A soothing anti-sensitivity composition, a process for its preparation and its use in the field of daily cosmetics

Abstract

The present application belongs to the technical field of cosmetics, and particularly relates to a soothing and anti-allergy composition, a preparation method thereof and application thereof in the field of daily-use cosmetics. The present application adopts supercritical CO2 extraction, ethanol, water and other different polar solvents to step-by-step extract mixed components of three raw materials of Sophora root, Centella asiatica and Platycladus orientalis, and simultaneously enriches non-polar components rich in volatile oil and triterpenoid acids, moderately polar components rich in flavonoids and saponins, and polar segment components rich in plant polysaccharides and alkaloids. Further, by adjusting pH, the stability and biological activity of the final composition are significantly improved, the synergistic coefficient CI is less than 0.5, and the present application is significantly superior to the prior art physical mixing CI greater than 0.9. The present application can realize significant soothing effects in multiple scenes such as face, scalp and body, and provides technical feasibility for one material for multiple uses.

Description

Technical Field

[0001] This invention belongs to the field of cosmetic technology, and specifically relates to a soothing and anti-allergic composition, its preparation method, and its application in the field of daily cosmetics. Background Technology

[0002] In recent years, with environmental changes, increased life pressures, and the rapid development of the cosmetics market, skin problems such as sensitive skin, damaged skin barrier, and irritant dermatitis have become increasingly common. Consumers' demand for natural plant-based skincare products with anti-allergic, soothing, repairing, and anti-inflammatory effects continues to grow. Compared to anti-allergy medications with clearly defined chemical ingredients that are prone to causing irritation, natural plant extracts, due to their gentleness, safety, and fewer side effects, have become the core ingredient in anti-allergic and soothing skincare products, offering both anti-inflammatory and skin barrier repair benefits.

[0003] Currently, there are many types of plant-based raw materials with soothing, anti-allergic, and antibacterial effects. Among them, Sophora flavescens root, Centella asiatica, and Platycladus orientalis have clear efficacy and high safety, and have broad application prospects in the field of soothing and repair. Sophora flavescens root mainly contains alkaloid active ingredients such as matrine and oxymatrine, which have good antibacterial effects and can relieve skin itching. Centella asiatica is rich in asiaticoside and asiatic acid, which can promote collagen synthesis, accelerate epidermal repair, and enhance the skin barrier function. Platycladus orientalis contains flavonoids, terpenes, and other active substances, which have antioxidant, anti-inflammatory, soothing, and skin-stabilizing effects, and can reduce the skin's reaction to external environmental irritants.

[0004] However, existing technologies often suffer from limitations when using extracts of Sophora flavescens, Centella asiatica, or Platycladus orientalis alone, resulting in limited efficacy, limited soothing effects, and difficulty in simultaneously addressing anti-inflammatory and repairing properties. While combining multiple plants can enhance efficacy to some extent, the following technical challenges remain common:

[0005] Firstly, most existing plant extraction processes only use traditional organic solvents such as water or alcohol (e.g., patents CN115475130A, CN107854404A, CN118649111A) or supercritical CO2 as a solvent (e.g., patent CN116327648A) to extract water-soluble, alcohol-soluble, and volatile oil components, followed by simple physical mixing. These extraction processes are somewhat one-sided or have limited extraction capabilities for heat-sensitive, volatile oils, and alkaloids in plants. Furthermore... Some processes overemphasize the separation and purification of single active ingredients. For example, patents CN101084989A, CN112773745A, and CN114903930A only focus on extracting marker components such as asiaticoside and matrine, while ignoring the overall synergistic effect of multiple components such as polyphenols, flavonoids, polysaccharides, and organic acids in plants. This not only results in a large waste of plant raw materials, but also damages the natural synergistic system of plants themselves, leading to slow anti-allergic effects, incomplete soothing, and insufficient barrier repair capabilities of the composition.

[0006] Secondly, most commercially available anti-allergy and soothing products currently use plant-based raw materials directly from commercially available products, such as patents CN107693426A, CN111214405A, CN118021663A, etc. Due to the different sources of commercially available extracts, large differences in extraction processes, large fluctuations in the content of effective ingredients, and uncontrollable impurities and solvent residues, the efficacy of the final composition is unstable, with large batch-to-batch differences, making it difficult to guarantee product quality and safety, and failing to meet the requirements of high-standard cosmetics and topical products.

[0007] Thirdly, because facial skin has lower sebaceous gland density, stratum corneum thickness, and hair follicle density than scalp, the microenvironment of facial skin and scalp is significantly different. Therefore, existing anti-allergy and soothing compositions can only be applied to one aspect, resulting in fragmented application scenarios.

[0008] Based on the above technical issues, a multi-target synergistic anti-allergic and soothing composition was developed. By improving the preparation process, the utilization rate of plant-based raw materials and the synergistic effect of the product were enhanced. This provides an anti-allergic and soothing composition raw material that can be applied to both facial and scalp skin, which is of great significance for improving the quality of daily cosmetic products. Summary of the Invention

[0009] To address the above technical problems, this invention proposes a method for preparing a soothing and anti-allergic composition and its application in the field of daily cosmetics.

[0010] The technical solution provided by this invention includes the following aspects:

[0011] The first aspect of the present invention is to provide a soothing and anti-allergic composition comprising: Sophora flavescens root extract, Centella asiatica extract, and Platycladus orientalis leaf extract, wherein the Sophora flavescens root extract, Centella asiatica extract, and Platycladus orientalis leaf extract are obtained by mixing Sophora flavescens root, Centella asiatica, and Platycladus orientalis leaf in a mass ratio of (2~4):(2~4):(1~2), and then sequentially performing supercritical CO2 extraction, organic solvent extraction, and water extraction, followed by merging the mixtures.

[0012] A second aspect of the present invention is that a method for preparing the above-mentioned soothing and anti-allergic composition is provided, specifically comprising the following steps:

[0013] Preparation of raw materials for S1: Take Sophora flavescens root, Centella asiatica and Platycladus orientalis leaves and mix them in a mass ratio of (2~4):(2~4):(1~2), crush and sieve them for later use;

[0014] S2 three-step extraction: The raw material powder in S1 is extracted sequentially with supercritical CO2, ethanol with a volume fraction of 60%~80% and water. The extracts are combined and concentrated under reduced pressure to obtain a concentrated solution.

[0015] The conditions for supercritical CO2 extraction are: extraction pressure 25~35 MPa, temperature 40~50℃, CO2 flow rate 20~30 L / h, and entrainer is ethanol with a volume fraction of 5%~10%.

[0016] The temperature for ethanol extraction is 75~85℃, and the temperature for water extraction is 90~100℃.

[0017] Induction of S3 precipitation: Adjust the pH of the concentrated solution in S2 to 5.0~6.5, control the temperature at 25~40℃, stir at 100~300 rpm for 1~2 h, and then let it stand at 4~10℃ for 12~24 h to promote sedimentation. Collect the precipitate by centrifugation and filtration.

[0018] S4 Purification and Drying: The precipitate obtained in S3 was washed with a 20% to 30% ethanol solution (pH 5.0 to 5.5), dried, pulverized, and sieved to obtain the soothing and anti-allergic composition.

[0019] In the preparation method of the above-mentioned composition provided by the present invention, preferably, the mass ratio of Sophora flavescens root: Centella asiatica: Platycladus orientalis in S1 is (2~3):(2~3):1.

[0020] As a further preferred embodiment, the mass ratio of Sophora flavescens root: Centella asiatica: Platycladus orientalis is 2:2:1.

[0021] As a preferred embodiment, the conditions for supercritical CO2 extraction in S2 are: extraction pressure 28~33 MPa, temperature 42~46℃, CO2 flow rate 22~26 L / h, extraction time 1.5~2.5 h, and entrainer 8% ethanol by volume.

[0022] Preferably, in the ethanol or water extraction described in S2, the mass-to-volume ratio of the raw material to be extracted to ethanol or water is 1 g: 8~12 mL, and the extraction is performed 1~3 times, with each extraction lasting 1.5~2 h.

[0023] Preferably, the relative density of the concentrate obtained by vacuum concentration in step S2 is 1.05 to 1.15.

[0024] Preferably, in step S3, the pH of the concentrate is adjusted with a 0.5-2 mol / L citric acid or lactic acid solution while stirring.

[0025] A third aspect of the present invention is to provide a method for improving the bioactivity of a soothing and anti-allergic composition. Preferably, the method specifically involves mixing and concentrating a supercritical CO2 extract, an ethanol extract with a volume fraction of 60% to 80%, and an aqueous extract. The pH of the concentrate is then adjusted to between 5.0 and 6.0, the temperature is controlled at 25 to 40°C, the stirring speed is 100 to 300 rpm, and the mixture is maintained for 1 to 2 hours. The mixture is then allowed to stand at 4 to 10°C for 12 to 24 hours to promote sedimentation. The precipitate is collected by centrifugation and filtration.

[0026] In this invention, the active ingredients in Sophora flavescens, Centella asiatica, and Platycladus orientalis leaves are first extracted using different processes. Through supercritical CO2, ethanol, and water extraction, the various active ingredients in the plant-based raw materials are fully enriched. Furthermore, a pH-induced method is used to promote the formation of a ternary complex precipitate, significantly enhancing the physiological efficacy of the soothing and anti-allergic composition. Experimental results show that TRPV1 inhibits IC50. 50 The concentration is 8.5 μg / mL, and the soothing activity is 2.2 times that of a simple mixture of single extracts (18.5 μg / mL). In addition, the present invention can also be applied to completely different application scenarios such as facial skin and scalp skin by adjusting the pH range, truly achieving the effect of multiple uses from one ingredient.

[0027] A fourth aspect of the present invention is to provide a product containing the composition, the product being a facial repair cosmetic, wherein the composition accounts for 2% to 5% of the mass of the facial repair cosmetic, the pH of the facial repair cosmetic is 5.0 to 6.5, and the cosmetic further contains at least ceramide, cholesterol, and fatty acids.

[0028] Preferably, the facial repair cosmetic comprises, by mass fraction: 3% of the soothing and anti-allergic composition, 2% of ceramide NP, 0.8% of cholesterol, 1.5% of fatty acids, 3% of panthenol, 0.3% of hyaluronic acid, 5% of 1,3-propanediol, 0.3% of carbomer 980, 0.3% of arginine, an appropriate amount of preservatives, and the balance being water.

[0029] Alternatively, the product is an anti-dandruff shampoo for scalp soothing. Preferably, the shampoo contains the soothing and anti-allergic composition as well as piroctone olamine salt, salicylic acid, and zinc salt, and the soothing and anti-allergic composition is added to the shampoo at a mass of 0.5% to 3%, and the pH of the shampoo is 5.0 to 6.0.

[0030] Preferably, the scalp-soothing and anti-dandruff shampoo comprises, by mass fraction: 1.5% of the soothing and anti-allergic composition, 0.5% of piroctone olamine salt OCT, 0.3% of salicylic acid, 0.8% of zinc pyrrolidone carboxylate (PCA zinc), 10% of sodium lauryl ether sulfate (SLES), 4% of cocamidopropyl betaine, 0.2% of menthol, 1.5% of panthenol, citric acid to adjust the pH to 5.5, an appropriate amount of preservatives, and water as the remainder.

[0031] Alternatively, the product may be a body lotion. Preferably, the body lotion contains 1% to 2% of the soothing and anti-allergic composition by mass, and also contains urea and shea butter.

[0032] The present invention has the following advantages and effects compared with the prior art:

[0033] (1) This invention provides a soothing and anti-allergic composition containing extracts of Sophora flavescens root, Centella asiatica, and Platycladus orientalis leaf. Sophora flavescens alkaloids can reduce stinging and itching by inhibiting the TRPV1 channel, inhibit the NF-κB pathway, and reduce the release of inflammatory factors IL-6 and TNF-α. Centella asiatica triterpenes can activate the TGF-β / Smad pathway to promote barrier repair and activate the PI3K / Akt pathway to inhibit excessive inflammatory response. Platycladus orientalis leaf flavonoids can reduce the synthesis of prostaglandins and leukotrienes by inhibiting COX-2 / 5-LOX, protect cells with antioxidant properties, and improve redness by constricting capillaries. The three components work synergistically to achieve soothing and repairing effects. The synergy coefficient CI < 0.6 is significantly better than the physical mixing of the prior art (CI > 0.9).

[0034] (2) In this invention, supercritical CO2 extraction, 60%~80% ethanol, water and other different polar solvents are used to extract the mixed components of the three raw materials. At the same time, non-polar components rich in volatile oil and triterpenic acid, medium polar components rich in flavonoids and saponins, and polar components rich in plant polysaccharides and alkaloids are enriched. Not only is the utilization rate of raw materials effectively improved, but the bioactivity of the obtained composition is also significantly improved.

[0035] (3) The present invention uses pH-induced precipitation method to induce precipitation of the extract obtained by the three-step extraction to obtain the final composition. When the pH is 5.0~6.5, the alkaloids of Sophora flavescens can be stably combined with the asiatic acid to form ion pairs. The hydroxyl groups in the flavonoids of Platycladus orientalis and asiatic acid form abundant hydrogen bonds, and finally a stable composition system is formed with alkaloid-triterpene acid ion pairs as the core, flavonoids and asiatic acid as the outer layer of auxiliary hydrogen bonds, and polysaccharides as the backbone. There is no precipitation after 6 months of storage at 4℃, and the activity is maintained at >90% after 3 months of accelerated storage at 50℃.

[0036] (4) The raw materials of the soothing and anti-allergic composition provided by the present invention can be adjusted by the amount added (1%~3%) and compatibility, and can achieve significant soothing effects in multiple scenarios such as face, scalp, and body. The CI is <0.6, which provides feasibility for multiple uses of one material. Detailed Implementation

[0037] To enable those skilled in the art to better understand the present invention, the present invention will now be further described in conjunction with specific embodiments.

[0038] Example 1

[0039] Preparation of raw materials for S1: Take 3 kg of Sophora flavescens root, 3 kg of Centella asiatica whole herb, and 1.5 kg of Platycladus orientalis leaves, mix and grind them, pass them through a 30-mesh sieve, and set aside.

[0040] S2 three-step extraction: The raw material powder in S1 was extracted sequentially using supercritical CO2, 70% ethanol (volume fraction), and water. The extracts were combined, stirred at 200 rpm for 30 min, and concentrated under reduced pressure at 60℃ until the relative density of the concentrate was 1.10.

[0041] The extraction pressure of supercritical CO2 was 30 MPa, the extraction temperature was 45℃, the CO2 flow rate was 25 L / h, 8% ethanol was used as an entrainer, and the extraction time was 2 h to obtain 180 g of extract (yield 4.0%).

[0042] The conditions for 70% ethanol reflux extraction were as follows: the filter residue after supercritical CO2 extraction was used as the extract material, the mass-to-volume ratio of the residue to ethanol was 1 g: 10 mL, the extraction temperature was 80℃, the extraction was performed twice, 2 h each time, the extracts were combined, and the ethanol extract was concentrated under reduced pressure to obtain 680 g of ethanol extract (yield 15.1%).

[0043] The conditions for water extraction were as follows: the filter residue after ethanol extraction was used as the extract material, and the mass-to-volume ratio of the residue to water was 1 g:8 mL. The extraction temperature was 95℃, the extraction time was 1.5 h, and the water extract was concentrated to obtain 320 g (yield 7.1%).

[0044] Induction of S3 precipitation: The pH of the concentrated solution in S2 was slowly adjusted to 5.5 with 1.0 mol / L citric acid solution, stirred at 30℃ and 200 rpm for 2 h, allowed to stand at 4℃ for 20 h, centrifuged at 4500 rpm for 15 min, and the precipitate was collected after filtration.

[0045] S4 Purification and Drying: The precipitate obtained from S3 was washed three times (400 mL each time) with 25% ethanol at pH 5.5, freeze-dried (pre-frozen at -40℃ for 4 h, dried at -20℃ for 40 h), and pulverized through a 100-mesh sieve to obtain 420 g of the soothing and anti-allergic composition.

[0046] The yield of the soothing and anti-allergic composition obtained in this embodiment was 9.3% (composition yield = mass of precipitate after drying / total mass of raw materials × 100%).

[0047] In the above-mentioned soothing and anti-allergic composition, by mass, the total alkaloids account for 6.2% (matrine 3.8%, oxymatrine 2.4%), the total triterpenes account for 12.5% ​​(asiatic acid 7.2%, hydroxyasiatic acid 5.3%), and the total flavonoids account for 9.1% (quercetin 4.5%, kaempferol 4.6%). The particle size of the obtained composition was measured to be D50=35 μm and D90=48 μm, which is within the colloidal system range, making it transdermal friendly. At pH 5.5, the composition's Zeta potential is -5 to +5 mV, indicating near-neutral properties and high stability. After being placed at 4℃ for 6 months, no precipitation occurred, and after accelerated treatment at 50℃ for 3 months, the activity remained >90%. It is easily soluble in cosmetic solvents such as 50% ethanol and 1,3-propanediol, and the drug synergy coefficient CI=0.52 (strong synergy).

[0048] In this invention, CI is calculated using the following formula: CI = (IC) 50 (mixture) / (IC) 50 A+IC 50 B+IC 50 C), where IC 50 A, IC 50 B, IC 50 C represents the half-inhibitory concentration (IC50) when each individual component is used alone. 50 The mixture represents the half-inhibitory concentration (CI) of the three drugs. CI < 1 indicates a synergistic effect between the drugs, and the smaller the CI value, the more significant the synergistic effect. CI > 1 indicates an antagonistic effect between the drugs. CI = 1 indicates no interaction between the drugs, i.e., an additive effect.

[0049] Example 2

[0050] This embodiment focuses on optimizing and verifying the pH range adjusted during the precipitation induction operation in S3 of the composition preparation process in Example 1. This is also one of the main innovations of this invention. In S3, the content of active ingredients in the obtained soothing and anti-allergic composition when the pH value of the concentrate is adjusted at different points is shown in Table 1 below. The content of each component is calculated as a mass percentage.

[0051] Table 1. Content of active ingredients in the composition under different pH induction conditions pH Composition yield Total alkaloids Total triterpenes Total flavonoids Coefficient of Synergy (CI) evaluate 4.0 4.2% 3.5% 8.5% 6.2% 0.85 Excessive protonation of alkaloids, electrostatic repulsion 4.5 6.8% 4.8% 10.2% 7.5% 0.72 Improved but still not ideal 5.0 8.5% 5.5% 11.5% 8.5% 0.58 Close to the best 5.5 10% 6.2% 12.5% 9.1% 0.52 Optimal charge matching 6.0 9.2% 6.0% 12.0% 8.8% 0.55 Close to the best 6.5 8% 5.8% 10.5% 7.8% 0.68 Alkaloid protonation decrease 7.0 6% 4.2% 8.2% 6.5% 0.78 Under neutral conditions, the composition dissociates. 8.0 3.5% 2.8% 5.5% 4.2% 0.95 Alkaloids are free and have no electrostatic effect.

[0052] The results in Table 1 show that when the pH value is too low (4.0~4.5) or too high (7.0~8.0), not only is the yield of the composition itself low, but the content of total alkaloids, flavonoids and triterpenoids in the composition is also at a low level, which ultimately leads to poor synergistic effect among the components of the composition.

[0053] As shown in Table 1, the pH value between 5.0 and 6.5 is the window period for high activity of the composition. In particular, when the pH value is adjusted to 5.5, it is the optimal extraction state. At this time, the yield of the composition is as high as 10%, and the contents of alkaloids, total triterpenes and flavonoids are the highest. The synergistic coefficient between the components is the smallest, and the synergistic effect is the best.

[0054] The above phenomenon is the result of a combination of factors. On the one hand, when the pH is 5.5, matrine (pKa=9.47, data source: ChemicalBook / SciFinder database, CAS: 519-02-8) is almost completely protonated and carries a positive charge, while oxymatrine (pKa=4.87, data source: ChemicalBook / SciFinder database, CAS: 16837-52-8) is about 18% protonated. Both provide positive charge centers. Simultaneously, asiatic acid, as a triterpene acid compound, has a negatively charged carboxyl group. The positive and negative charges combine through electrostatic forces to form stable ion pairs, constituting the stable core of the composition. On the other hand, thujone flavonoids (quercetin, etc.) at pH... At pH 5.5, phenolic hydroxyl groups exist primarily in a neutral molecular form, with abundant hydrogen bond donors. These phenolic hydroxyl groups can form hydrogen bonds with the hydroxyl groups abundant in asiatic acid. The formed hydrogen bonds and the π-π stacking of aromatic rings encapsulate the ion pair core. Finally, the long-chain, multi-hydroxyl structure of the Centella asiatica polysaccharide stabilizes the three-dimensional structure of the composition, preventing aggregation and sedimentation. Ultimately, a stable composition system is formed with alkaloid-triterpene acid ion pairs as the core, flavonoids and asiatic acid as the auxiliary hydrogen bonds as the outer layer, and polysaccharides as the backbone. When the pH deviates excessively from the window period, it may cause excessive protonation of alkaloids, leading to electrostatic repulsion, or cause alkaloid ionization, reducing the electrostatic interaction between ion pairs, thus affecting the overall synergistic effect of the composition.

[0055] Comparative Example 1

[0056] In this comparative example, a completely different process route was adopted from that in Example 1. Following the method of patent CN101084989A, the active ingredients in Sophora flavescens root, Platycladus orientalis leaf, and Centella asiatica whole herb (raw material ratio is the same as in Example 1) were extracted separately. After purification by D101 macroporous resin, the purified extracts were subjected to simple physical mixing.

[0057] Comparative Example 2

[0058] Unlike Example 1, in S3 of this comparative example, precipitation was carried out under alkaline conditions and the pH was adjusted to 9.0. All other aspects were the same as in Example 1.

[0059] Comparative Example 3

[0060] Unlike Example 1, step S3 is omitted. The extract obtained by the three-step extraction method in S2 is concentrated and then dried, pulverized and sieved according to the method in Example 1 to obtain the composition.

[0061] Comparative Example 4

[0062] The difference between this comparative example and Example 1 is that in S2, water extraction is used instead of the three-step extraction operation to obtain the extract. The conditions for water extraction are: material-to-liquid ratio of 1 g: 8 mL, extraction temperature of 95°C, extraction twice, each extraction for 1.5 h, to obtain the composition.

[0063] Comparative Example 5

[0064] The difference between this comparative example and Example 1 is that in S2, alcohol extraction was used instead of the three-step extraction operation to obtain the extract. The extraction conditions using 70% ethanol were: material-to-liquid ratio of 1 g:10 mL, extraction temperature of 80°C, extraction twice, and extraction for 3 hours each time to obtain the composition.

[0065] Comparative Example 6

[0066] The difference between this comparative example and Example 1 is that in S2, supercritical CO2 extraction is used instead of the three-step extraction operation to obtain the extract. The conditions for supercritical CO2 extraction are the same as in Example 1, and the composition is obtained.

[0067] Experimental Example 1

[0068] In this experimental example, the content of active ingredients in the compositions obtained by different extraction processes of Comparative Examples 3-6 and Example 1 was further determined. The active ingredients in the compositions obtained by different extraction processes were divided into three categories according to polarity: non-polar segment (i.e., volatile oil + triterpene acid components), medium polar segment (flavonoid glycosides, saponins, etc.), and polar segment (polysaccharides, alkaloid salts). The specific content of each component in the composition is shown in Table 2 below.

[0069] Table 2. Content of active ingredients in compositions obtained by different extraction processes experimental group Total extraction rate / % Non-polar segment (volatile oil + triterpenic acid) / % Medium polarity segment (flavonoid glycosides + saponins) / % Polar segment (polysaccharide + alkaloid salt) / % Example 1 35.2 14.8 18.5 11.9 Comparative Example 3 26.2 8.5 10.2 7.5 Comparative Example 4 28.5 1.2 8.5 18.8 Comparative Example 5 32.8 12.5 15.2 5.1 Comparative Example 6 4.0 3.8 0.2 0

[0070] As shown in Table 2, the total extraction rate of the composition using the method employed in Example 1 of this invention reached 35.2%, with a relatively balanced proportion of non-polar, medium-polar, and polar components, accounting for 14.8%, 18.5%, and 11.9% respectively, laying the foundation for the subsequent efficacy of the composition.

[0071] In addition, Comparative Example 3, based on Example 1, also adopted a three-step extraction method, but omitted the pH-induced precipitation step in S3. As can be seen from the data in the table, the total extraction rate of the composition was 26.2%. Not only was the total extraction rate significantly reduced, but the active ingredients in each polar segment were also greatly reduced, and the component ratio was seriously unbalanced. The possible reason is that after omitting the pH-induced precipitation step, acidic components such as triterpenoids could not be selectively enriched and precipitated through pH 5.5 control. At the same time, the lack of a precipitate as a solid carrier to encapsulate and protect the active ingredients led to thermal degradation of heat-sensitive components (such as asiatic acid and quercetin) during the concentration and drying process. More importantly, without low-temperature static crystallization and centrifugation, a large number of soluble impurities (small molecule sugars, inorganic salts, pigments) formed a mixture with the active ingredients, causing the loss of effective ingredients during the drying process. Furthermore, polar components such as alkaloid salts were lost with the supernatant due to the lack of enrichment by the precipitate phase. Ultimately, the total extraction rate of the composition was reduced by 25.6% compared to Example 1, the component ratio of the three polar segments was unbalanced, and the purity and efficacy synergy were greatly reduced.

[0072] In Comparative Examples 4-6, only one method was used to extract the active ingredients from the plant-based raw materials. The results show that the extraction effect of a single solvent is limited, and only one polar component can be extracted. For example, in Comparative Example 4, only water was used for extraction, and the volatile oil components in the raw materials were difficult to enrich or were damaged or lost due to prolonged high temperature. In Comparative Example 5, only 70% extraction was used, which prevented the extraction of a large number of polysaccharide components in the raw materials. In Comparative Example 6, only supercritical CO2 extraction was used, which only achieved good enrichment of non-polar components. All of the above extraction processes resulted in a large waste of raw materials, and the content of active ingredients in the obtained composition was damaged, which limited its efficacy.

[0073] Experimental Example 2

[0074] Transient receptor potential vanillic acid subtype 1 (TRPV1 receptor) is a non-selective cation channel widely expressed in sensory neuron terminals, keratinocytes, and immune cells in the skin. It can be activated by a variety of endogenous and exogenous stimuli, including capsaicin, heat (>43°C), acid, and inflammatory mediators. Therefore, TRPV1 receptor has become a key target with great potential for developing products to soothe sensitive skin. Effectively inhibiting the overactivation of TRPV1 receptor can simultaneously relieve neurosensory discomfort and neurogenic inflammation from the root cause, achieving multi-dimensional intervention for sensitivity symptoms.

[0075] In this invention, the inhibition rate of the compositions prepared by the methods of Example 1 and Comparative Examples 1-3 on TRPV1 receptors was measured respectively. The soothing and anti-allergic effects of the compositions obtained by each method were verified by the inhibition effect. The results are shown in Table 3.

[0076] Table 3. Results of verification of the soothing and anti-allergic effects of different compositions experimental group Total return Coefficient of Synergy (CI) <![CDATA[TRPV1 inhibitor IC 50 (μg / mL)]]> Example 1 9.30% 0.52 8.5 Comparative Example 1 8.50% 0.92 18.5 Comparative Example 2 6.20% 1.15 22.3 Comparative Example 3 7.80% 0.78 15.2

[0077] The data in the table show that the composition prepared by the method of Example 1 of this invention exhibits the strongest synergistic effect among its components, with a half-inhibition rate of 8.5 μg / mL against TRPV1 receptor. In Comparative Example 1, after extracting each raw material component using traditional physical methods, specific monomers were separated by resin, and the composition was further obtained by simple physical mixing. The composition showed poor synergy, with a CI value of 0.92, indicating poor inhibition of TRPV1 receptor. Furthermore, the preparation process of the composition was cumbersome, and the resin consumption greatly increased the production cost of the composition.

[0078] In Comparative Example 2, a strong alkaline environment was used to precipitate the composition. The strong alkaline environment destroyed the structure of the triterpenic acid, causing an imbalance in its ratio with the alkaloids. Ultimately, this resulted in a certain antagonistic effect between the components of the composition, with a CI value greater than 1. The half-inhibition rate of the TRPV1 receptor was 22.3 μg / mL, and the inhibition effect was only 1 / 4 of that in Example 1.

[0079] In Comparative Example 3, the pH was not adjusted, resulting in a high impurity content in the obtained composition and dilution of the active ingredient concentration. This led to an increase in the synergistic coefficient (CI) of the composition to 0.78, weakening the synergistic effect; the TRPV1 receptor half-inhibition rate (IC50) was also reduced. 50 The concentration was 15.2 μg / mL, and the soothing and anti-allergic efficacy decreased by approximately 44% compared to Example 1. Furthermore, due to the lack of selective enrichment and purification through pH-induced precipitation, the extraction rates and relative proportions of the three major active ingredients—triterpenoid acids, flavonoid glycosides, and alkaloid salts—deviated from the optimal range. The total yield of the composition was only 7.80%, lower than the 9.30% of Example 1. Moreover, the product stability decreased, and precipitation and stratification were prone to occur during storage, affecting the quality and efficacy sustainability of the composition.

[0080] Experimental Example 3

[0081] The structures of the compositions obtained in Example 1 and Comparative Example 3 were characterized, and the analysis and comparison of the characterization results are shown in Table 4.

[0082] Table 4. Structural characterization results of each composition

[0083] Table 4 shows that the FT-IR in the composition of Example 1 is at 3400 cm⁻¹ -1 The peak broadened significantly, from 1650 to 1635 cm⁻¹. -1The shift peaks are prominent, a new melting peak appears on the DSC display at 185℃, the original peak weakens, and XRD diffraction results show broadening of the diffraction peaks. All of these indicate that the composition has formed a new phase and molecular interaction forces have been established. In contrast, characterization data of the composition in Comparative Example 3 shows that the characteristic peaks of the three components are simply superimposed, with poor intermolecular forces and no new phase product appearing. Furthermore, the composition obtained in Example 1 has a more uniform particle size, D... 50 At 35 μm, the Zeta potential is close to neutral, and its stability is much higher than that of the composition in Comparative Example 3 (D). 50 =125 μm), which can exist stably in different application scenarios.

[0084] Application Example 1

[0085] A facial soothing and repairing essence containing the soothing and anti-allergic composition of Example 1 is shown in Table 5 below.

[0086] Table 5 Facial Soothing and Repairing Essence Formula Element content / % effect Example 1: Soothing and Anti-allergic Composition 3 Soothing core (high concentration) Ceramide NP 2 Barrier repair cholesterol 0.8 Barrier repair fatty acid 1.5 Barrier repair Panthenol 3 Moisturizing and Repairing Hyaluronic acid 0.3 Moisturizing film formation 1,3-Propanediol 5 Solvent + Moisturizer Carbomer 980 0.3 Thickening Arginine 0.3 Neutralization (pH 5.8) Deionized water margin preservative Appropriate amount

[0087] 1.1 Evaluation of Human Efficacy

[0088] Thirty-two volunteers with facial sensitivity were randomly selected, and the experiment lasted for 28 days. The results are shown in Table 6.

[0089] Table 6. Efficacy Evaluation of Facial Soothing and Repairing Essence index Baseline 14 days 28 days rate of change Skin sensitivity (stirring test, 0-4) 3.2±0.8 1.8±0.6 1.2±0.5 -62.50% Reddish area (%) 12.5±3.5 6.8±2.1 3.5±1.8 -72.00% <![CDATA[TEWL(g / h / m 2 )]]> 18.5±4.2 12.8±3.5 10.2±3.0 -44.90% skin moisture content 38.2±6.5 52.6±7.2 58.3±8.5 52.60%

[0090] The results in the table show that after 28 days of use, the facial soothing and repairing essence reduced skin sensitivity by 62.5%, significantly reduced redness on the skin surface, reduced transepidermal water loss by up to 44.9%, and significantly increased skin moisture content.

[0091] 1.2 Accelerated stability (40℃ / 75%RH, 3 months): Activity remained >90%, and CI remained stable at 0.48~0.53.

[0092] Application Example 2

[0093] A scalp-soothing and anti-dandruff shampoo, the formula of which is shown in Table 7 below.

[0094] Table 7. Formulas for Soothing and Anti-Dandruff Shampoo Element content(%) effect Example 1: Soothing and Anti-allergic Composition 1.5 Soothing core (low to medium concentration) Piroctone ethanolamine salt OCT 0.5 Anti-dandruff main salicylic acid 0.3 Keratin Regulation PCA Zinc 0.8 Oil control and antibacterial SLES 10 clean Cocamidopropyl Betaine 4 Foaming and gentle Menthol 0.2 Instant relief from itching Panthenol 1.5 Scalp Repair Citric acid Appropriate amount Adjust the pH to 5.5. Deionized water margin preservative Appropriate amount

[0095] Human efficacy evaluation (60 volunteers with dandruff and sensitive scalp, 28 days), results are shown in Table 8 below.

[0096] Table 8. Effects of Scalp Soothing and Anti-Dandruff Shampoo Application index Baseline 14 days 28 days rate of change Dandruff rating (0-4) 2.8±0.6 1.4±0.5 0.8±0.4 -71.40% Scalp itching VAS (0-10) 6.5±1.5 2.8±1.2 1.5±0.8 -76.90% Area of ​​scalp redness (%) 18.3±5.2 8.5±3.1 3.8±2.2 -79.20% <![CDATA[Malassezia count (CFU / cm 2 )]]> <![CDATA[3.2×10 4 ]]> <![CDATA[7.5×10 3 ]]> <![CDATA[3.8×10 3 ]]> -88.10%

[0097] As shown in Table 8, the control group (2% OCT + 0.3% salicylic acid, without the soothing and anti-allergic composition prepared in this invention) experienced a dandruff reduction rate of -58.3%, a pruritus reduction of -45.2%, and a redness reduction of -38.5% after 28 days of use. In contrast, the anti-dandruff shampoo provided by this invention achieved a pruritus reduction rate and a scalp redness reduction rate of over 76%, demonstrating the superiority of the product provided by this invention.

[0098] Application Example 3

[0099] Table 9. Verification of Multiple Uses of a Single Material Across Scenarios Application scenarios Raw material addition amount Core Compatibility 28-day main effects Improvement rate Facial Sensitive Repair 3.00% Ceramides + Cholesterol + Fatty Acids Redness area decreased, TEWL decreased, sensitivity score decreased. -72%，-44%，-62.5% Facial Acne Assistance 2.00% Salicylic acid + nicotinamide Acne redness and swelling decrease, acne scars fade increase. -69%，+47% Scalp soothing and dandruff removal 1.50% OCT + Salicylic Acid + Zinc PCA Dandruff decreased, itching decreased, Malassezia decreased -71%，-77%，-88% Scalp cosmetic surgery 3.00% Panthenol + Niacinamide Stinging pain VAS decreases, redness and swelling area decreases. -89%，-85% Dry and itchy body 1.00% Urea + Shea Butter Dryness and itching ↓ -65%

[0100] The above application results show that the soothing and anti-allergic composition raw materials provided by the present invention can achieve significant soothing effects in multiple scenarios such as face, scalp, and body by adjusting the amount added (1%~3%) and compatibility. The CI values ​​are all <0.6, further confirming the feasibility of using one material for multiple purposes.

[0101] The above are merely preferred embodiments of the present invention and do not limit the scope of the patent. All equivalent changes and modifications made within the scope of the present invention should still fall within the scope of the present invention.

Claims

1. A soothing and anti-allergic composition, characterized in that, include: Sophora flavescens root extract, Centella asiatica extract, and Platycladus orientalis leaf extract are obtained by mixing Sophora flavescens root, Centella asiatica, and Platycladus orientalis leaf in a mass ratio of (2~4):(2~4):(1~2), followed by supercritical CO2 extraction, organic solvent extraction, and water extraction, and then combining the extracts.

2. The method for preparing the soothing and anti-allergic composition according to claim 1, characterized in that, The steps include the following: Preparation of raw materials for S1: Take Sophora flavescens root, Centella asiatica and Platycladus orientalis leaves and mix them in a mass ratio of (2~4):(2~4):(1~2), crush and sieve them for later use; S2 three-step extraction: The raw material powder in S1 is extracted sequentially with supercritical CO2, ethanol with a volume fraction of 60%~80% and water. The extracts are combined and concentrated under reduced pressure to obtain a concentrated solution. The conditions for supercritical CO2 extraction are: extraction pressure 25~35 MPa, temperature 40~50℃, CO2 flow rate 20~30 L / h, and entrainer is ethanol with a volume fraction of 5%~10%. The temperature for ethanol extraction is 75~85℃, and the temperature for water extraction is 90~100℃. Induction of S3 precipitation: Adjust the pH of the concentrated solution in S2 to 5.0~6.5, control the temperature at 25~40℃, stir at 100~300rpm for 1~2 h, and then let it stand at 4~10℃ for 12~24 h to promote sedimentation. Collect the precipitate by centrifugation and filtration. S4 Purification and Drying: The precipitate obtained in S3 was washed with ethanol at pH 5.0-5.5 and a volume fraction of 20%-30%, dried, pulverized and sieved to obtain the soothing and anti-allergic composition.

3. The preparation method according to claim 2, characterized in that, The mass ratio of Sophora flavescens root, Centella asiatica and Platycladus orientalis leaf in S1 is (2~3):(2~3):

1.

4. The preparation method according to claim 2, characterized in that, The conditions for supercritical CO2 extraction described in S2 are: extraction pressure 28~33 MPa, temperature 42~46℃, CO2 flow rate 22~26 L / h, extraction time 1.5~2.5 h, and entrainer 8% ethanol by volume.

5. The preparation method according to claim 2, characterized in that, When performing ethanol or water extraction as described in S2, the mass-to-volume ratio of the raw material to be extracted to ethanol or water is 1 g: 8~12 mL, and the extraction is performed 1~3 times, with each extraction lasting 1.5~2 h.

6. The preparation method according to claim 2, characterized in that, The relative density of the concentrated solution obtained by vacuum concentration as described in S2 is 1.05~1.

15.

7. The preparation method according to claim 2, characterized in that, In S3, the pH of the concentrate is adjusted with 0.5~2 mol / L citric acid or lactic acid solution while stirring.

8. A facial repair cosmetic comprising the composition of claim 1, characterized in that, The composition accounts for 2% to 5% of the mass of the facial repair cosmetic, the pH of the facial repair cosmetic is 5.0 to 6.5, and the cosmetic also contains at least ceramide, cholesterol, and fatty acids.

9. A dandruff-relieving shampoo for scalp soothing, characterized in that, The shampoo contains the soothing and anti-allergic composition of claim 1, as well as pyrrolidone ethanolamine salt, salicylic acid, and zinc salt, wherein the soothing and anti-allergic composition is added to the shampoo at a mass of 0.5% to 3%, and the pH of the shampoo is 5.0 to 6.

0.

10. A body lotion, characterized in that, The body lotion contains the soothing and anti-allergic composition of claim 1, wherein the soothing and anti-allergic composition is added to the body lotion at a mass of 1% to 2%, and the body lotion also contains urea and shea butter.

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