A high-stability soothing composition, a preparation method therefor, and an application thereof

Abstract

The application belongs to the technical field of cosmetics, and discloses a high-stability soothing functional composition and a preparation method and application thereof. The composition comprises active functional components, a natural stable carrier, a natural preservative system and a cosmetically acceptable aqueous base, wherein the active functional components are inclusion EGCG, microcapsule-encapsulated chamomile extract and phospholipid-complexed calendula extract, and a full-natural broad-spectrum preservative system is constructed in a matched manner. Through the synergistic use of triple stabilization technology, the application solves the industry pain points that natural soothing active ingredients are prone to oxidation inactivation, have poor dispersibility, low bioavailability and traditional preservatives are prone to irritating sensitive skin, greatly improves the storage stability and transdermal penetration effect of the active ingredients, and the product is mild and non-irritating, is suitable for industrial large-scale production, and can be widely applied to the preparation of anti-allergy soothing and skin barrier repair cosmetics.

Description

Technical Field

[0001] This invention belongs to the field of cosmetic technology, specifically relating to a highly stable soothing composition, its preparation method, and its application, and is particularly suitable for the development and production of cosmetics for sensitive skin care. Background Technology

[0002] With increasing environmental pollution, irregular lifestyles, excessive cleansing and skincare, and the widespread use of cosmetic procedures, the global population with sensitive skin continues to expand. According to the "Chinese Expert Consensus on the Diagnosis and Treatment of Sensitive Skin," 36.1% of women in my country have sensitive skin, with over 20% experiencing moderate to severe sensitivity. The core pathological characteristics of sensitive skin are a damaged skin barrier, increased nerve sensitivity, and enhanced inflammatory responses. Clinical manifestations include redness, dryness, itching, stinging, visible blood vessels, and burning sensations, placing extremely high demands on the gentleness, safety, and efficacy of skincare products.

[0003] Natural plant-derived active ingredients have become a core focus in the development of skincare products for sensitive skin due to their advantages such as gentleness, low irritation, targeted efficacy, and alignment with consumers' natural skincare philosophy. Among them, EGCG (epigallocatechin gallate) from green tea extract, flavonoids and bisabolol from chamomile extract, and triterpenoid saponins from calendula extract are currently the three most widely used soothing active substances in the cosmetics industry. EGCG achieves anti-allergic and antioxidant effects by inhibiting histamine release, scavenging free radicals, and blocking inflammatory signaling pathways; chamomile extract can quickly relieve skin redness, itching, and burning symptoms, and reduce nerve sensitivity; calendula extract can promote keratinocyte proliferation and repair damaged skin barriers. The combination of these three ingredients achieves a synergistic effect of "immediate soothing + long-lasting repair."

[0004] However, in actual industrial applications, the aforementioned natural active ingredients face four common technical challenges that severely restrict their large-scale application in cosmetics: First, they exhibit extremely poor chemical stability and short shelf life. EGCG, chamomile flavonoids, and calendula triterpenes are all polyphenols and flavonoids, containing numerous phenolic hydroxyl groups in their molecular structure. They are highly susceptible to oxidative degradation due to light, temperature, oxygen, and pH, resulting in product discoloration, off-odors, and rapid loss of activity. In existing technologies, water-based skincare products containing these ingredients retain less than 60% of their activity after 3 months of storage at room temperature, and almost completely lose their activity after 6 months. They are also prone to appearance problems such as sedimentation and layering, resulting in a shelf life generally less than 6 months, failing to meet the 2-3 year shelf-life requirement for cosmetics.

[0005] Secondly, the water solubility and dispersibility are poor, resulting in extremely low bioavailability. EGCG has limited water solubility and is prone to aggregation. Bisabolol, the core active ingredient in chamomile extract, is a fat-soluble substance, and the triterpenoids in calendula extract have extremely poor water solubility. These components are prone to uneven dispersion, aggregation, and sedimentation in water-based skincare products, making it impossible to distribute them evenly in the formulation system. Furthermore, unmodified active ingredients have difficulty penetrating the stratum corneum and reaching the dermis to exert their effects, with a transdermal penetration rate of less than 10%. Even with high doses, the expected soothing and repairing effects cannot be achieved, resulting in significant waste of raw materials.

[0006] Third, there is a core contradiction between natural and safe preservative systems. Skincare products for sensitive skin must strictly avoid the irritation risks posed by traditional chemical preservatives. Traditional preservatives such as parabens, isothiazolinones, and imidazolidinyl ureas can damage the skin barrier structure, causing secondary irritation to sensitive skin and even leading to contact dermatitis, which completely contradicts the development philosophy of products for sensitive skin. Meanwhile, existing natural preservative systems generally suffer from narrow antibacterial spectrum, poor antibacterial effect, and inability to inhibit microbial growth for extended periods, further exacerbating the problem of short product shelf life and failing to achieve a balance between "natural gentleness and long-lasting preservation."

[0007] Fourth, existing stabilization technologies have significant limitations. Currently, most stabilization technologies for natural active ingredients in the industry are single-method approaches, such as using cyclodextrin encapsulation, single microcapsule encapsulation, or liposome encapsulation alone. However, single encapsulation technologies can only address the stability of a single type of ingredient and cannot simultaneously address the stabilization needs of water-soluble polyphenols, fat-soluble flavonoids, and triterpenoids, nor can they simultaneously achieve the multiple effects of "antioxidant protection + uniform dispersion + enhanced penetration and sustained release." Some existing technologies add chemically synthesized antioxidants such as BHT and BHA to improve stability, which not only contradicts the natural product positioning but also poses potential risks of skin irritation.

[0008] In summary, there is currently no technical solution in the industry that can simultaneously address the four core pain points of natural soothing active ingredients: oxidative inactivation, poor dispersibility, low bioavailability, and irritation from preservative systems. It is impossible to achieve a balance of "high stability + high efficacy + all-natural + non-irritating". There is an urgent need to develop a highly stable soothing composition that meets the needs of sensitive skin. Summary of the Invention

[0009] Addressing the shortcomings of existing technologies and industry pain points, the present invention aims to provide a highly stable composition with soothing efficacy, its preparation method, and its applications. This invention utilizes a precise synergistic combination of triple stabilization technologies—cyclodextrin inclusion, polysaccharide microcapsule encapsulation, and phospholipid complexation—to achieve customized stabilization modification of active ingredients with different structures. Simultaneously, it constructs a broad-spectrum preservative system derived entirely from natural sources, completely solving the industry problems of easy oxidation and inactivation of natural soothing active ingredients, poor dispersibility, low bioavailability, and the irritation of sensitive skin by traditional preservatives. It achieves an activity retention rate of >90% after 18 months of storage at room temperature, while also possessing excellent soothing, anti-allergic, and barrier repair effects. It is completely gentle and non-irritating to sensitive skin, making it suitable for large-scale industrial production.

[0010] The objective of this invention can be achieved through the following technical solutions: A highly stable soothing composition, by weight, comprises the following components: 1-5 parts of active active ingredient, 3-8 parts of natural stabilizer, 1-3 parts of natural preservative system, and the balance being a cosmetically acceptable aqueous matrix; wherein the active active ingredient includes inclusion EGCG, microencapsulated chamomile extract, phospholipid complex calendula extract, and Dendrobium nobile extract; the natural stabilizer includes at least two of cyclodextrin, natural polysaccharide microcapsule wall material, and phospholipids; and the natural preservative system includes at least two of 1,2-hexanediol, capryloyl hydroxamic acid, and tea tree oil microcapsules.

[0011] Further, by weight, the active ingredients include: 1-2 parts of inclusion EGCG, 1-2 parts of microcapsule-encapsulated chamomile extract, 0.5-1 parts of phospholipid complex calendula extract, and 0.5-2 parts of Dendrobium nobile extract.

[0012] Further, by weight, the natural stable carrier comprises: 2-5 parts cyclodextrin, 0.5-2 parts sodium alginate, 0.5-1 parts chitosan, and 0.5-2 parts hydrogenated lecithin.

[0013] Further, by weight, the natural preservative system comprises: 1-2 parts of 1,2-hexanediol, 0.1-0.5 parts of capryloyl hydroxamic acid, and 0.1-0.5 parts of tea tree oil microcapsules.

[0014] Furthermore, the EGCG in the inclusion state is EGCG incorporated with β-cyclodextrin or hydroxypropyl-β-cyclodextrin, with an inclusion rate ≥85%; the EGCG is the core active ingredient of green tea extract, with a purity ≥98%.

[0015] Furthermore, the chamomile extract encapsulated in the microcapsules is a polysaccharide microcapsule with sodium alginate-chitosan complex as the wall material, with a particle size of 1-10 μm and an encapsulation rate of ≥80%; the chamomile extract is German chamomile flower extract with a total flavonoid content of ≥5%; the tea tree oil microcapsules are microcapsules with sodium alginate-chitosan as the wall material, with a particle size of 0.5-5 μm and an encapsulation rate of ≥75%.

[0016] Furthermore, the phospholipid complex calendula extract is a nanoliposome complex obtained by combining calendula extract and hydrogenated lecithin at a mass ratio of 1:1-3, with a particle size of 50-200 nm; the calendula extract is calendula flower extract with a total triterpenoid content of ≥3%.

[0017] This invention also provides a method for preparing the above-mentioned highly stable soothing composition, comprising the following steps: Preparation of Inclusion-Formed EGCG (S1): Cyclodextrin was added to deionized water and heated and stirred until completely dissolved to obtain a 5%-10% (w / w) cyclodextrin aqueous solution; EGCG was added to anhydrous ethanol and stirred until dissolved to obtain a 10%-15% (w / w) EGCG alcohol solution; the EGCG alcohol solution was slowly added dropwise to the cyclodextrin aqueous solution at a rate of 0.5-2 mL / min, and the reaction was carried out at a constant temperature of 40-60℃ with stirring for 3-6 h. After the reaction was completed, the mixture was naturally cooled to room temperature, refrigerated at 2-6℃ and allowed to stand for 8-24 h, filtered, and the filter cake was washed 2-4 times with anhydrous ethanol and dried under vacuum at 35-45℃ for 10-15 h to obtain inclusion-formed EGCG. S2 Preparation of microcapsule-encapsulated chamomile extract: Chamomile extract was dispersed in deionized water to obtain a core material solution with a mass concentration of 10%-20%; sodium alginate was added to deionized water and stirred at 20-30℃ for 8-16 hours until completely swollen to obtain a wall material aqueous solution with a mass concentration of 1%-3%; the core material solution was added to the wall material aqueous solution and homogenized at 8000-12000 rpm for 3-8 minutes to obtain an oil-in-water emulsion; the emulsion was slowly added dropwise at a rate of 1-3 mL / min to a chitosan-acetic acid aqueous solution with a mass concentration of 0.5%-2%; the mixture was stirred and solidified at 25-35℃ for 1-3 hours; the mixture was centrifuged at 2000-4000 rpm for 8-15 minutes; the precipitate was collected, washed 2-4 times with deionized water, and freeze-dried at -30~-50℃ for 18-30 hours to obtain microcapsule-encapsulated chamomile extract; Preparation of phospholipid-based calendula extract (S3): Hydrogenated lecithin was added to anhydrous ethanol and heated and stirred at 35-45℃ until completely dissolved, yielding a phosphatidyl alcohol solution with a mass concentration of 3%-8%. Calendula extract was added to the phosphatidyl alcohol solution and stirred until completely dissolved. The anhydrous ethanol was removed by rotary evaporation under reduced pressure at 35-45℃, forming a uniform lipid film on the inner wall of the container. Phosphate buffer solution with pH 7.2-7.4 was added, and the mixture was hydrated at 35-45℃ for 20-40 min. The mixture was then homogenized at 8000-12000 rpm for 2-5 min, followed by high-pressure homogenization at 600-1000 bar for 2-4 times to obtain the phospholipid-based calendula extract. S4 Preparation of Natural Preservative System: Mix 1,2-hexanediol and octanoyl hydroxamic acid, heat and stir at 35-45℃ until completely dissolved to obtain a homogeneous solution; add tea tree oil microcapsules to the above solution, stir and disperse evenly to obtain a natural preservative system; S5 Composition Formulation: Add deionized water to the mixing tank, add the natural stabilizing carrier, and stir until completely dispersed; sequentially add the inclusion-encapsulated EGCG prepared in S1, the microcapsule-encapsulated chamomile extract prepared in S2, the phospholipid complex calendula extract prepared in S3, and the Dendrobium nobile extract, and stir at a constant temperature of 30-40℃ for 20-40 minutes to disperse evenly; add the natural preservative system prepared in S4, stir for 15-30 minutes, add deionized water to the required amount, and stir evenly to obtain a highly stable composition with soothing effects.

[0018] This invention also protects the use of the above-mentioned highly stable soothing composition in the preparation of anti-allergic, soothing, and skin barrier repair cosmetics, including but not limited to serums, toners, lotions, creams, masks, cleansers, and post-medical aesthetic repair products.

[0019] The present invention also provides an anti-allergic and soothing cosmetic, comprising the above-mentioned highly stable soothing composition, wherein the amount of the composition added to the cosmetic is 2-20 wt%.

[0020] The beneficial effects of this invention are: 1. This invention overcomes the limitations of existing single stabilization methods by innovatively combining cyclodextrin inclusion technology, natural polysaccharide microencapsulation technology, and phospholipid complex technology. This allows for customized stabilization modification of active ingredients with different structural characteristics, forming a triple stabilization barrier of "molecular-level encapsulation - micron-level isolation - nanometer-level protection." For EGCG, which is highly water-soluble and has easily oxidized phenolic hydroxyl groups, hydroxypropyl-β-cyclodextrin is used for molecular-level inclusion, completely encapsulating the EGCG molecule within the hydrophobic cavity of the cyclodextrin, thus completely isolating it from oxygen. The treatment targets the phenolic hydroxyl groups under light and temperature, preventing oxidative degradation at its source. For chamomile extract, which is highly lipid-soluble and volatile, sodium alginate-chitosan natural polysaccharide microcapsules are used for micron-level encapsulation, forming a dense polysaccharide protective film to isolate it from external environmental influences while achieving sustained release of active ingredients. For calendula extract, which has poor water solubility and weak skin permeability, hydrogenated lecithin is used for nano-phospholipid complexation to form nanoliposomes with controllable particle size, which avoids direct contact between active ingredients and the aqueous phase and improves storage stability.

[0021] 2. This invention completely abandons traditional chemical preservatives and innovatively constructs an all-natural preservative system consisting of 1,2-hexanediol, capryloyl hydroxamic acid, and tea tree oil microcapsules. The three components work synergistically to achieve a broad-spectrum antibacterial effect: 1,2-hexanediol is a naturally derived polyol that combines moisturizing and broad-spectrum antibacterial effects, can disrupt the cell membrane structure of microorganisms, and has excellent inhibitory effects on both Gram-positive and Gram-negative bacteria; capryloyl hydroxamic acid is a naturally derived amino acid derivative that blocks the nutrient supply to microorganisms by chelating metal ions in the system, while also having a specific inhibitory effect on fungi and yeasts, thus compensating for the deficiency of polyols in inhibiting fungi; the tea tree oil microcapsules are encapsulated with natural polysaccharide wall materials, achieving a sustained release of antibacterial components, which can maintain the antibacterial concentration in the system for a long time, while avoiding the volatility and irritation of tea tree oil.

[0022] 3. The triple stabilization technology of this invention not only improves stability but also simultaneously solves industry pain points such as poor dispersibility, weak skin penetration, and low bioavailability of active ingredients: cyclodextrin inclusion significantly improves the water solubility of EGCG, avoiding the aggregation and sedimentation of active ingredients in the aqueous phase and achieving nanoscale uniform dispersion in the formulation system; polysaccharide microencapsulation technology achieves stable dispersion of chamomile extract in the aqueous phase, avoiding the floating and stratification of lipid-soluble components; phospholipid complex-formed nanoliposomes, with a particle size controlled at 50-200nm, can penetrate through the intercellular spaces of the stratum corneum to the dermis for targeted release, significantly improving the transdermal penetration rate of active ingredients.

[0023] 4. The preparation method of this invention has clear and controllable process parameters, and the inclusion rate, encapsulation rate, and particle size all exhibit excellent batch stability. It requires no special, expensive production equipment and can be directly adapted to existing industrial production lines in the cosmetics industry. It boasts low production costs and high production efficiency, making it suitable for large-scale application. Furthermore, the composition of this invention has strong compatibility and can be added to various water-based, oil-based, and emulsified cosmetic systems. The addition amount within the range of 2-20 wt% maintains excellent stability and efficacy, making its application scope extremely wide. Detailed Implementation

[0024] To further illustrate the technical means and effects adopted by the present invention to achieve the intended purpose, the following detailed description of the specific implementation methods, structures, features and effects of the present invention, in conjunction with embodiments, is provided below.

[0025] Example 1: Preparation of a highly stable soothing composition This embodiment is a preferred embodiment, and the specific preparation steps are as follows: Preparation of Inclusion-Formed EGCG (S1): 4.0 parts of hydroxypropyl-β-cyclodextrin were added to 40 parts of deionized water and heated and stirred at 50°C until completely dissolved to obtain an 8% (w / w) cyclodextrin aqueous solution. 1.5 parts of EGCG (98% purity) were added to 10 parts of anhydrous ethanol and stirred until dissolved to obtain a 13% (w / w) EGCG alcoholic solution. The EGCG alcoholic solution was slowly added dropwise to the cyclodextrin aqueous solution at a rate of 1 mL / min, and the reaction was carried out at 50°C with stirring for 4 h. After the reaction, the mixture was allowed to cool naturally to room temperature, refrigerated at 4°C for 12 h, filtered, and the filter cake was washed three times with anhydrous ethanol. The mixture was then vacuum dried at 40°C for 12 h to obtain inclusion-formed EGCG. The inclusion rate was found to be 89.2%. S2 Preparation of microcapsule-encapsulated chamomile extract: 1.5 parts of German chamomile extract (total flavonoid content 6.2%) were dispersed in 10 parts of deionized water to obtain a core material solution with a mass concentration of 15%; 1.2 parts of sodium alginate were added to 50 parts of deionized water and stirred at 25℃ for 12 hours until completely swollen to obtain a wall material aqueous solution with a mass concentration of 2%; the core material solution was added to the wall material aqueous solution and homogenized at 10000 rpm for 5 minutes to obtain a uniform oil-in-water emulsion; the emulsion was slowly added dropwise to 0.8 parts of chitosan in a 1% acetic acid aqueous solution at a rate of 2 mL / min, stirred and solidified at 30℃ for 2 hours, centrifuged at 3000 rpm for 10 minutes, the precipitate was collected, washed three times with deionized water, and freeze-dried at -40℃ for 24 hours to obtain microcapsule-encapsulated chamomile extract. The particle size was measured to be 2-8 μm, and the encapsulation rate was 83.5%. Preparation of phospholipid-complexed calendula extract (S3): 1.0 part hydrogenated lecithin was added to 20 parts anhydrous ethanol and heated and stirred at 40°C until completely dissolved to obtain a 5% (w / w) phosphatidyl alcohol solution. 1.0 part calendula extract (total triterpenoid content 3.8%) was added to the phosphatidyl alcohol solution and stirred until completely dissolved. The anhydrous ethanol was removed by rotary evaporation under reduced pressure at 40°C, forming a uniform lipid film on the inner wall of the rotating flask. 30 parts pH 7.4 phosphate buffer were added, hydrated at 40°C for 30 min, homogenized at 10000 rpm for 3 min, and then homogenized three times under high pressure at 800 bar to obtain the phospholipid-complexed calendula extract. The particle size was measured to be 80-150 nm, and the encapsulation rate was 86.7%. S4 Preparation of Natural Preservative System: Take 1.5 parts of 1,2-hexanediol and 0.3 parts of capryloyl hydroxamic acid, heat and stir at 40℃ until completely dissolved to obtain a homogeneous and transparent solution; add 0.2 parts of tea tree oil microcapsules (sodium alginate-chitosan wall material, particle size 1-3μm, encapsulation rate 78.2%), stir and disperse evenly to obtain the natural preservative system; S5 Composition Formulation: Add 30 parts of deionized water to a mixing tank, add a natural stabilizing carrier while stirring, and stir until completely dispersed; sequentially add 0.5 parts of the inclusion-encapsulated EGCG prepared in S1, the microcapsule-encapsulated chamomile extract prepared in S2, the phospholipid complex calendula extract prepared in S3, and the Dendrobium nobile extract (Shaanxi Lvlai Biotechnology Co., Ltd.), and stir at 35℃ for 30 minutes to disperse evenly; add the natural preservative system prepared in S4, stir for 20 minutes, add deionized water to 100 parts, and stir evenly to obtain a highly stable soothing composition. The pH value was tested to be 5.8, which is within the physiological pH range of the skin.

[0026] Example 2: Preparation of a highly stable soothing composition Preparation of Inclusion-Formed EGCG (S1): 2.0 parts of hydroxypropyl-β-cyclodextrin were added to 25 parts of deionized water and heated and stirred at 45°C until completely dissolved to obtain a 7% (w / w) cyclodextrin aqueous solution. 1.0 part of EGCG (98% purity) was added to 8 parts of anhydrous ethanol and stirred until dissolved to obtain an 11% (w / w) EGCG alcoholic solution. The EGCG alcoholic solution was slowly added dropwise to the cyclodextrin aqueous solution at a rate of 0.8 mL / min, and the reaction was carried out at 45°C with constant stirring for 3.5 h. After the reaction, the mixture was allowed to cool naturally to room temperature, refrigerated at 4°C for 10 h, filtered, and the filter cake was washed three times with anhydrous ethanol. The mixture was then vacuum dried at 38°C for 11 h to obtain inclusion-formed EGCG. The inclusion rate was measured to be 86.7%. S2 Preparation of microcapsule-encapsulated chamomile extract: 1.0 part of German chamomile extract (total flavonoid content 6.2%) was dispersed in 8 parts of deionized water to obtain a core material solution with a mass concentration of 12%; 0.5 parts of sodium alginate were added to 30 parts of deionized water and stirred at 25℃ for 10 h until completely swollen to obtain a wall material aqueous solution with a mass concentration of 1.5%; the core material solution was added to the wall material aqueous solution and homogenized at 9000 rpm for 4 min to obtain a uniform oil-in-water emulsion; the emulsion was slowly added dropwise to 0.5 parts of chitosan in 0.8% acetic acid aqueous solution at a rate of 1.5 mL / min, stirred and solidified at 28℃ for 1.5 h, centrifuged at 2500 rpm for 12 min, the precipitate was collected, washed 3 times with deionized water, and freeze-dried at -40℃ for 20 h to obtain microcapsule-encapsulated chamomile extract. The particle size was detected to be 3-9 μm, and the encapsulation rate was 81.2%; Preparation of phospholipid-complexed calendula extract (S3): 0.5 parts hydrogenated lecithin were added to 15 parts anhydrous ethanol and heated and stirred at 38°C until completely dissolved, yielding a 3.5% (w / w) phosphatidyl alcohol solution. 0.5 parts calendula extract (total triterpenoid content 3.8%) were added to the phosphatidyl alcohol solution and stirred until completely dissolved. Anhydrous ethanol was removed by rotary evaporation under reduced pressure at 38°C, forming a uniform lipid film on the inner wall of the rotating flask. 20 parts pH 7.4 phosphate buffer were added, hydrated at 38°C for 25 min, homogenized at 9000 rpm for 2 min, and then homogenized twice under high pressure at 700 bar to obtain the phospholipid-complexed calendula extract. The particle size was measured to be 100-180 nm, with an encapsulation rate of 85.1%. S4 Preparation of Natural Preservative System: Take 1.0 part of 1,2-hexanediol and 0.1 part of capryloyl hydroxamic acid, heat and stir at 38°C until completely dissolved to obtain a homogeneous and transparent solution; add 0.1 part of tea tree oil microcapsules, stir and disperse evenly to obtain the natural preservative system; S5 Composition Formulation: Add 25 parts of deionized water to the mixing tank, add the natural stabilizing carrier while stirring, and stir until completely dispersed; add in sequence the inclusion-encapsulated EGCG prepared in S1, the microcapsule-encapsulated chamomile extract prepared in S2, the phospholipid complex calendula extract prepared in S3, and 1.5 parts of Dendrobium nobile extract, and stir at 32℃ for 25 minutes to disperse evenly; add the natural preservative system prepared in S4, stir for 18 minutes, add deionized water to 100 parts, and stir evenly to obtain a highly stable soothing composition with a pH value of 5.7.

[0027] Example 3: Preparation of a highly stable soothing composition Preparation of Inclusion-Formed EGCG (S1): 5.0 parts of hydroxypropyl-β-cyclodextrin were added to 50 parts of deionized water and heated and stirred at 55°C until completely dissolved to obtain a 9% (w / w) cyclodextrin aqueous solution. 2.0 parts of EGCG (98% purity) were added to 12 parts of anhydrous ethanol and stirred until dissolved to obtain a 14% (w / w) EGCG alcohol solution. The EGCG alcohol solution was slowly added dropwise to the cyclodextrin aqueous solution at a rate of 1.5 mL / min, and the mixture was stirred at 55°C for 5 h. After the reaction, the mixture was allowed to cool naturally to room temperature, refrigerated at 4°C for 18 h, filtered, and the filter cake was washed four times with anhydrous ethanol. The mixture was then vacuum dried at 42°C for 14 h to obtain inclusion-formed EGCG. The inclusion rate was found to be 90.5%. S2 Preparation of microcapsule-encapsulated chamomile extract: 2.0 parts of German chamomile extract (total flavonoid content 6.2%) were dispersed in 12 parts of deionized water to obtain a core material solution with a mass concentration of 18%; 2.0 parts of sodium alginate were added to 60 parts of deionized water and stirred at 28℃ for 14 h until completely swollen to obtain a wall material aqueous solution with a mass concentration of 2.5%; the core material solution was added to the wall material aqueous solution and homogenized at 11000 rpm for 7 min to obtain a uniform oil-in-water emulsion; the emulsion was slowly added dropwise to 1.0 part of a 1.5% acetic acid aqueous solution of chitosan at a rate of 2.5 mL / min, stirred and solidified at 32℃ for 2.5 h, centrifuged at 3500 rpm for 12 min, the precipitate was collected, washed 4 times with deionized water, and freeze-dried at -45℃ for 28 h to obtain microcapsule-encapsulated chamomile extract. The particle size was measured to be 1-7 μm, and the encapsulation rate was 84.8%. Preparation of phospholipid-complexed calendula extract (S3): 2.0 parts hydrogenated lecithin were added to 25 parts anhydrous ethanol and heated and stirred at 42°C until completely dissolved to obtain a 7% (w / w) phosphatidyl alcohol solution. 1.0 part calendula extract (total triterpenoid content 3.8%) was added to the phosphatidyl alcohol solution and stirred until completely dissolved. The anhydrous ethanol was removed by rotary evaporation under reduced pressure at 42°C, forming a uniform lipid film on the inner wall of the rotating flask. 35 parts pH 7.4 phosphate buffer were added, hydrated at 42°C for 35 min, homogenized at 11000 rpm for 4 min, and then homogenized four times under high pressure at 900 bar to obtain the phospholipid-complexed calendula extract. The particle size was measured to be 50-120 nm, and the encapsulation efficiency was 88.3%. S4 Preparation of Natural Preservative System: Take 2.0 parts of 1,2-hexanediol and 0.5 parts of capryloyl hydroxamic acid, heat and stir at 42℃ until completely dissolved to obtain a homogeneous and transparent solution; add 0.5 parts of tea tree oil microcapsules, stir and disperse evenly to obtain the natural preservative system; S5 Composition Formulation: Add 35 parts of deionized water to the mixing tank, add the natural stabilizing carrier while stirring, and stir until completely dispersed; add the inclusion-encapsulated EGCG prepared in S1, the microcapsule-encapsulated chamomile extract prepared in S2, the phospholipid complex calendula extract prepared in S3, and 2 parts of Dendrobium nobile extract in sequence, stir at 38℃ for 35 min, and disperse evenly; add the natural preservative system prepared in S4, stir for 25 min, add deionized water to 100 parts, stir evenly, and obtain a highly stable soothing composition with a pH value of 5.9.

[0028] Comparative Example 1 The EGCG was not encapsulated with cyclodextrin; the unencapsulated EGCG was directly added to the mixing tank in step S5, and the remaining steps were completely consistent with those in Example 1. Comparative Example 2 The chamomile extract was not encapsulated in microcapsules. Instead, the unencapsulated chamomile extract was directly added to the mixing tank in step S5. The remaining steps were exactly the same as in Example 1. Comparative Example 3 The calendula extract was not compounded with phospholipids. Instead, the uncompounded calendula extract was directly added to the mixing tank in step S5. The remaining steps were completely consistent with those in Example 1. Comparative Example 4 Only the phospholipid complex technology was retained, and the cyclodextrin inclusion and microencapsulation technologies were not used. The remaining steps were completely consistent with those in Example 1. Comparative Example 5 Only the cyclodextrin inclusion technology was retained, and the microcapsule encapsulation and phospholipid complex technology were not used. The remaining steps were completely consistent with those in Example 1. Comparative Example 6 Traditional preservatives are used to replace the natural preservative system, and the remaining components and steps are completely consistent with those in Example 1. Comparative Example 7 The tea tree oil microcapsules were removed from the natural preservative system, while the remaining components and steps were completely consistent with those in Example 1. Comparative Example 8 The amount of EGCG added was 0.5 parts, which is lower than the range of 1-2 parts specified in this invention. The remaining components and steps were completely consistent with those in Example 1. Comparative Example 9 The amount of EGCG added was 3.0 parts, which is higher than the range of 1-2 parts specified in this invention. The remaining components and steps were completely consistent with those in Example 1. Comparative Example 10 Chamomile microcapsules were prepared by using gelatin-gum arabic wall material instead of sodium alginate-chitosan wall material, and the remaining preparation parameters and steps were completely consistent with those in Example 1. Comparative Example 11 No stabilization technology was used; all active ingredients were added directly, and all natural stabilizers were removed. The remaining components and steps were completely consistent with those in Example 1. Comparative Example 12 No inclusion reaction was performed on EGCG; instead, EGCG was physically mixed with hydroxypropyl-β-cyclodextrin. The remaining components and steps were completely consistent with those in Example 1.

[0029] Performance testing The present invention conducted comprehensive performance tests on all embodiments and comparative examples, including stability testing, preservative challenge tests, irritation testing, soothing efficacy testing, and skin permeability testing. All testing methods adopted the common standard methods in the cosmetics industry, and the test results are as follows.

[0030] 1. Stability testing Detection method: Accelerated stability test: The samples of each example and the comparative example were placed in a constant temperature and humidity incubator at 45°C and 75% relative humidity and stored for 3 months. The appearance of the samples (color change, precipitation, and layering) was observed at 0 days, 1 month, 2 months and 3 months. The pH value change was detected. The contents of EGCG, total chamomile flavonoids and total calendula triterpenes in the samples were detected by high performance liquid chromatography (HPLC), and the activity retention rate was calculated.

[0031] Long-term stability test: The samples of each example and the comparative example were stored at room temperature and protected from light for 18 months. The content of each active ingredient was detected by HPLC and the activity retention rate was calculated.

[0032] Test results: The results of the accelerated stability test are detailed in Table 1, and the results of the long-term stability test (18 months) activity retention rate are detailed in Table 2.

[0033] Table 1. Results of accelerated stability tests (45°C, 3 months) for each example and comparative example.

[0034] Table 2. Long-term stability test (18 months at room temperature) results of each example and comparative example (unit: %)

[0035] 2. Corrosion Resistance Challenge Test Test method: Referring to the preservative challenge test method in the 2022 edition of the "Cosmetic Safety Technical Specifications", the samples of each example and comparative example were inoculated. The inoculated microorganisms included: mixed bacteria (Escherichia coli, Staphylococcus aureus, and Pseudomonas aeruginosa), with an initial inoculation concentration of 1.0 × 10⁻⁶. 6CFU / g; mixed fungal strain (Candida albicans, Aspergillus niger), initial inoculum concentration 1.0 × 10⁻⁶. 5 CFU / g. The number of microbial colonies in the samples was measured at 7, 14, and 28 days after inoculation to evaluate the preservative effect.

[0036] Test results: See Table 3 for details.

[0037] Table 3. Corrosion resistance challenge test results for each example and comparative example (unit: CFU / g)

[0038] 3. Irritation test Detection method: Heteroalanine membrane test (HET-CAM): SPF-grade white Leghorn chicken embryos were incubated for 10 days. 0.3 mL of sample solution was added to the chorioalanine membrane of the embryo. The vascular bleeding, coagulation, and vascular lysis of the allantoic membrane were observed within 5 minutes. The irritation score was calculated to evaluate the eye irritation of the sample. A irritation score <1 indicates no irritation, 1-5 indicates mild irritation, 5-9 indicates moderate irritation, and >9 indicates severe irritation.

[0039] Human skin patch test: Thirty healthy subjects with sensitive skin, aged 18-45 years, were selected. The sample was applied to the upper back of the subjects using a patch applicator. The patch applicator was left in place for 24 hours. After removing the patch applicator, the skin reaction was observed at 30 minutes, 24 hours, and 48 hours. The skin reaction was scored according to the "Cosmetic Safety Technical Specifications", and the number of positive reactions was recorded.

[0040] Test results: See Table 4 for details.

[0041] Table 4. Irritation test results of each embodiment and comparative example.

[0042] 4. Testing of soothing effects and skin barrier repair effects Detection method: Histamine release inhibition rate test: RBL-2H3 rat basophilic leukemia cells were used. The sample and cells were co-incubated. C48 / 80 was used to induce cell degranulation and release histamine. The histamine content in the supernatant was detected by enzyme-linked immunosorbent assay (ELISA). The histamine release inhibition rate was calculated. The higher the inhibition rate, the better the anti-allergic and soothing effect.

[0043] Human efficacy trial: Thirty subjects with sensitive skin exhibiting symptoms such as facial redness, dryness, itching, and barrier damage were selected. The sample was applied to the subjects' faces twice daily for 28 consecutive days. On days 0, 7, and 28, facial skin redness a* value, transepidermal water loss (TEWL) value, and stratum corneum moisture content were measured using a skin analyzer. The redness relief rate, TEWL decrease rate, and stratum corneum moisture content increase rate were calculated.

[0044] Test results: See Table 5 for details.

[0045] Table 5. Test results of soothing efficacy and barrier repair effect of each embodiment and comparative example.

[0046] 5. In vitro skin permeability test Detection method: A modified Franz diffusion cell was used, with excised pig skin as the skin model. The receiving solution was a phosphate buffer-anhydrous ethanol (7:3) mixture at pH 7.4. The sample was added to the supply cell and stirred at 37°C. Samples were taken at 2h, 4h, 8h, 12h and 24h. The content of each active ingredient in the receiving solution was detected by HPLC. The cumulative transdermal penetration over 24h was calculated to evaluate the skin permeability of the active ingredients.

[0047] Test results: See Table 6 for details.

[0048] Table 6. 24-hour cumulative transdermal penetration results for each example and comparative example (unit: μg / cm²).

[0049] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any way. Although the present invention has been disclosed above with reference to preferred embodiments, it is not intended to limit the present invention. Any person skilled in the art can make some modifications or alterations to the above-disclosed technical content to create equivalent embodiments without departing from the scope of the present invention. Any simple modifications, equivalent changes and alterations made to the above embodiments based on the technical essence of the present invention without departing from the scope of the present invention shall still fall within the scope of the present invention.

Claims

1. A high-stable soothing efficacy composition, characterized in that, By weight, it comprises the following components: 1-5 parts of active ingredient, 3-8 parts of natural stabilizer, 1-3 parts of natural preservative system, and the balance being a cosmetically acceptable aqueous matrix; wherein, the active ingredient includes encapsulated epigallocatechin gallate (EGCG), microencapsulated chamomile extract, phospholipid complex calendula extract, and Dendrobium nobile extract; the natural stabilizer includes at least two of cyclodextrin, natural polysaccharide microcapsule wall material, and phospholipids; the natural preservative system includes at least two of 1,2-hexanediol, capryloyl hydroxamic acid, and tea tree oil microcapsules.

2. The highly stable, soothing efficacy composition according to claim 1, characterized in that, By weight, the active ingredients include: 1-2 parts of incorporated EGCG, 1-2 parts of microcapsule-encapsulated chamomile extract, 0.5-1 parts of phospholipid complex calendula extract, and 0.5-2 parts of Dendrobium nobile extract.

3. The highly stable, soothing efficacy composition according to claim 1, characterized by, By weight, the natural stable carrier comprises: 2-5 parts cyclodextrin, 0.5-2 parts sodium alginate, 0.5-1 parts chitosan, and 0.5-2 parts hydrogenated lecithin.

4. The highly stable, soothing efficacy composition according to claim 1, characterized by, By weight, the natural preservative system comprises: 1-2 parts of 1,2-hexanediol, 0.1-0.5 parts of capryloyl hydroxamic acid, and 0.1-0.5 parts of tea tree oil microcapsules.

5. The highly stable, soothing efficacy composition according to claim 1, wherein The EGCG in the inclusion state is EGCG encapsulated by β-cyclodextrin or hydroxypropyl-β-cyclodextrin, with an inclusion rate ≥85%; the EGCG is the core active ingredient of green tea extract, with a purity ≥98%.

6. The highly stable, soothing efficacy composition according to claim 1, wherein The microcapsules encapsulating chamomile extract are polysaccharide microcapsules with sodium alginate-chitosan complex as the wall material, with a particle size of 1-10 μm and an encapsulation rate of ≥80%; the chamomile extract is German chamomile flower extract with a total flavonoid content of ≥5%; the tea tree oil microcapsules are microcapsules with sodium alginate-chitosan as the wall material, with a particle size of 0.5-5 μm and an encapsulation rate of ≥75%.

7. The highly stable, soothing efficacy composition according to claim 1, wherein The phospholipid complex calendula extract is a nanoliposome complex obtained by combining calendula extract and hydrogenated lecithin in a mass ratio of 1:1-3, with a particle size of 50-200 nm; the calendula extract is calendula flower extract with a total triterpenoid content ≥3%.

8. A method for preparing a composition with highly stable soothing effects as described in any one of claims 1-7, characterized in that, Includes the following steps: Preparation of Inclusion-Formed EGCG (S1): Cyclodextrin was added to deionized water and heated and stirred until completely dissolved to obtain a 5%-10% (w / w) cyclodextrin aqueous solution; EGCG was added to anhydrous ethanol and stirred until dissolved to obtain a 10%-15% (w / w) EGCG alcohol solution; the EGCG alcohol solution was slowly added dropwise to the cyclodextrin aqueous solution at a rate of 0.5-2 mL / min, and the reaction was carried out at a constant temperature of 40-60℃ with stirring for 3-6 h. After the reaction was completed, the mixture was naturally cooled to room temperature, refrigerated at 2-6℃ and allowed to stand for 8-24 h, filtered, and the filter cake was washed 2-4 times with anhydrous ethanol and dried under vacuum at 35-45℃ for 10-15 h to obtain inclusion-formed EGCG. S2 Preparation of microcapsule-encapsulated chamomile extract: Chamomile extract was dispersed in deionized water to obtain a core material solution with a mass concentration of 10%-20%; sodium alginate was added to deionized water and stirred at 20-30℃ for 8-16 hours until completely swollen to obtain a wall material aqueous solution with a mass concentration of 1%-3%; the core material solution was added to the wall material aqueous solution and homogenized at 8000-12000 rpm for 3-8 minutes to obtain an oil-in-water emulsion; the emulsion was slowly added dropwise at a rate of 1-3 mL / min to a chitosan-acetic acid aqueous solution with a mass concentration of 0.5%-2%; the mixture was stirred and solidified at 25-35℃ for 1-3 hours; the mixture was centrifuged at 2000-4000 rpm for 8-15 minutes; the precipitate was collected, washed 2-4 times with deionized water, and freeze-dried at -30~-50℃ for 18-30 hours to obtain microcapsule-encapsulated chamomile extract; Preparation of phospholipid-based calendula extract (S3): Hydrogenated lecithin was added to anhydrous ethanol and heated and stirred at 35-45℃ until completely dissolved, yielding a phosphatidyl alcohol solution with a mass concentration of 3%-8%. Calendula extract was added to the phosphatidyl alcohol solution and stirred until completely dissolved. The anhydrous ethanol was removed by rotary evaporation under reduced pressure at 35-45℃, forming a uniform lipid film on the inner wall of the container. Phosphate buffer solution with pH 7.2-7.4 was added, and the mixture was hydrated at 35-45℃ for 20-40 min. The mixture was then homogenized at 8000-12000 rpm for 2-5 min, followed by high-pressure homogenization at 600-1000 bar for 2-4 times to obtain the phospholipid-based calendula extract. S4 Preparation of Natural Preservative System: Mix 1,2-hexanediol and octanoyl hydroxamic acid, heat and stir at 35-45℃ until completely dissolved to obtain a homogeneous solution; add tea tree oil microcapsules to the above solution, stir and disperse evenly to obtain a natural preservative system; S5 Composition Formulation: Add deionized water to the mixing tank, add the natural stabilizing carrier, and stir until completely dispersed; sequentially add the inclusion-encapsulated EGCG prepared in S1, the microcapsule-encapsulated chamomile extract prepared in S2, the phospholipid complex calendula extract prepared in S3, and the Dendrobium nobile extract, and stir at a constant temperature of 30-40℃ for 20-40 minutes to disperse evenly; add the natural preservative system prepared in S4, stir for 15-30 minutes, add deionized water to the required amount, and stir evenly to obtain a highly stable composition with soothing effects.

9. The use of a composition with highly stable soothing effects as described in any one of claims 1-7 in the preparation of anti-allergic, soothing, and skin barrier repair cosmetics.

10. An anti-irritation soothing cosmetic product, characterized in that, A composition comprising the highly stable soothing efficacy as described in any one of claims 1-7, wherein the amount of the composition added to the cosmetic is 2-20 wt%.

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