Prinsepia utilis royle anti-allergy composition and application thereof in sensitive skin care

Abstract

The invention discloses a prinsepia utilis royle anti-allergy composition and application thereof in sensitive skin care. The prinsepia utilis royle allergy-relieving composition is prepared by scientifically compounding three special plants including prinsepia utilis royle, myrothamnus flabellifolia and mangnolia officinalis and adopting a plurality of advanced extraction technical means such as ultrasonic assistance, low-temperature control, inert gas protection and secondary molecular distillation. A novel cosmetic composition which is based on a multi-target mechanism and has instant soothing and long-term repairing effects is prepared.

Description

Technical Field

[0001] This invention relates to the field of cosmetics, specifically to a soothing composition of *Cynanchum paniculatum* and its application in the care of sensitive skin. Background Technology

[0002] Consumer demand for cosmetics with "soothing," "repairing," and "anti-irritation" effects has increased significantly, and soothing skincare products have become an important sub-category of functional cosmetics. The soothing effect typically refers to a product's ability to reduce or prevent skin discomfort caused by external stimuli (such as ultraviolet rays, chemicals, temperature changes, or mechanical friction), including subjective symptoms such as stinging, burning, redness, and itching, and to a certain extent, inhibiting the release of inflammatory factors and regulating hypersensitive nerve states.

[0003] From a mechanistic perspective, skin sensitivity is related to multiple factors, primarily including: damage to the skin barrier structure leading to easier penetration of external irritants; abnormal activation of epidermal sensory nerve endings and excessive response of transient receptor potential (TRP) channels (such as TRPV1); release of pro-inflammatory mediators such as histamine, interleukin-6 (IL-6), and tumor necrosis factor-α (TNF-α) from local immune cells (such as Langerhans cells and mast cells); and further amplification of inflammatory signals due to imbalance in the skin microecology. Therefore, ideal soothing effects should encompass a multi-dimensional synergistic effect including barrier repair, nerve calming, anti-inflammatory regulation, and microecological balance.

[0004] However, existing soothing cosmetics still have significant technological limitations. First, most products rely on a single classic ingredient (such as bisabolol, dipotassium glycyrrhizate, allantoin, etc.), which, while possessing certain anti-inflammatory or soothing effects, cannot fully intervene in the complex pathways that lead to sensitivity. Second, some soothing formulas neglect the reconstruction of the skin barrier function, only pursuing an immediate "cooling sensation" or "redness reduction," and cannot achieve long-lasting protection.

[0005] Prinsepia utilis Royle, a distinctive woody oilseed plant mainly distributed in high-altitude regions of Yunnan and Sichuan provinces in my country, has demonstrated significant application value in skin soothing and barrier repair in recent years. Chinese patent document CN108553527A discloses a method for preparing a total flavonoid extract from Prinsepia utilis kernels. This method uses Prinsepia utilis kernels as a single raw material, and through steps such as defatting, reflux extraction with alcohol or aqueous solution, and separation and purification with macroporous resin column, it enriches the total flavonoid extract. While this technology achieves the enrichment of specific active ingredients (total flavonoids) from Prinsepia utilis, it only targets a single plant material, limiting the extraction target to flavonoid compounds and failing to fully utilize the synergistic skincare effects of multiple active ingredients (such as unsaturated fatty acids and polyphenols) in Prinsepia utilis. Furthermore, the process involves heated reflux extraction and macroporous resin separation, which are relatively cumbersome, and the heating process may cause loss of heat-sensitive active ingredients.

[0006] Therefore, the market urgently needs to develop a new cosmetic composition based on a multi-target mechanism that combines immediate soothing and long-term repair capabilities. Summary of the Invention

[0007] The technical problem to be solved by the present invention is to provide a novel cosmetic composition based on a multi-target mechanism that has both immediate soothing and long-term repair effects.

[0008] The specific technical solution of the present invention is as follows: A soothing composition made from sea buckthorn fruit is prepared by a method comprising the following steps: (1) The fruit of the Chinese prickly ash, the myrrh, and the magnolia bark were screened, dried, and pulverized to obtain a mixed powder. This step aims to pre-treat the three raw materials according to a unified pre-treatment standard in order to improve the efficiency and uniformity of the subsequent extraction process.

[0009] In some embodiments, the prickly ash fruit is pulverized to 40-60 mesh, the myrrh to 60-80 mesh, and the magnolia bark to 40-60 mesh, and then they are mixed evenly in a weight ratio of 5-10:1-5:1-3.

[0010] (2) Add antioxidants and enzyme inhibitors to the mixed powder, then extract with an ethanol-ethyl acetate composite solvent, and collect the supernatant after filtration and centrifugation. The purpose of adding antioxidants and enzyme inhibitors in this step is to inhibit the oxidation of active ingredients and the degradation of magnolol.

[0011] In some embodiments, the amount of antioxidant added is 0.01-0.05% of the total weight of the mixed powder, and the antioxidant is a mixture of vitamin E and ascorbate palmitate in a weight ratio of 1-5:1-5.

[0012] In some embodiments, the enzyme inhibitor is disodium EDTA, and the amount added is 0.01-0.1% of the total weight of the mixed powder.

[0013] This extraction process uses an ethanol-ethyl acetate composite solvent system, which takes into account the solubility of both polar and non-polar components, and is conducive to the efficient dissolution of various types of active ingredients.

[0014] In some embodiments, the volume ratio of ethanol to ethyl acetate in the ethanol-ethyl acetate composite solvent is 1-3:1, the ratio of the mixed powder to the composite solvent is controlled at 1:10-15 g / mL, and nitrogen gas is introduced for protection throughout the process.

[0015] In some embodiments, the extraction conditions are: constant temperature of 45°C, stirring at 80 r / min, combined with 200W ultrasonic-assisted extraction, intermittent ultrasonication for 3 seconds at a time, and extraction time of 2.5 hours. Maintaining the temperature at 45°C avoids degradation of heat-sensitive components; the intermittent ultrasonic mode effectively prevents localized overheating and ensures component stability. An inert atmosphere is used throughout the process, with nitrogen gas purging to effectively isolate oxygen and prevent degradation or deterioration of easily oxidized components (such as phenols and unsaturated fatty acids), thereby improving product purity and stability.

[0016] In some embodiments, the filtration and centrifugation conditions are as follows: after extraction, the coarse filter residue is first removed by filtration through gauze, and then the filtrate is placed in a high-speed centrifuge and centrifuged at 4500 r / min for 20 min, and the supernatant is collected; the filter residue is replenished with 1 / 3 of the original amount of composite solvent, and the extraction is repeated for 30 min, and the two supernatants are combined. This step adopts a high-yield recovery strategy: the extract undergoes two-stage solid-liquid separation through coarse filtration (gauze) + high-speed centrifugation (4500 r / min, 20 min) to ensure clarity; the filter residue is replenished with 1 / 3 of the original amount of fresh composite solvent, and a second short-time extraction (30 min) is performed, and the two supernatants are combined, which significantly improves the total yield of the target component.

[0017] The process in step (2) integrates solvent compounding, ultrasonic assistance, low temperature control, inert protection and residue re-extraction, and has the advantages of high efficiency, stability, energy saving and high yield. It is suitable for the green extraction of natural products that are sensitive to oxidation and unstable to heat.

[0018] (3) The heavy components were collected by two-stage molecular distillation to obtain the soothing composition of *Cynanchum paniculatum*. Compared with conventional vacuum concentration, molecular distillation can more thoroughly remove solvent residues and further purify active ingredients. At the same time, the low-temperature operation can better preserve the activity of the components. More importantly, the low-temperature and high-vacuum environment of molecular distillation can minimize the oxidation of unsaturated fatty acids in *Cynanchum paniculatum*, the degradation of magnolol, and the denaturation of active factors in *Myrothamnus flabellifolia*. At the same time, it can further improve the purity of the extract, control the solvent residue, and better meet the requirements of raw materials for mid-to-high-end skin care products.

[0019] In some embodiments, the specific process of step (3) is as follows: the combined supernatant is first filtered through a 0.22 μm organic filter membrane to remove minute impurities (to avoid impurities affecting the molecular distillation effect); then the filtrate is sent to a molecular distillation device and a two-stage molecular distillation process is adopted. The specific parameters are: first-stage distillation (solvent removal): evaporation temperature 75-80℃, condensation temperature 20℃, vacuum degree 0.001 MPa, feed rate 2 mL / min, scraper rotation speed 200 r / min, to remove the ethanol-ethyl acetate composite solvent (the solvent can be recycled and reused); second-stage distillation (purification): the evaporation temperature is adjusted to 110-115℃, condensation temperature 30℃, vacuum degree 0.0005 MPa, feed rate 1.5 mL / min, scraper rotation speed 250 r / min, to remove residual trace impurities (such as a small amount of water-soluble small molecule impurities), and the heavy components are collected, which is a high-purity viscous mixed extract.

[0020] (4) Add 5% of the weight of the extract to the extract obtained in step (3) and stir to dissolve, forming a uniform oily system. Place it in a brown sealed container and refrigerate at 4°C for later use.

[0021] This invention provides a soothing composition of *Prickly pear* fruit and its preparation method, which has the following advantages compared with the prior art: 1. Multi-target synergy for immediate relief and long-term repair This invention scientifically combines three distinctive plants—Rhizoma Cirsium japonicum (thorn fruit), Herba Frangipani (myrothamnus flabellifolia), and Cortex Magnoliae Officinalis (magnolia officinalis)—to construct a multi-target mechanism of action. Rhizoma Cirsium japonicum is rich in unsaturated fatty acids and various active nutrients, enabling rapid penetration and repair of the skin barrier; Herba Frangipani (myrothamnus flabellifolia) extract possesses extremely strong moisturizing and repairing abilities, instantly soothing dry and uncomfortable skin; and Cortex Magnoliae Officinalis contains active ingredients such as magnolol, which have excellent antioxidant and anti-inflammatory effects. The synergistic effect of these three ingredients not only quickly alleviates skin sensitivity but also strengthens the skin from the root, achieving both immediate soothing and long-term repair.

[0022] 2. Integrated and innovative processes provide comprehensive protection for active ingredients. The preparation method of this invention integrates multiple advanced technologies such as solvent compounding, ultrasound-assisted extraction, low-temperature control, inert gas protection, and two-stage molecular distillation, forming a highly efficient, mild, and stable extraction and purification system. Through multiple measures including antioxidants, enzyme inhibitors, low-temperature extraction, intermittent ultrasound, and continuous nitrogen protection, the oxidation of unsaturated fatty acids in *Cynanchum paniculatum*, the degradation of magnolol components, and the inactivation of thermosensitive active factors in *Myrothamnus flabellifolia* are effectively avoided, thus preserving the natural activity of the raw materials to the greatest extent possible.

[0023] 3. Molecular distillation purification significantly improves product quality. This invention innovatively applies two-stage molecular distillation technology to the purification of this composition. Compared to traditional vacuum concentration, molecular distillation operates at a higher vacuum and lower temperature, which not only more thoroughly removes solvent residues such as ethanol and ethyl acetate, making the product safer and purer, but also effectively removes small molecule impurities, further enriching the target active ingredients. The resulting high-purity, viscous extract has a pure odor and excellent color, fully meeting the stringent quality requirements for raw materials in mid-to-high-end skincare products.

[0024] 4. High extraction efficiency and environmentally friendly process. By employing a composite solvent of ethanol and ethyl acetate with different polarities, both polar and non-polar active components in the raw materials can be dissolved efficiently and simultaneously. Combining ultrasound-assisted extraction and a two-stage extraction strategy (re-extraction of residue) significantly improves the overall yield of the target components and reduces raw material waste. Furthermore, the solvent used in the molecular distillation process can be recycled and reused, reducing production costs and embodying a green and environmentally friendly approach.

[0025] 5. The product has good stability and excellent application performance. The final product, formulated with the addition of sea buckthorn fruit oil, forms a homogeneous and stable oily system, facilitating its subsequent addition to various cosmetic formulations. The entire preparation process, through precise control of temperature, vacuum, and inert atmosphere, ensures the chemical and physical stability of the composition throughout its shelf life. This composition can be widely used in high-value-added soothing and repairing skincare products such as serums, creams, and masks. Attached Figure Description

[0026] Figure 1 The appearance of the oil droplet essences obtained in Examples 4 and 5 Detailed Implementation The embodiments described in this specification are for illustrative purposes only and do not limit the scope of protection of this invention. The scope of protection of this invention is defined only by the claims, and any omissions, substitutions, or modifications made based on the embodiments disclosed in this invention will fall within the scope of protection of this invention.

[0027] As used herein, the terms “prepared from” and “comprising” are synonymous. The terms “comprising,” “including,” “having,” “containing,” or any other variations thereof, as used herein, are intended to cover non-exclusive inclusion. For example, a composition, step, method, article, or apparatus that includes the listed elements is not necessarily limited to those elements, but may include other elements not expressly listed or elements inherent to such composition, step, method, article, or apparatus.

[0028] When a quantity, concentration, or other value or parameter is expressed as a range, a preferred range, or a range defined by a series of upper and lower preferred values, this should be understood as specifically disclosing all ranges formed by any pair of any upper or preferred value with any lower or preferred value, regardless of whether the range is disclosed individually. For example, when the range “1 to 5” is disclosed, the described range should be interpreted as including the ranges “1 to 4”, “1 to 3”, “1 to 2”, “1 to 2 and 4 to 5”, “1 to 3 and 5”, etc. When numerical ranges are described herein, unless otherwise stated, the range is intended to include its endpoints and all integers and fractions within that range.

[0029] Furthermore, the indefinite articles “a” and “an” preceding the elements or components of this invention do not impose any limitation on the quantity requirement (i.e., the number of times) of the elements or components. Therefore, “an” or “a” should be interpreted as including one or at least one, and the singular form of an element or component also includes the plural form, unless the quantity clearly refers to the singular form.

[0030] To enhance understanding of the present invention, the present invention will be further described in detail below with reference to embodiments. These embodiments are only used to explain the present invention and do not constitute a limitation on the scope of protection of the present invention.

[0031] Example 1 A soothing composition made from sea buckthorn fruit is prepared by the following method: (1) Raw material pretreatment: Prickly pear fruit is crushed and passed through a 50-mesh sieve, Myrothamnus fruticosa is crushed and passed through a 70-mesh sieve, and Magnolia officinalis is crushed and passed through a 50-mesh sieve. 8 parts of Prickly pear fruit powder, 3 parts of Myrothamnus fruticosa powder, and 2 parts of Magnolia officinalis powder are weighed by weight and mixed evenly to obtain a mixed powder.

[0032] (2) Extraction: Add 0.03% by weight of antioxidant and 0.05% by weight of disodium EDTA to the mixed powder. The antioxidant is a mixture of vitamin E and ascorbate palmitate in a weight ratio of 3:1. Add ethanol-ethyl acetate composite solvent at a material-to-liquid ratio of 1:12 g / mL, wherein the volume ratio of ethanol to ethyl acetate is 2:1. Nitrogen gas is purged throughout the extraction process. Under constant temperature of 45℃, the mixture is stirred at 80 r / min and subjected to 200W ultrasonic-assisted extraction in an intermittent ultrasonic mode (3 seconds of ultrasonication followed by 3 seconds of pause) for 2.5 hours. After extraction, filter the mixture through gauze to remove coarse residue. Centrifuge the filtrate at 4500 r / min for 20 minutes and collect the supernatant. Add 1 / 3 of the original volume of fresh composite solvent to the filter residue and extract again for 30 minutes. Combine the two supernatants after centrifugation.

[0033] (3) Purification: The combined supernatant was first filtered through a 0.22 μm organic filter membrane, and then subjected to two-stage molecular distillation. First-stage distillation (solvent removal): Evaporation temperature 78℃, condensation temperature 20℃, vacuum degree 0.001 MPa, feed rate 2 mL / min, scraper rotation speed 200 r / min, to remove ethanol-ethyl acetate solvent (recovery). Second-stage distillation (purification): Evaporation temperature 112℃, condensation temperature 30℃, vacuum degree 0.0005 MPa, feed rate 1.5 mL / min, scraper rotation speed 250 r / min, to collect the heavy components, thus obtaining the Qingci fruit soothing composition.

[0034] (4) Preparation: Add 5% of the weight of the extract to the above extract, stir to dissolve evenly, and obtain a uniform oily system. Place it in a brown sealed container and refrigerate at 4°C for later use.

[0035] Example 2 A soothing composition made from sea buckthorn fruit is prepared by the following method: (1) Raw material pretreatment: Prickly pear fruit is crushed through a 40-mesh sieve, Myrothamnus fruticosa is crushed through a 60-mesh sieve, and Magnolia officinalis is crushed through a 40-mesh sieve. Weigh out 5 parts of Prickly pear fruit powder, 5 parts of Myrothamnus fruticosa powder, and 1 part of Magnolia officinalis powder by weight, and mix them evenly to obtain a mixed powder.

[0036] (2) Extraction: Add 0.01% by weight of antioxidant and 0.1% by weight of disodium EDTA to the mixed powder. The antioxidant is a mixture of vitamin E and ascorbate palmitate in a weight ratio of 1:1. Add ethanol-ethyl acetate composite solvent at a material-to-liquid ratio of 1:10 g / mL, wherein the volume ratio of ethanol to ethyl acetate is 1:1. Nitrogen gas is purged throughout the extraction process. Extraction conditions: constant temperature of 45℃, stirring at 80 r / min, 200W ultrasonic assistance, intermittent ultrasonication for 3 seconds and then stopping for 3 seconds, extraction time of 2.5 hours. After extraction, the following operations are performed: filtration, centrifugation, and re-extraction of the filter residue, as in Example 1. Combine the supernatants.

[0037] (3) Purification: The supernatant was filtered through a 0.22 μm filter membrane and then subjected to two-stage molecular distillation: the first-stage distillation evaporation temperature was 75℃, the condensation temperature was 20℃, the vacuum degree was 0.001 MPa, the feed rate was 2 mL / min, and the scraper rotation speed was 200 r / min; the second-stage distillation evaporation temperature was 110℃, the condensation temperature was 30℃, the vacuum degree was 0.0005 MPa, the feed rate was 1.5 mL / min, and the scraper rotation speed was 250 r / min. The heavy components were collected.

[0038] (4) Preparation: Same as in Example 1.

[0039] Example 3 A soothing composition made from sea buckthorn fruit is prepared by the following method: (1) Raw material pretreatment: Same as in Example 1, the mixed powder ratio is 10 parts of Qingci fruit powder, 1 part of Myrothamnus fruticosa powder and 3 parts of Magnolia officinalis powder.

[0040] (2) Extraction: Add 0.05% by weight of antioxidant (vitamin E: ascorbate palmitate = 5:1) and 0.01% by weight of disodium EDTA to the mixed powder. Add ethanol-ethyl acetate composite solvent (volume ratio 3:1) at a material-to-liquid ratio of 1:15 g / mL. The remaining extraction conditions are the same as in Example 1.

[0041] (3) Purification: First-stage distillation evaporation temperature 80℃, second-stage distillation evaporation temperature 115℃, other parameters are the same as in Example 1.

[0042] (4) Preparation: Same as in Example 1.

[0043] Comparative Example 1 A soothing composition made from sea buckthorn fruit is prepared by the following method: (1) Raw material pretreatment: Prickly pear fruit is crushed and passed through a 50-mesh sieve, Myrothamnus fruticosa is crushed and passed through a 70-mesh sieve, and Magnolia officinalis is crushed and passed through a 50-mesh sieve. 8 parts of Prickly pear fruit powder, 3 parts of Myrothamnus fruticosa powder, and 2 parts of Magnolia officinalis powder are weighed by weight and mixed evenly to obtain a mixed powder.

[0044] (2) Add 10 times the amount of 70% ethanol, heat and reflux twice for 2 hours each time, combine the extracts, concentrate under reduced pressure to obtain a paste, dry to obtain the extract. Mix the extract with 5% sea buckthorn fruit oil for later use.

[0045] Comparative Example 2 A soothing composition made from sea buckthorn fruit is prepared by the following method: (1) Raw material pretreatment: Crush the prickly pear fruit and pass it through a 50-mesh sieve for later use. Weigh 8 parts of the prickly pear fruit powder by weight and mix them evenly to obtain a mixed powder.

[0046] (2) Extraction: Add 0.03% by weight of antioxidant and 0.05% by weight of disodium EDTA to the mixed powder. The antioxidant is a mixture of vitamin E and ascorbate palmitate in a weight ratio of 3:1. Add ethanol-ethyl acetate composite solvent at a material-to-liquid ratio of 1:12 g / mL, wherein the volume ratio of ethanol to ethyl acetate is 2:1. Nitrogen gas is purged throughout the extraction process. Under constant temperature of 45℃, the mixture is stirred at 80 r / min and subjected to 200W ultrasonic-assisted extraction in an intermittent ultrasonic mode (3 seconds of ultrasonication followed by 3 seconds of pause) for 2.5 hours. After extraction, filter the mixture through gauze to remove coarse residue. Centrifuge the filtrate at 4500 r / min for 20 minutes and collect the supernatant. Add 1 / 3 of the original volume of fresh composite solvent to the filter residue and extract again for 30 minutes. Combine the two supernatants after centrifugation.

[0047] (3) Purification: The combined supernatant was first filtered through a 0.22 μm organic filter membrane, and then subjected to two-stage molecular distillation. First-stage distillation (solvent removal): Evaporation temperature 78℃, condensation temperature 20℃, vacuum degree 0.001 MPa, feed rate 2 mL / min, scraper rotation speed 200 r / min, to remove ethanol-ethyl acetate solvent (recovery). Second-stage distillation (purification): Evaporation temperature 112℃, condensation temperature 30℃, vacuum degree 0.0005 MPa, feed rate 1.5 mL / min, scraper rotation speed 250 r / min, to collect the heavy components, thus obtaining the Qingci fruit soothing composition.

[0048] (4) Preparation: Add 5% of the weight of the extract to the above extract, stir to dissolve evenly, and obtain a uniform oily system. Place it in a brown sealed container and refrigerate at 4°C for later use.

[0049] Comparative Example 3 A soothing composition made from sea buckthorn fruit is prepared by the following method: (1) Raw material pretreatment: The myrothamnus flabellifolia is crushed and passed through a 70-mesh sieve and set aside. Weigh 3 parts by weight of myrothamnus flabellifolia powder and mix them evenly to obtain a mixed powder.

[0050] (2) Extraction: Add 0.03% by weight of antioxidant and 0.05% by weight of disodium EDTA to the mixed powder. The antioxidant is a mixture of vitamin E and ascorbate palmitate in a weight ratio of 3:1. Add ethanol-ethyl acetate composite solvent at a material-to-liquid ratio of 1:12 g / mL, wherein the volume ratio of ethanol to ethyl acetate is 2:1. Nitrogen gas is purged throughout the extraction process. Under constant temperature of 45℃, the mixture is stirred at 80 r / min and subjected to 200W ultrasonic-assisted extraction in an intermittent ultrasonic mode (3 seconds of ultrasonication followed by 3 seconds of pause) for 2.5 hours. After extraction, filter the mixture through gauze to remove coarse residue. Centrifuge the filtrate at 4500 r / min for 20 minutes and collect the supernatant. Add 1 / 3 of the original volume of fresh composite solvent to the filter residue and extract again for 30 minutes. Combine the two supernatants after centrifugation.

[0051] (3) Purification: The combined supernatant was first filtered through a 0.22 μm organic filter membrane, and then subjected to two-stage molecular distillation. First-stage distillation (solvent removal): Evaporation temperature 78℃, condensation temperature 20℃, vacuum degree 0.001 MPa, feed rate 2 mL / min, scraper rotation speed 200 r / min, to remove ethanol-ethyl acetate solvent (recovery). Second-stage distillation (purification): Evaporation temperature 112℃, condensation temperature 30℃, vacuum degree 0.0005 MPa, feed rate 1.5 mL / min, scraper rotation speed 250 r / min, to collect the heavy components, thus obtaining the Qingci fruit soothing composition.

[0052] (4) Preparation: Add 5% of the weight of the extract to the above extract, stir to dissolve evenly, and obtain a uniform oily system. Place it in a brown sealed container and refrigerate at 4°C for later use.

[0053] Comparative Example 4 A soothing composition made from sea buckthorn fruit is prepared by the following method: (1) Raw material pretreatment: Magnolia officinalis powder is crushed and passed through a 50-mesh sieve and set aside. Weigh 2 parts of Magnolia officinalis powder by weight and mix them evenly to obtain mixed powder.

[0054] (2) Extraction: Add 0.03% by weight of antioxidant and 0.05% by weight of disodium EDTA to the mixed powder. The antioxidant is a mixture of vitamin E and ascorbate palmitate in a weight ratio of 3:1. Add ethanol-ethyl acetate composite solvent at a material-to-liquid ratio of 1:12 g / mL, wherein the volume ratio of ethanol to ethyl acetate is 2:1. Nitrogen gas is purged throughout the extraction process. Under constant temperature of 45℃, the mixture is stirred at 80 r / min and subjected to 200W ultrasonic-assisted extraction in an intermittent ultrasonic mode (3 seconds of ultrasonication followed by 3 seconds of pause) for 2.5 hours. After extraction, filter the mixture through gauze to remove coarse residue. Centrifuge the filtrate at 4500 r / min for 20 minutes and collect the supernatant. Add 1 / 3 of the original volume of fresh composite solvent to the filter residue and extract again for 30 minutes. Combine the two supernatants after centrifugation.

[0055] (3) Purification: The combined supernatant was first filtered through a 0.22 μm organic filter membrane, and then subjected to two-stage molecular distillation. First-stage distillation (solvent removal): Evaporation temperature 78℃, condensation temperature 20℃, vacuum degree 0.001 MPa, feed rate 2 mL / min, scraper rotation speed 200 r / min, to remove ethanol-ethyl acetate solvent (recovery). Second-stage distillation (purification): Evaporation temperature 112℃, condensation temperature 30℃, vacuum degree 0.0005 MPa, feed rate 1.5 mL / min, scraper rotation speed 250 r / min, to collect the heavy components, thus obtaining the Qingci fruit soothing composition.

[0056] (4) Preparation: Add 5% of the weight of the extract to the above extract, stir to dissolve evenly, and obtain a uniform oily system. Place it in a brown sealed container and refrigerate at 4°C for later use.

[0057] Example 1: Evaluation of Soothing Effect – Inflammatory Factor Inhibition Test The anti-inflammatory and soothing effects of the compositions of the present invention were evaluated using an in vitro cell model. An inflammation model was established by stimulating RAW264.7 macrophages with lipopolysaccharide (LPS), and the inhibitory effect of the samples on the release of inflammatory factors TNF-α and IL-6 was detected. The specific experiments were conducted in accordance with the methods described in the literature "Sui Haijuan, Jin Ying, Pan Yuexing, et al. Effects of pioglitazone on the release of inflammatory cytokines induced by LPS in astrocytes [J]. Chinese Journal of Pharmacology, 2010, 26(09):1226-1230."

[0058] The soothing compositions of *Cynanchum paniculatum* prepared in Examples 1-3 and Comparative Examples 1-4 were diluted to 50 μg / mL with DMEM medium, added to cells and incubated for 1 h, followed by LPS stimulation for 24 h. Cell supernatants were collected, and TNF-α and IL-6 levels were detected by ELISA. Wells containing only LPS and no sample served as the model control group, while wells containing neither LPS nor sample served as the blank control group. The inhibition rate of inflammatory factors was calculated, and the results are shown in Table 1.

[0059] Table 1 Inhibition rate of inflammatory factors in each test group As shown in Table 1, the compositions of Examples 1-3 significantly inhibited the release of TNF-α and IL-6, with inhibition rates all exceeding 70%, significantly higher than Comparative Example 1 (conventional extraction) and Comparative Examples 2-4 (only one raw material was added). This indicates that the compositions prepared in this invention possess excellent anti-inflammatory and soothing activity, and the extraction and purification process of this invention better preserves the active ingredients.

[0060] Comparative Example 5 The difference from Example 1 is that no antioxidants and enzyme inhibitors are added during extraction, and nitrogen gas is not introduced for protection. The remaining steps are the same as in Example 1.

[0061] Example 2: Stability Test The soothing compositions of *Cypripedium sarmentosum* prepared in Examples 1-3 and Comparative Example 5 were stored in a constant temperature incubator at 45°C for 3 months. Samples were taken at 0 days, 1 month, 2 months, and 3 months to detect the peroxide value (POV) and observe the changes in appearance. The results are shown in Table 2.

[0062] Table 2 Stability Test Records Table 2 shows that the peroxide value of the *Corydalis yanhusuo* soothing compositions prepared in Examples 1-3 did not increase significantly during the accelerated testing, and their appearance remained clear without any rancidity. In contrast, the peroxide value of Comparative Example 5 increased significantly, and signs of rancidity appeared. This indicates that the method of the present invention, through inert protection, low-temperature extraction, and molecular distillation purification, effectively prevents the oxidation of unsaturated fatty acids, resulting in good product stability.

[0063] Example 4 A soothing oil droplet essence comprising the following components in percentage by weight: 3% glycerol 1,3-Propanediol 10% Carbomer 0.2% p-Hydroxyacetophenone 0.6% 1,2-Hexanediol 0.4% Sodium hydroxide 0.03% 5% olive oil Cocoyl alcohol-caprylate / decanoate 3% 1% castor oil / IPDI copolymer Caprylic / Capric Triglyceride 5% 1% Prisepia utilis oil The 5% of the soothing composition of *Prickly pear* fruit prepared in Example 1 Water balance.

[0064] Preparation process: Water, glycerin, 1,3-propanediol, carbomer, p-hydroxyacetophenone, and 1,2-hexanediol were added to an emulsifying pot and heated to 85 degrees Celsius with slow stirring. The pot was then turned on to homogenize and disperse the contents until they were evenly dissolved. Sodium hydroxide was then added and stirred until homogeneous to obtain a dilute gel system. Coco-caprylate / capric acid ester, castor oil / IPDI copolymer, and caprylic / capric acid triglycerides were added to an oil phase pot and heated to dissolve with stirring. Olive (Olea europaea) fruit oil, PRINSEPIAUTILIS oil, and a soothing combination of prickly ash fruit were then added and stirred until homogeneous to obtain the oil phase. The emulsifying pot was turned on with medium-speed stirring and cooled to 60 degrees Celsius. The oil phase was then slowly added to the emulsifying pot and stirred until homogeneous to obtain a soothing essence with a gel system of evenly dispersed fine oil droplets.

[0065] Example 5 A soothing oil droplet essence comprising the following components in percentage by weight: 10% glycerin 1,3-Propanediol 3% Carbomer 0.4% p-Hydroxyacetophenone 0.2% 1,2-Hexanediol 0.8% Sodium hydroxide 0.08% 1% olive oil Cocoyl alcohol-caprylate / decanoate 8% Castor oil / IPDI copolymer 0.5% Caprylic / capric triglycerides 0.3% 5% oil from Prisepia utilis The 1% of the prickly pear fruit soothing composition prepared in Example 2 Water balance.

[0066] Preparation process: Water, glycerin, 1,3-propanediol, carbomer, p-hydroxyacetophenone, and 1,2-hexanediol were added to an emulsifying pot and heated to 85 degrees Celsius with slow stirring. The pot was then turned on to homogenize and disperse the contents until they were evenly dissolved. Sodium hydroxide was then added and stirred until homogeneous to obtain a dilute gel system. Coco-caprylate / capric acid ester, castor oil / IPDI copolymer, and caprylic / capric acid triglycerides were added to an oil phase pot and heated to dissolve with stirring. Olive (Olea europaea) fruit oil, PRINSEPIAUTILIS oil, and a soothing combination of prickly ash fruit were then added and stirred until homogeneous to obtain the oil phase. The emulsifying pot was turned on with medium-speed stirring and cooled to 60 degrees Celsius. The oil phase was then slowly added to the emulsifying pot and stirred until homogeneous to obtain a soothing essence with a gel system of evenly dispersed fine oil droplets.

[0067] Example 3: Moisturizing and Repairing Effects - Human Trial Experiment Thirty volunteers with sensitive facial skin (characterized by dryness, redness, and tightness) were recruited and randomly divided into two groups of 15 each. One group used the soothing oil droplet essence (as described in Example 4), while the other used a commercially available soothing essence. Both were applied twice daily, morning and evening, for four consecutive weeks. Skin stratum corneum moisture content and transepidermal water loss (TEWL) were measured before use and at 2 and 4 weeks after use. The results were averaged and are shown in Table 3.

[0068] Table 3 Human Test Result Recording Sheet Table 3 shows that the soothing oil droplet essence from Example 4 significantly increases the moisture content of the stratum corneum and reduces transepidermal water loss, with effects significantly superior to commercially available products. This indicates that the composition of the present invention has excellent moisturizing and skin barrier repair effects.

[0069] The technical features of the above embodiments can be combined in any way. For the sake of brevity, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0070] The above embodiments merely illustrate several implementation methods of the present invention, and their descriptions are relatively specific and detailed, but they should not be construed as limiting the scope of the invention patent. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention, and these all fall within the protection scope of the present invention. Therefore, the protection scope of this invention patent should be determined by the appended claims.

Claims

1. A soothing composition made from sea buckthorn fruit, characterized in that, It is obtained through the following preparation method: (1) The fruit of the Chinese prickly pear, the wood of the mulberry tree and the magnolia bark were screened, dried and pulverized respectively, and then mixed to obtain a mixed powder; (2) Add antioxidants and enzyme inhibitors to the mixed powder, then add ethanol-ethyl acetate composite solvent for extraction, and collect the supernatant after filtration and centrifugation; (3) Collect the heavy components by two-stage molecular distillation; (4) Add the prickly pear fruit oil, stir to dissolve, and form a uniform oily system to obtain the prickly pear fruit soothing composition.

2. The soothing composition of *Prickly pear* fruit according to claim 1, characterized in that, In step (1), the prickly pear fruit is crushed to 40-60 mesh, the myrrh to 60-80 mesh, and the magnolia bark to 40-60 mesh, and then they are mixed evenly in a weight ratio of 5-10:1-5:1-3.

3. The soothing composition of *Prickly pear* fruit according to claim 1, characterized in that, The amount of antioxidant added in step (2) is 0.01-0.05% of the total weight of the mixed powder. The antioxidant is a mixture of vitamin E and ascorbate palmitate in a weight ratio of 1-5:1-5. The enzyme inhibitor is disodium EDTA, and the amount added is 0.01-0.1% of the total weight of the mixed powder.

4. The soothing composition of *Prickly pear* fruit according to claim 1, characterized in that, In step (2), the volume ratio of ethanol to ethyl acetate in the ethanol-ethyl acetate composite solvent is 1-3:1, the ratio of the mixed powder to the composite solvent is 1:10-15 g / mL, and nitrogen gas is introduced for protection throughout the extraction process.

5. The soothing composition of *Prickly pear* fruit according to claim 1, characterized in that, The extraction conditions described in step (2) are: constant temperature at 45℃, stirring at 80 r / min, combined with 200 W ultrasonic assisted extraction, intermittent ultrasonic 3 s / 3 s, and extraction time of 2.5 h.

6. The soothing composition of *Prickly pear* fruit according to claim 1, characterized in that, The filtration and centrifugation in step (2) are as follows: After the extraction is completed, filter the coarse filter residue with gauze, then centrifuge the filtrate at 4500 r / min for 20 min and collect the supernatant; add 1 / 3 of the original amount of compound solvent to the filter residue, repeat the extraction for 30 min, and combine the two supernatants.

7. The soothing composition of *Prickly pear* fruit according to claim 1, characterized in that, Before the secondary molecular distillation described in step (3), the combined supernatant is filtered through a 0.22 μm organic filter membrane.

8. The soothing composition of *Prickly pear* fruit according to claim 1 or 7, characterized in that, The specific parameters for the second-order molecular distillation described in step (3) are as follows: First-stage distillation: evaporation temperature 75-80℃, condensation temperature 20℃, vacuum degree 0.001 MPa, feed rate 2 mL / min, scraper rotation speed 200 r / min; Secondary distillation: evaporation temperature 110-115℃, condensation temperature 30℃, vacuum degree 0.0005 MPa, feed rate 1.5 mL / min, scraper rotation speed 250 r / min.

9. The use of the prickly pear fruit soothing composition according to any one of claims 1-8 in the preparation of cosmetics with soothing, repairing and moisturizing effects.

10. A soothing oil droplet essence, characterized in that, The components include the following components by mass percentage: Glycerin 3-10% 1,3-Propanediol 3-10% Carbomer 0.2-0.4% p-Hydroxyacetophenone 0.2-0.6% 1,2-Hexanediol 0.4-0.8% Sodium hydroxide 0.03-0.08% Olive (Olea Europaea) fruit oil 1-5% Cocoyl alcohol-caprylate / caprylate 3-8% Castor oil / IPDI copolymer 0.1-1% Caprylic / capric triglycerides 0.3-5% Prisepia utilis oil 1-5% 1-5% of the prickly pear fruit soothing composition according to any one of claims 1-8 Water balance; Preparation process: Water, glycerin, 1,3-propanediol, carbomer, p-hydroxyacetophenone, and 1,2-hexanediol were added to an emulsifying pot and heated to 85 degrees Celsius with slow stirring. The pot was then turned on to homogenize and disperse the mixture until it was completely dissolved. Sodium hydroxide was then added and stirred until homogeneous to obtain a dilute gel system. Coco-caprylate / capric acid ester, castor oil / IPDI copolymer, and caprylic / capric acid triglyceride were added to an oil phase pot and heated to dissolve with stirring. Olive (Olea europaea) fruit oil, PRINSEPIA UTILIS oil, and a soothing combination of prickly ash fruit were then added and stirred until homogeneous to obtain the oil phase. The emulsifying pot was turned on and stirred at medium speed. The temperature was lowered to 60 degrees Celsius, and the oil phase was slowly added to the emulsifying pot and stirred until homogeneous to obtain a soothing essence with a gel system of finely dispersed oil droplets.

Images