-08-21
Publication Date
2024-12-17

AI Technical Summary

Technical Problem

The existing masks did not fully consider the impact of circadian rhythm on the skin during design, which generally became mediocre in skin care, and it was difficult to achieve efficient penetration and absorption of active ingredients. Some mask materials were difficult to degrade, affecting environmental protection.

Method used

Using compositions based on circadian rhythm regulation, including rice fermentation broth, bean seed extract and drought-yellow lotus extract, the active ingredient is fixed on the biofiber membrane cloth through lyophilization technology, and combined with ultra-low temperature sublimation technology to achieve the active ingredient Efficient release and absorption, and reduce environmental burden through degradable materials of biofiber membrane cloth.

Benefits of technology

Significantly improve skin roughness, reduce wrinkles, improve skin firmness and relieve sensitivity, provide comprehensive nourishment and protection, effectively combat skin aging problems, and achieve environmentally friendly facial mask material degradation.

✦ Generated by Eureka AI based on patent content.

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Patent Text Reader

Abstract

The invention discloses a composition based on a circadian rhythm regulation effect, a freeze-dried functional solution, a freeze-dried mask and a preparation method. The composition is prepared from a rice fermentation solution, a lens culinaris seed extract and a trollius chinensis bunge extract in a mass ratio of (0.1-10): (0.1-3): (0.01-5). Freeze-dried functional liquid is fixed on mask cloth of the mask, and the freeze-dried functional liquid contains rice fermentation liquid, a lens culinaris seed extract and a trollius chinensis bunge extract. Compared with the prior art, from the four dimensions of roughness improvement, wrinkle reduction, skin compactness improvement and sensitivity relief, comprehensive nourishing and protection are provided for the skin, and the skin aging problem is effectively resisted.
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Description

Technical Field

[0001] The present invention belongs to the technical field of cosmetics, and in particular relates to a composition based on circadian rhythm regulation efficacy, a freeze-dried efficacy liquid, a freeze-dried facial mask and a preparation method. Background Art

[0002] As an endogenous time regulation mechanism of organisms, circadian rhythm has a profound impact on various physiological functions of the body by regulating processes such as gene expression, hormone secretion and cell metabolism. It enables organisms to predict and adapt to periodic changes in the environment, such as the alternation of day and night. In the human body, circadian rhythm is dominated by the suprachiasmatic nucleus (SCN) located in the hypothalamus. This nucleus acts as a "master clock" and can synchronize the "sub-clocks" in peripheral tissues, thereby coordinating the expression of circadian rhythm throughout the body.

[0003] In the skin, circadian rhythm also plays a vital role. Skin cells, including keratinocytes, fibroblasts and melanocytes, all show obvious circadian rhythm oscillations. This oscillation not only affects cell proliferation, differentiation and migration, but also regulates physiological processes such as skin barrier function, antioxidant defense mechanism and pigmentation. Nighttime is the peak period for skin cell repair and regeneration, while during the day, the skin is more involved in resisting external environmental stress and ultraviolet radiation.

[0004] At present, although many traditional facial masks contain a variety of skin care ingredients, due to the material or formula of the membrane cloth, these ingredients are difficult to effectively penetrate into the deep layers of the skin, resulting in low absorption efficiency and limited skin care effects; Patent application CN202410328406.6 discloses the use of fermented products of nasturtium callus in delaying skin aging. The fermented products of nasturtium callus have been shown to promote the expression of COL-1 in HDF cells in both states (the highest promotion rate is 56.25%), downregulate the level of MMP-1, and show surprising anti-aging activity. However, the preparation process involves multiple steps, including inducing callus, crushing, extraction, fermentation, etc. These steps require a high degree of operational precision and environmental condition control, which increases the complexity and cost of preparation. In addition, the circadian oscillation of skin cells has an important influence on the function and aging process of the skin, and this technology does not fully consider the impact of circadian rhythm on the skin.

[0005] In fact, most facial masks are not designed with full consideration of the impact of circadian rhythm on the skin, and fail to provide precise skin care based on the specific needs of the skin at different time periods, resulting in generally mediocre skin care results.

[0006] Some facial masks may have problems such as the essence flowing easily and the mask cloth not sticking well during use, which affects the user experience and reduces the skin care effect;

[0007] Some facial mask materials are difficult to degrade, which poses a burden to the environment after use and does not meet the modern consumers' pursuit of environmental protection.

[0008] Patent CN202111344537.6 discloses a composition for regulating circadian rhythm and its application, comprising components: coenzyme Q10, rice extract, albizzia bark extract, and sea buckthorn extract. The composition for regulating circadian rhythm complements each other in exerting the three-in-one effects of defense, moisturizing, and repair. It can effectively protect the skin from light damage during the day and moisturize and repair the skin at night, forming a cyclic process to regulate the skin's rhythm, thereby restoring the skin to a stable and healthy state. This patent only solves a single or limited skin care effect, such as moisturizing and repairing, and fails to effectively combat skin aging problems; it lacks innovation in product preparation technology and fails to achieve efficient and intensive release and absorption of active ingredients. Summary of the invention

[0009] The purpose of the present invention is to overcome the defects of the above-mentioned prior art and to provide a composition based on circadian rhythm regulation function, a freeze-dried effective liquid, a freeze-dried mask and a preparation method, which provide comprehensive nourishment and protection for the skin from four dimensions: roughness improvement, wrinkle reduction, skin firmness enhancement and sensitivity relief, and effectively combat skin aging problems.

[0010] The purpose of the present invention can be achieved by the following technical scheme: a composition based on circadian rhythm regulation efficacy, the composition comprising: rice fermentation liquid, lentil seed extract, and nasturtium extract in a mass ratio of (0.1-10): (0.1-3): (0.01-5).

[0011] Furthermore, the mass ratio of the rice fermentation liquid, the lentil seed extract and the nasturtium extract is: (0.5-2): (0.7-1.5): (0.3-1.5).

[0012] The present invention also provides a freeze-dried efficacy liquid containing a composition based on circadian rhythm regulation efficacy, comprising the following components in percentage by weight:

[0013] Phase A:

[0014] Water Remaining

[0015] Xanthan gum 0.1-5.0wt%,

[0016] Mannitol 2.0-3.0wt%,

[0017] Sodium hyaluronate 0.1-1.0wt%,

[0018] Glycerol 0.5-10wt%,

[0019] Butanediol 2.0-3.0wt%,

[0020] Phase B:

[0021] Dipotassium glycyrrhizinate 1.0-2.0wt%,

[0022] 1,2-Pentanediol 0.1-5.0wt%,

[0023] Phase C:

[0024] Rice fermented liquid 0.1-10.0wt%,

[0025] Lentil (LENS ESCULENTA) seed extract 0.1-3.0wt%,

[0026] Tropaeolum majus flower extract 0.01-5.0 wt%.

[0027] The present invention also provides a method for preparing a freeze-dried efficacy liquid, comprising the following steps:

[0028] a: After fully moistening and mixing the rest of the raw materials of phase A, add them into water, stir thoroughly until completely dissolved, and heat to 75-80°C.

[0029] b. Mix the raw materials of phase B and heat to 75-80°C, stirring until completely dissolved.

[0030] c: Add the mixture of step b to the aqueous phase of step a, stir at 250-350 rpm for 3-5 minutes and homogenize at 2500-3500 rpm for 3-10 minutes.

[0031] d. After cooling to 35-38°C, add phase C raw materials, stir at 250-350 rpm and homogenize at 2500-3500 rpm for 3-10 minutes to obtain freeze-dried efficacy liquid.

[0032] The present invention also provides a freeze-dried facial mask containing the freeze-dried efficacy liquid, wherein the freeze-dried efficacy liquid is fixed on the membrane cloth of the freeze-dried facial mask.

[0033] Furthermore, the membrane cloth of the freeze-dried facial mask is a biofiber membrane cloth.

[0034] The present invention also provides a method for preparing a freeze-dried facial mask, wherein the active ingredients of the freeze-dried efficacy liquid are fixed on the membrane cloth by an ultra-low temperature sublimation method.

[0035] Furthermore, the method specifically includes the following steps: spraying the freeze-dried efficacy liquid onto the biofiber facial mask cloth, freezing the membrane cloth at -50 to -40°C for 2 to 4 hours after fully soaking it, vacuum drying, analytical drying, and fixing the active ingredients of the freeze-dried efficacy liquid on the membrane cloth to obtain the product.

[0036] Further, the infiltration conditions are: infiltration at a constant temperature of 50°C-60°C for 10-30 minutes;

[0037] The vacuum drying conditions are as follows: primary drying is performed in a vacuum freeze dryer at a temperature of -40 to -20°C, the vacuum is controlled at 10Pa to 80Pa, and the primary drying time is 8 to 15 hours;

[0038] The analytical drying conditions are as follows: analytical drying is carried out in a freeze dryer at a temperature of 30-50°C, a vacuum control of 10Pa-80Pa, and an analytical drying time of 4-8h.

[0039] Furthermore, vacuum drying removes 85-95 wt % of the moisture of the material, and analytical drying removes the remaining 5-15 wt % of the moisture of the material.

[0040] Compared with the prior art, the present invention has the following beneficial effects:

[0041] 1. The freeze-dried facial mask of the present invention is based on the fusion of circadian rhythm regulation and natural extracts. The active ingredients such as rice fermentation liquid, lentil (LENS ESCULENTA) seed extract, and nasturtium (TROPAEOLUM MAJUS) flower extract are fixed on the biofiber membrane cloth through ultra-low temperature sublimation technology. Combined with the promotion of circadian rhythm on skin repair and regeneration, it can achieve significant improvements in skin roughness, wrinkles, firmness and sensitivity.

[0042] 2. The present invention combines natural, biodegradable biofiber membranes with highly concentrated freeze-dried active ingredients to achieve efficient delivery and absorption of active ingredients. By applying the dry membrane to fully moistened skin, the membrane is rehydrated and in close contact with the skin surface by the activation effect of water, thereby accelerating the deep penetration of active molecules and ensuring the maximum skin care effect.

[0043] 3. The mask of the present invention starts from four dimensions: improving roughness, reducing wrinkles, enhancing skin firmness and alleviating sensitivity. Through comprehensive formula and technological innovation, it provides comprehensive nourishment and protection for the skin and effectively combats skin aging problems.

[0044] 4. The present invention utilizes the circadian rhythm as an endogenous time regulation mechanism of the organism, takes into account the physiological changes of skin cells during the alternation of day and night, and achieves precise skin care.

[0045] Nasturtium extract is used to activate the mitochondrial respiratory chain and stabilize HIF-1α expression, thereby improving the energy supply and metabolic adaptability of skin cells during the day, while promoting cell proliferation and repair at night.

[0046] Lentil extract is introduced and its oligosaccharide components are used to build an efficient moisturizing barrier. The synthesis of type I collagen is promoted by activating the TGF-β / Smad signaling pathway, thereby enhancing the skin's firmness and anti-wrinkle ability.

[0047] Rice fermented liquid is used as the core ingredient, and its rich biochemical components such as succinic acid, choline, amino acids, peptides and polysaccharides are used to comprehensively promote the metabolism, repair and barrier function of skin cells.

[0048] The components work synergistically to regulate gene expression, hormone secretion, cell metabolism and other processes, ensuring that the metabolic activity, repair and regeneration of skin cells and other physiological processes are synchronized with the circadian rhythm, thereby reducing skin aging problems caused by biological clock disorders. DETAILED DESCRIPTION

[0049] The following examples further illustrate various embodiments within the scope of the present invention. These examples are given for illustrative purposes only and are not intended to limit the present invention, as many variations of the present invention may be made without departing from the spirit and scope of the present invention.

[0050] The present invention provides a composition freeze-dried facial mask with circadian rhythm regulation efficacy, wherein the active ingredient of the freeze-dried efficacy liquid is fixed on the membrane cloth, and the active ingredient is fixed on the membrane cloth by the ultra-low temperature sublimation method of the freeze-dried efficacy liquid, and the freeze-dried efficacy liquid contains 0.1-10.0wt% of rice fermentation liquid, 0.1-3wt% of lentil (LENS ESCULENTA) seed extract, and 0.01-5.0wt% of nasturtium (TROPAEOLUM MAJUS) flower extract. The components in the composition have clear efficacy and cooperate with each other, and specifically include:

[0051] 1. Tropaeolum majus, a perennial herb belonging to the Tropaeolaceae family, is rich in polysaccharide complexes, mainly galactoarabinan.

[0052] Tropaeolum majus flower extract is a commercially available product. Tropaeolum majus flower extract significantly improves mitochondrial efficiency and enhances the oxidative phosphorylation process of cells, thereby promoting efficient conversion and utilization of energy. Specifically, Tropaeolum majus flower extract activates the mitochondrial respiratory chain, optimizes the electron transport chain between complexes I to IV, accelerates the synthesis rate of ATP (adenosine triphosphate), and ensures that cells have sufficient energy supply during daytime activities. In addition, Tropaeolum majus flower extract can also stabilize the expression level of HIF-1α (hypoxia-inducible factor-1α), regulate the gene expression pattern related to oxygen sensing and adaptability, and enhance the metabolic adaptability of cells in oxygen-rich environments.

[0053] At night, skin cells enter the peak period of proliferation and repair. Tropaeolum majus flower extract precisely intervenes in the cell cycle regulatory network, especially activates TGF-β / Smad and PI3K / Akt / mTOR signaling pathways, promotes the proliferation and differentiation of keratinocytes, accelerates the synthesis and reconstruction of the extracellular matrix, and thus strengthens the natural repair process of the skin. This mechanism is closely related to the cell activity cycle driven by the circadian rhythm, which helps to achieve efficient repair and regeneration of the skin at night.

[0054] 2. Lens esculenta, belongs to the Fabaceae family. Lens esculenta seed extract is rich in a variety of bioactive ingredients. The oligosaccharide components in Lens esculenta seed extract have excellent moisturizing ability. They optimize the structure and function of the stratum corneum of the skin and build an efficient moisturizing barrier. These oligosaccharide molecules can penetrate into the gaps in the stratum corneum, enhance the binding force of keratinocytes, reduce transepidermal water loss, thereby maintaining the water-oil balance of the skin and improving the softness and elasticity of the skin.

[0055] In addition, as the most important structural protein in the skin, the content of type I collagen gradually decreases with age and the increase of external environmental pressure, leading to sagging skin, fine lines and wrinkles. Oligosaccharides and small molecule peptides in lens esculenta seed extract act on skin cells and significantly upregulate the gene expression of type I collagen by activating the TGF-β / Smad signaling pathway. This process promotes the synthesis and deposition of new collagen fibers in skin cells, strengthens the structural support of the skin, and thus improves the skin's firmness, elasticity and anti-wrinkle ability.

[0056] Lentil seed extract is a commercially available product.

[0057] 3. As a natural product prepared by precision fermentation technology, rice fermentation liquid has complex and diverse biochemical components and contains rich bioactive substances. Its core biochemical components include but are not limited to the following categories:

[0058] Succinic acid, as an important intermediate product in the tricarboxylic acid cycle, exhibits a significant metabolic promoting effect in rice fermentation broth, which can accelerate the energy metabolism process of skin cells and promote cell renewal and repair.

[0059] As an important neurotransmitter precursor, choline also plays a key role in regulating skin lipid metabolism. The choline component in rice fermentation liquid helps optimize the lipid barrier on the skin surface, maintain the water and oil balance of the skin, and reduce the damage to the skin caused by external stimuli.

[0060] Amino acids are the basic units that make up proteins, while polypeptides are small molecule proteins formed by connecting multiple amino acids through peptide bonds. The amino acids and polypeptide components in rice fermentation liquid not only provide necessary nutritional support for skin cells, but also participate in the synthesis and repair process of skin collagen, helping to improve skin elasticity and firmness.

[0061] Polysaccharides, as a type of high molecular carbohydrates, exist in various forms in rice fermentation liquid. They not only have good moisturizing properties, but can also form a protective film on the skin surface to lock in moisture and prevent evaporation; they can also enhance the skin's self-defense ability by strengthening the immune regulation function of skin cells.

[0062] Rice fermented liquid is also rich in a variety of antioxidants, such as vitamins, flavonoids, etc. These ingredients can effectively remove free radicals, reduce the damage of oxidative stress to the skin, and delay the aging process of the skin.

[0063] These biochemical components work synergistically with each other in rice fermentation liquid, which can not only promote the metabolism and repair of skin cells, but also enhance the skin barrier function, improve the skin's moisturizing and defense capabilities, and provide comprehensive nourishment and protection for the skin.

[0064] The rice fermentation liquid used in the present invention can be a commercially available product, or can be prepared by the method reported in existing public literature. The rice fermentation liquid used in the following embodiments is prepared by the method disclosed in CN202211506070.5.

[0065] The mask of the present invention adopts innovative technology to comprehensively combat skin aging problems from four key dimensions: roughness improvement, wrinkle reduction, skin firmness improvement and sensitivity relief. The unique freeze-drying technology is combined with the biofiber membrane cloth to ensure that the active ingredients are efficiently and intensively released into the deep layers of the skin during use, thereby improving the absorption efficiency. Combined with highly effective active ingredients, significant improvements in the skin can be achieved through simple use steps. This is an innovative solution that combines a natural, biodegradable freeze-dried film with highly concentrated active ingredients. When the dry film is applied to the fully moistened skin, the film body is quickly rehydrated under the action of water and comes into close contact with the skin surface, thereby achieving the best adhesion effect. In this process, the polysaccharide chains in the matrix become more fluid, allowing the active molecules to be efficiently and intensively released into the deep layers of the skin, ensuring efficient absorption and utilization of the ingredients.

[0066] The facial mask of the present invention uses biofiber membrane cloth as the membrane cloth, and uses ultra-low temperature sublimation technology to fix active ingredients such as rice fermentation liquid, lentil (LENS ESCULENTA) seed extract, and nasturtium (TROPAEOLUM MAJUS) flower extract in the freeze-dried efficacy liquid on the biofiber membrane cloth, combined with the promotion effect of circadian rhythm on skin repair and regeneration, to achieve significant improvement in skin roughness, wrinkles, firmness and sensitivity.

[0067] The freeze-dried efficacy liquid includes the components in percentage by weight as shown in Table 1 below:

[0068] Table 1. Proportion of freeze-dried efficacy liquid components

[0069]

[0070] Preparation of freeze-dried efficacy solution:

[0071] a: Place water in a container with a stirring device and stir. After fully moistening and mixing the rest of raw material A, add it into the water, stir thoroughly until completely dissolved, and heat to 75-80°C.

[0072] b. Mix raw material B and heat to 75-80°C, stirring until completely dissolved.

[0073] c: Add the mixture of step b to the aqueous phase of step a, stir at 250-350 rpm for 3-5 minutes and homogenize at 2500-3500 rpm for 3-10 minutes.

[0074] d. After the temperature drops to 35-38°C, add combination C, stir at 250-350 rpm and homogenize at 2500-3500 rpm for 3-10 minutes to obtain the desired freeze-dried efficacy liquid. Filter and sterilize before freeze-drying and spray, and test the bacterial content, toxins, immunogenicity, etc. for quality control.

[0075] The preparation method of the freeze-dried facial mask comprises the following steps:

[0076] The freeze-dried efficacy liquid is formulated according to the ingredients of the freeze-dried efficacy liquid, and the freeze-dried efficacy liquid is sprayed onto the biofiber facial mask cloth, and soaked for 10-30 minutes under a constant temperature condition of 50°C-60°C. After sufficient soaking, the membrane cloth is frozen at -50 to -40°C in an ultra-low temperature freeze dryer for 2-4 hours; then it is dried once in a vacuum freeze dryer at a temperature of -40 to -20°C, the vacuum control is 10PA-80PA, the primary drying time is 8-15 hours, and 85-95wt% of the moisture of the material is dried and removed; finally, it is subjected to analytical drying in a freeze dryer at a temperature of 30 to 50°C, the vacuum control is 10PA-80PA, the analytical drying time is about 4-8h, and the remaining 5-15wt% of the moisture of the material is dried and removed. At this time, the active ingredients of the freeze-dried efficacy liquid are fixed on the membrane cloth to obtain the product.

[0077] The following is further described by specific examples:

[0078] Examples 1-3 and Comparative Examples 1-7

[0079] The freeze-dried mask of the composition based on the circadian rhythm regulation effect adopts the formula as described in Table 2:

[0080] Table 2 Ratio of raw material components of Examples 1-3 and Comparative Examples 1-7

[0081]

[0082] The difference between Example 2 and Example 1 is only the increase of each effective ingredient, and the difference between Example 3 and Example 1 is only the reduction of each effective ingredient.

[0083] The difference between Comparative Examples 1-3 and Example 1 is only the lack of one key composition component, the difference between Comparative Examples 4-6 and Example 1 is only the lack of two key composition components, and the difference between Comparative Example 7 and Example 1 is only the lack of all key composition components.

[0084] The preparation methods of the freeze-dried efficacy liquid and freeze-dried facial mask of each embodiment and comparative example are the same as above.

[0085] Efficacy evaluation test

[0086] (I) Cell proliferation effect test

[0087] According to the formula in Table 3, the rice fermentation liquid, lentil seed extract, nasturtium extract and water were evenly mixed to prepare the experimental samples.

[0088] Table 3 Weight distribution ratio of raw material components in the cell proliferation effect test experiment (wt%)

[0089]

[0090] Test method:

[0091] 1) Immortalized human epidermal cells (HaCat) were cultured at 10 3 -10 4 The cells were seeded at a density of 100 cells / well in a 96-well plate, 100 μL of DMEM medium was added to the wells, and the cells were incubated in CO 2 Incubate at 37°C in an incubator for 24 hours.

[0092] 2) The experimental samples of Experimental Examples 1-3 and Blank Examples 1-7 were added to the plate and incubated in an incubator for 48 hours.

[0093] 3) Use a repeating pipette to add 10 μL of CCK8 solution to each well of the culture plate and incubate the culture plate in an incubator for 1-4 hours.

[0094] 4) Use an ELISA reader to measure the absorbance at 450 nm and create a standard curve for data analysis.

[0095] 5) Using blank example 7 as a reference, calculate the cell proliferation change rate, cell proliferation change rate (%) = (test group absorbance - blank example 7 absorbance) / blank example 7 absorbance * 100%. The test results are shown in Table 4 below.

[0096] Table 4 Cell proliferation rate change

[0097] sample Cell proliferation rate (%) Experimental Example 1 42.51 Experimental Example 2 48.73 Experimental Example 3 33.68 Blank example 1 24.25 Blank example 2 22.73 Blank example 3 21.06 Blank example 4 16.23 Blank example 5 13.77 Blank example 6 15.17 Blank example 7 0.00

[0098] As shown in Table 4, after cell culture using the experimental samples of Experimental Examples 1-3 and Blank Examples 1-6, the cell proliferation rate is significantly improved. However, compared with Blank Examples 1-6, the improvement effect of Experimental Examples 1-3 is more significant. As can be seen from the comparison of the results, compared with the composition without circadian rhythm regulation effect (Blank Example 7), or only using one or two of Lens Esculenta seed extract, Tropaeolum majus flower extract and rice fermented liquid (Blank Examples 1-6), when Lens Esculenta seed extract, Tropaeolum majus flower extract and rice fermented liquid are used at the same time (Experimental Examples 1-3), the cell proliferation rate improvement effect is more obvious. It shows that Lens Esculenta seed extract, Tropaeolum majus flower extract and rice fermented liquid have a synergistic effect, which has the effect of improving cell viability and delaying cell aging.

[0099] (II) Safety Testing

[0100] 1) Test sample: freeze-dried efficacy liquid of Examples 1-3 and Comparative Examples 1-7 described in Table 2.

[0101] 2) Number of participants: 110 participants, half male and half female, aged between 20 and 45 years old, all meeting the criteria for subjects.

[0102] 3) Test method: 110 subjects who met the test criteria were randomly divided into 11 groups, and the corresponding test subjects used the freeze-dried efficacy liquid obtained in Examples 1-3 and Comparative Examples 1-7 described in Table 2, and the blank group 1 was not smeared with any sample, with 10 subjects in each group; the safety was tested by a third-party testing agency. The selected area should not exceed 50mm 2, a suitable patch with a depth of about 1mm, add about 0.02-0.025ml (g) of the test substance into the patch tester by the closed patch test method. The patch tester is attached to the curved side of the subject's forearm, and the test substance is removed after 24 hours. The skin reaction is observed at 0.5h, 24h, and 48h after removal: the results are recorded according to the skin reaction grading standards in the "Cosmetic Safety Technical Regulations 2015".

[0103] Table 5 Patch test results

[0104]

[0105]

[0106] Note: Skin reaction grading standards:

[0107] Grade 0: negative reaction;

[0108] Grade 1: Suspicious reaction; only slight erythema;

[0109] Grade 2: weak positive reaction (erythema reaction); erythema, infiltration, edema, and papules may be present;

[0110] Grade 3: Strong positive reaction (herpes reaction); erythema, infiltration, edema, papules, herpes: the reaction may extend beyond the test area;

[0111] Grade 4: Extremely strong reaction (confluent herpes reaction): obvious erythema, severe infiltration, edema, confluent herpes, and the reaction exceeds the test area.

[0112] 4) Test results: The results in Table 5 show no irritation and pass the safety test.

[0113] (III) Stability test

[0114] 1) Test sample: the freeze-dried efficacy liquid of Examples 1-3 described in Table 2.

[0115] 2) Test method: Internal control standard, observe the appearance color, viscosity and pH for three months.

[0116] Table 6 Stability test results

[0117] time 45℃ 40℃ 37℃ 25℃ 5℃ -15℃ CYCLE illumination 1W √ √ √ √ √ √ √ √ 2W √ √ √ √ √ √ √ √ 3W √ √ √ √ √ √ √ √ 4W √ √ √ √ √ √ √ √ 2M √ √ √ √ √ √ √ √ 3M √ √ √ √ √ √ √ √

[0118] Among them, W stands for week, M stands for month, and "CYCLE" refers to cycle. The cycle setting is: heating from -15℃ to 45℃, and cooling from 45℃ to -15℃ for five times.

[0119] 3) Test results: The results in Table 6 show that the freeze-dried efficacy liquid in Examples 1-3 is stable in properties within 3 months.

[0120] (IV) Evaluation of anti-aging effects

[0121] 1) Test samples: freeze-dried facial masks of Examples 1-3 and freeze-dried facial masks of Comparative Examples 1-7.

[0122] 2) Test subjects: 100 healthy women (23-45 years old, average age 34.6 years old) were randomly divided into 10 groups, each with 10 people, regardless of gender, and each group used the same formula product. Written informed consent was signed. Before enrollment, a series of questions about medical history and health status were asked according to the inclusion and exclusion criteria. At the same time, the skin of the test site was evaluated for compliance and skin color test screening, and the results were recorded;

[0123] Environmental conditions: During the test, visual assessment and instrument testing are carried out in an environment with a temperature of 21±1℃ and a relative humidity of 50±10% RH. Visual assessment is carried out under constant lighting conditions (fluorescent lamps or LED lighting with a color temperature of 5500-6500K). The subjects need to adapt to this environmental condition for at least 30 minutes before evaluation and testing can be carried out.

[0124] 3) Test method: Use the samples every night, apply the freeze-dried masks of Examples 1-3 and Comparative Examples 1-7 on the face, tear off the masks after 15 minutes, and do not need to be washed off. The test lasts for 4 weeks. The subjects apply sunscreen products on the entire face every morning.

[0125] The test results were taken at the following three time periods: before using the sample (D0), 14 days after using the sample (D14), and 28 days after using the sample (D28).

[0126] 4) Test items are:

[0127] ①Primos is used for facial image acquisition;

[0128] ②Corneometer CM825 is used to collect the moisture content of the stratum corneum;

[0129] ③ MPA580 is used for skin tightening collection.

[0130] 5) The test results can be calculated using the following formula:

[0131] Change rate = (average analysis value of 10 people in each group after using the product - average analysis value of 10 people in each group before using the product) ÷ average analysis value of 10 people in each group before using the product × 100%

[0132] 6) Test results

[0133] ① Skin wrinkles (outer corners of eyes)

[0134] Primos CR was used to collect facial images, skin wrinkles and photo analysis, and the test results are shown in Table 7. The smaller the analysis value, the better the skin wrinkles.

[0135] Table 7 Skin wrinkle Ra value change rate

[0136]

[0137]

[0138] As shown in Table 7, after using the freeze-dried mask, the change rate of the Ra value of skin wrinkles in Examples 1-3 and Comparative Examples 1-6 decreased with the extension of the use time, indicating that the skin wrinkles were improved. However, compared with Comparative Examples 1-6, when used for the same time, the change rate of the Ra value of skin wrinkles in Example 1-3 was greater, indicating that the improvement effect of skin wrinkles after using the freeze-dried mask of Example 1-3 was more significant. There was no obvious improvement in the skin wrinkles of Comparative Example 7.

[0139] From the comparison of the results of Examples 1-3 and Comparative Examples 1-7, it can be seen that when Lens Esculenta seed extract, Tropaeolum Majus flower extract and rice fermentation liquid are used simultaneously, the improvement effect of skin wrinkles is better than that of the composition without circadian rhythm regulation effect, or only one or two of Lens Esculenta seed extract, Tropaeolum Majus flower extract and rice fermentation liquid. This shows that Lens Esculenta seed extract, Tropaeolum Majus flower extract and rice fermentation liquid have a synergistic effect, can effectively improve skin wrinkles, and have an anti-aging effect.

[0140] ②Test results of moisture content of stratum corneum (Corneometer CM825)

[0141] Corneometer CM825 was used to collect the moisture content of the stratum corneum. The results are shown in Table 8. The higher the measured value, the higher the moisture content of the stratum corneum of the skin.

[0142] Table 8 Change rate of moisture content in stratum corneum

[0143]

[0144]

[0145] As shown in Table 8, after using the freeze-dried mask, as the use time increases, the change rate of the water content of the stratum corneum of the skin of Examples 1-3 and Comparative Examples 1-7 increases, indicating that the water content of the stratum corneum of the skin has improved. However, compared with Comparative Examples 1-7, when used for the same time, the change rate of the water content of the stratum corneum of Example 1-3 is greater, indicating that the improvement effect of the water content of the stratum corneum of the skin after using the freeze-dried mask of Example 1-3 is more significant.

[0146] From the comparison of the results of Examples 1-3 and Comparative Examples 1-7, it can be seen that when Lens Esculenta seed extract, Tropaeolum Majus flower extract and rice fermentation liquid are used simultaneously, the improvement effect of the water content of the stratum corneum of the skin is better than that of the composition without circadian rhythm regulation effect, or only one or two of Lens Esculenta seed extract, Tropaeolum Majus flower extract and rice fermentation liquid. This shows that Lens Esculenta seed extract, Tropaeolum Majus flower extract and rice fermentation liquid have a synergistic effect, can effectively improve the water content of the stratum corneum of the skin, and have an anti-aging effect.

[0147] ③ Skin firming ( MPA580)(Cheek)

[0148] use MPA580 collects facial skin firmness data, and the results are shown in Table 9. The larger the measurement value, the better the skin firmness.

[0149] Table 9 Skin firmness change rate

[0150] sample After 14 days of use % After 28 days of use % Example 1 26.72 38.44 Example 2 28.15 39.79 Example 3 25.33 37.06 Comparative Example 1 20.26 30.15 Comparative Example 2 19.79 29.83 Comparative Example 3 19.41 29.22 Comparative Example 4 16.37 22.69 Comparative Example 5 15.78 21.53 Comparative Example 6 16.03 22.14 Comparative Example 7 12.15 15.21

[0151] From the results in Table 9, it can be seen that after using the freeze-dried mask, as the use time increases, the skin firmness change rate of Examples 1-3 and Comparative Examples 1-7 increases, indicating that the skin firmness has improved. However, compared with Comparative Examples 1-7, when used for the same time, the skin firmness change rate of Example 1-3 is greater, indicating that the improvement effect of the skin firmness after using the freeze-dried mask of Example 1-3 is more significant.

[0152] From the comparison of the results of Examples 1-3 and Comparative Examples 1-7, it can be seen that when Lens Esculenta seed extract, Tropaeolum Majus flower extract and rice fermentation liquid are used simultaneously, the skin firmness improvement effect is better than that of the composition without circadian rhythm regulation effect, or only one or two of Lens Esculenta seed extract, Tropaeolum Majus flower extract and rice fermentation liquid. This indicates that Lens Esculenta seed extract, Tropaeolum Majus flower extract and rice fermentation liquid have a synergistic effect, can effectively improve skin firmness, and have an anti-aging effect.

[0153] In summary, it can be seen that the present invention can affect the expression of biological clock genes in skin cells through the synergistic effect of the effective ingredients of rice fermentation liquid, Lens Esculenta seed extract, and Tropaeolum Majus flower extract. This regulation helps to ensure that the metabolic activities, repair and regeneration of skin cells and other physiological processes are synchronized with the circadian rhythm, thereby reducing skin aging problems caused by biological clock disorders. The metabolic activities of skin cells, such as energy production, nutrient absorption, and waste discharge, are all subject to the fine regulation of circadian rhythms. The ingredients in the present invention regulate circadian rhythms by regulating processes such as gene expression, hormone secretion, and cell metabolism, thereby achieving four dimensions from roughness improvement, wrinkle reduction, skin firmness improvement, and sensitivity relief, providing comprehensive nourishment and protection for the skin, and effectively combating skin aging problems.

[0154] The anti-aging composition of the present invention is processed by freeze-drying technology, the effective ingredients in the essence are quickly frozen at low temperature, and the water is removed by vacuum sublimation to form a freeze-dried powder. This technology can not only effectively retain the activity and stability of the ingredients, but also avoid the problem of liquid flow before the mask is used. Consumers only need to add a small amount of clean water when using it. Under the action of water, the membrane body quickly restores the hydration state and fits tightly to the skin surface to achieve the best adhesion effect. In this process, the polysaccharide chains contained in the matrix show higher fluidity, which promotes the efficient and concentrated penetration of active substances into the deep layers of the skin, ensuring the effective absorption and full utilization of skin care ingredients.

[0155] The freeze-dried facial mask of the present invention adopts a degradable biofiber membrane cloth, which can be naturally degraded after use, reducing the burden on the environment and meeting the pursuit of environmental protection by modern consumers.

[0156] The above description of the embodiments is to facilitate the understanding and use of the invention by those skilled in the art. It is obvious that those skilled in the art can easily make various modifications to these embodiments and apply the general principles described herein to other embodiments without creative work. Therefore, the present invention is not limited to the above embodiments, and improvements and modifications made by those skilled in the art based on the disclosure of the present invention without departing from the scope of the present invention should be within the scope of protection of the present invention.

Claims

1. A composition based on circadian rhythm regulation efficacy, characterized in that: The composition comprises: rice fermentation liquid, lentil seed extract and nasturtium extract in a mass ratio of (0.1-10): (0.1-3): (0.01-5).

2. The composition based on circadian rhythm regulation efficacy according to claim 1, characterized in that: The mass ratio of the rice fermentation liquid, the lentil seed extract and the nasturtium extract is: (0.5-2): (0.7-1.5): (0.3-1.5).

3. A freeze-dried efficacy liquid containing the composition based on circadian rhythm regulation efficacy according to claim 1 or 2, characterized in that: The composition comprises the following weight percentages: Phase A: Water Remaining Xanthan gum 0.1-5.0wt%, Mannitol 2.0-3.0wt%, Sodium hyaluronate 0.1-1.0wt%, Glycerol 0.5-10wt%, Butanediol 2.0-3.0wt%, Phase B: Dipotassium glycyrrhizinate 1.0-2.0wt%, 1,2-Pentanediol 0.1-5.0wt%, Phase C: Rice fermented liquid 0.1-10.0wt%, Lentil (LENS ESCULENTA) seed extract 0.1-3.0wt%, Tropaeolum majus flower extract 0.01-5.0 wt%.

4. A method for preparing the freeze-dried efficacy liquid according to claim 3, characterized in that: The following steps are involved: a: After fully moistening and mixing the rest of the raw materials of phase A, add them into water, stir thoroughly until completely dissolved, and heat to 75-80°C. b: Mix the raw materials of phase B and heat to 75-80°C, stirring until completely dissolved. c: Add the mixture of step b to the aqueous phase of step a, stir at 250-350 rpm for 3-5 minutes and homogenize at 2500-3500 rpm for 3-10 minutes. d. After cooling to 35-38°C, add phase C raw materials, stir at 250-350 rpm and homogenize at 2500-3500 rpm for 3-10 minutes to obtain freeze-dried efficacy liquid.

5. A freeze-dried facial mask containing the freeze-dried efficacy liquid according to claim 3, characterized in that: The freeze-dried effective liquid is fixed on the membrane cloth of the freeze-dried facial mask.

6. The freeze-dried facial mask according to claim 5, characterized in that The membrane cloth of the freeze-dried facial mask is a biofiber membrane cloth.

7. A method for preparing a freeze-dried facial mask as claimed in claim 5, characterized in that: The active ingredients of the freeze-dried efficacy liquid are fixed on the membrane cloth through the ultra-low temperature sublimation method.

8. The preparation method according to claim 5, characterized in that: The specific steps include: The freeze-dried efficacy liquid is sprayed onto the biofiber mask cloth, and after being fully soaked, the mask cloth is frozen at -50 to -40°C for 2 to 4 hours, vacuum dried, and analytically dried, so that the active ingredients of the freeze-dried efficacy liquid are fixed on the mask cloth to obtain the product.

9. The preparation method according to claim 8, characterized in that: The infiltration conditions are: infiltration at a constant temperature of 50°C-60°C for 10-30 minutes; The vacuum drying conditions are as follows: primary drying is performed in a vacuum freeze dryer at a temperature of -40 to -20°C, the vacuum is controlled at 10Pa to 80Pa, and the primary drying time is 8 to 15 hours; The analytical drying conditions are as follows: analytical drying is carried out in a freeze dryer at a temperature of 30-50°C, a vacuum control of 10Pa-80Pa, and an analytical drying time of 4-8h.

10. The preparation method according to claim 8, characterized in that: Vacuum drying removes 85-95 wt% of the moisture in the material, and analytical drying removes the remaining 5-15 wt% of the moisture in the material.