Acne-removing composition containing multiple plants and antibacterial allergy-relieving agent and preparation method of acne-removing composition
By combining plant extracts and antibacterial soothing agents in a specific ratio, using a three-stage evaporation process and ultrasonic treatment, nano-scale inclusions are formed, which solves the single mechanism problem of traditional acne-removing products, achieves multiple functions of efficient acne removal, anti-inflammatory and oil control, and improves product stability and transdermal absorption.
Patent Information
- Application Number
- CN202511024354.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-07-24
- Publication Date
- 2025-09-05
AI Technical Summary
Traditional acne treatment products mostly rely on a single ingredient or a single mechanism, which makes it difficult to achieve comprehensive treatment of acne. They may also lead to drug resistance or damage the skin barrier. In addition, fat-soluble antibacterial agents have poor dispersion stability in aqueous systems and low bioavailability.
A specific ratio of plant extracts such as Scutellaria root, Salvia miltiorrhiza root, and Phellodendron bark is combined with antibacterial and soothing agents such as cymene. Nano-scale inclusions are formed through a three-stage evaporation process and intermittent ultrasonic mode, combined with a compound of alcohol solvent and hydroxypropyl cyclodextrin to improve water dispersibility and transdermal penetration.
It achieves a triple synergistic effect, effectively eliminating pathogens, inhibiting inflammation and controlling oil, increasing acne removal efficiency by 50%, stability by 3.2 times, transdermal penetration by 2.8 times, and reducing skin irritation.
Smart Images

Figure CN120585703A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of cosmetics, in particular to an anti-acne composition containing multiple plants and antibacterial soothing agents and a preparation method thereof. Background Art
[0002] In the modern skincare landscape, the treatment of acne (commonly known as "pimples") has long been a focus of attention for consumers and researchers. The causes of acne are complex, involving multiple factors, including pathogenic microbial infection, inflammatory responses, and excessive sebaceous gland secretion. Traditional acne-removing products often target only one or two of these factors, making comprehensive and effective treatment difficult. Furthermore, many products contain irritating ingredients that can exacerbate skin sensitivity and even damage the skin barrier.
[0003] Traditional acne removal products mostly rely on a single ingredient or a single mechanism, such as antibiotics targeting pathogenic microorganisms and hormonal drugs suppressing inflammation. Although these methods can relieve acne symptoms to a certain extent, they do not completely eliminate pathogens. Although antibiotics can kill pathogenic microorganisms such as Propionibacterium acnes, long-term use may lead to drug resistance problems and cannot completely eliminate pathogens. Among them, although hormonal drugs can suppress inflammation, they may cause side effects such as skin atrophy and pigmentation, and have limited effects on non-inflammatory acne. At the same time, oil-control products on the market mostly rely on physical adsorption or chemical inhibition, which makes it difficult to regulate sebaceous gland secretion from the source. The effect is short-lived and may cause dry skin. Summary of the Invention
[0004] In response to the shortcomings of the existing technology, the present invention provides an acne-removing composition containing multiple plants and antibacterial and soothing agents and a preparation method thereof, which solves the problems that fat-soluble antibacterial agents have poor dispersion stability in aqueous systems, resulting in low bioavailability, a single plant active ingredient is difficult to simultaneously achieve the triple synergistic effects of antibacterial, anti-inflammatory and oil control, and traditional extraction processes cause large-scale degradation of heat-sensitive active ingredients.
[0005] To achieve the above objectives, the present invention is implemented through the following technical solutions: An acne-removing composition containing multiple plants and antibacterial and soothing agents, comprising the following components by weight percentage: Plant extract complex 30-50%, prepared by extracting and concentrating scutellaria root, Acorus calamus, Stephania tetrandra, Sophora flavescens root, Phellodendron amurense bark, Salix alba bark and Salvia miltiorrhiza root with 75% ethanol; 0.5-5% of an antibacterial and soothing agent, selected from at least one of cymene, pyrrolidine, bisabolol, and camellia seed oil; 22-35% alcohol solvent, composed of 2-5% isopentyl glycol and 20-30% butanediol; Hydroxypropyl cyclodextrin 0.5-2%; Tocopherol 0.1-0.2%; The balance is water, which makes up to 100%.
[0006] By adopting the above technical solution: the active ingredients are extracted through a three-stage evaporation process with a specific ratio of Scutellaria root: Salvia miltiorrhiza root: Phellodendron bark = 5:20:20, achieving triple synergy: berberine from Phellodendron bark inhibits bacteria, baicalin from Scutellaria root inhibits TNF-α inflammatory factors, and tanshinone ⅡA from Salvia miltiorrhiza root regulates sebaceous gland secretion; the three are extracted and concentrated with ethanol to maximize the retention of activity, and acne is cured from the dimensions of pathogen elimination, inflammation blocking, and oil control; through intermittent ultrasound mode combined with ice-water bath temperature control and gradient water addition method, fat-soluble antibacterial agents such as cymene form nano-scale inclusions, breaking through their water-solubility limitations; the combination of hydroxypropyl cyclodextrin and tocopherol forms a stable inclusion complex under the action of an ultrasonic power density of 50-80W / L, and the water dispersibility is increased by 3.2 times, expanding its application to multiple dosage forms such as aqueous solutions, emulsions, and creams.
[0007] Preferably, the raw material mass ratio of the plant extract complex is: Scutellaria root: Acorus calamus: Stephania tetrandra: Sophora flavescens root: Phellodendron amurense bark: Salix alba bark: Salvia miltiorrhiza root = (5-10): (5-10): (10-20): (10-20): (15-25): (15-25): (15-25).
[0008] Preferably, the antibacterial and soothing agent is composed of at least one of cymene 0.1-2%, pionin 0.1-1.5%, bisabolol 0.2-1%, and camellia seed oil 0.1-3%, and the total weight percentage of the selected components is 0.5-5%.
[0009] Preferably, a method for preparing an acne-removing composition containing multiple plants and an antibacterial soothing agent is used for the acne-removing composition containing multiple plants and an antibacterial soothing agent, the method comprising the following steps: S1. Preparation of plant extract complex: Weigh 5-10 g of Scutellaria root, 5-10 g of Acorus calamus, 10-20 g of Stephania tetrandra, 10-20 g of Sophora flavescens root, 15-25 g of Phellodendron amurense bark, 15-25 g of Salix alba bark, and 15-25 g of Salvia miltiorrhiza root, respectively; grind and pass through a 70-mesh sieve; add 8-12 times the total weight of the raw materials in 75% ethanol; soak at room temperature for 5-8 hours, filter, and collect the filtrate; and concentrate by rotary evaporation at 70-80°C for 30-60 minutes each time, repeat three times, and concentrate to 1 / 4-1 / 3 of the amount of ethanol added. S2. Functional component pretreatment: Mix 0.5-5% of an antibacterial desensitizer, 22-35% of an alcohol solvent, 0.5-2% of hydroxypropyl cyclodextrin, and 0.1-0.2% of tocopherol; heat to 60-70°C and stir to dissolve; place in an ice-water bath and ultrasonicate for 1-3 minutes; S3. Synthesis of composition: Take 30-50% of the filtrate obtained from S1 and mix it with the S2 solution; heat it in a water bath to 50-60°C and stir for 3-5 minutes; add water to 100%, place it in an ice water bath; ultrasonically treat it for 8-12 minutes; and stir it for 5-10 minutes to obtain the product.
[0010] Preferably, the rotary evaporation in S1 is carried out in three stages: the first stage is constant temperature evaporation at 65-70°C for 30 minutes, the second stage is constant temperature evaporation at 75-80°C for 40 minutes, and the third stage is constant temperature evaporation at 70-75°C for 50 minutes.
[0011] Preferably, the ultrasonic treatment in S3 adopts an intermittent mode: working for 2 seconds and then resting for 1 second in a cycle, and the power density of the ultrasonic treatment is 50-80 W / L.
[0012] Preferably, the amount of 75% ethanol added in S1 is 10 times the total dry weight of the raw materials.
[0013] Preferably, the temperature of the S2 dissolution process is controlled at 68±2°C; the ice water bath temperature is 0-5°C, the ice water bath treatment time does not exceed 5 minutes, and the ultrasonic frequency is 20-40kHz.
[0014] Preferably, the water bath heating in S3 adopts a constant temperature water bath, and the stirring rate is 200-400 rpm; the water adding process adopts a gradient water addition method: 60% of the total water is added for the first time, and the remaining water is added after stirring for 3 minutes.
[0015] Preferably, the rotary evaporation in S1 is performed under a vacuum condition of -0.098 MPa.
[0016] The present invention provides an anti-acne composition containing multiple plants and antibacterial and soothing agents and a preparation method thereof. It has the following beneficial effects: 1. In the present invention, the active ingredients of the specific ratio of Scutellaria root: Salvia miltiorrhiza root: Phellodendron bark = 5:20:20 are extracted through a three-stage evaporation process, achieving triple synergy: berberine from Phellodendron bark inhibits bacteria, baicalin from Scutellaria root inhibits TNF-α inflammatory factors, and tanshinone IIA from Salvia miltiorrhiza root regulates sebaceous gland secretion; the three are extracted and concentrated with ethanol to maximize their activity, thereby curing acne from the dimensions of pathogen elimination, inflammation blocking, and oil control.
[0017] 2. In the present invention, intermittent ultrasonic mode is combined with ice-water bath temperature control and gradient water addition method to form nano-scale inclusions of fat-soluble antibacterial agents such as cymene, breaking through their water solubility limitations; the combination of hydroxypropyl cyclodextrin and tocopherol forms a stable inclusion complex under the action of ultrasonic power density of 50-80W / L, and the water dispersibility is increased by 3.2 times, which can be expanded to multiple dosage forms such as aqueous solutions, emulsions, and creams.
[0018] 3. In the present invention, a compound solvent of 2-5% isopentyl glycol and 20-30% butylene glycol is combined with gradient water addition to significantly enhance the transdermal rate of plant active ingredients; hydroxypropyl cyclodextrin is dissolved at 68±2°C and under the action of intermittent ultrasound, synchronously encapsulating the antibacterial agent and the plant extract active ingredients, thereby increasing the drug concentration in the acne lesion site by 2.8 times and improving the acne removal efficiency by 50% compared with a single component.
[0019] 4. In the present invention, the three-stage temperature control and vacuum degree of rotary evaporation are -0.098Mpa, so that the retention rate of heat-sensitive components is greater than 95%; the amount of ethanol used is 10 times the dry weight of the raw material to ensure the adequacy of extraction, and the ice bath time is ≤5 minutes to inhibit the degradation of components; the final product has a uniform particle size distribution, which significantly improves the overall stability. BRIEF DESCRIPTION OF THE DRAWINGS
[0020] Figure 1 This is a flow chart of a method for preparing an acne-removing composition containing multiple plants and antibacterial soothing agents according to the present invention; Figure 2 Schematic diagram of the inhibition zone experiment of an acne-removing composition containing multiple plants and antibacterial soothing agents of the present invention; Figure 3 This is a schematic diagram of the volume of acne scars in the experimental group in the acne removal efficacy test of an acne removal composition containing multiple plants and antibacterial soothing agents of the present invention; Figure 4 This is a schematic diagram of the change in acne scar volume in the experimental group during the acne treatment efficacy test of an acne treatment composition containing multiple plants and antibacterial soothing agents according to the present invention; Figure 5 This is a schematic diagram of the acne scar volume of the control group in the acne removal efficacy test of an acne removal composition containing multiple plants and antibacterial soothing agents of the present invention; Figure 6 This is a schematic diagram of the change in acne scar volume of the control group in the acne removal efficacy test of an acne removal composition containing multiple plants and antibacterial soothing agents of the present invention; Figure 7 A schematic diagram showing the redness of acne marks in the experimental group during the anti-inflammatory efficacy test of an acne-removing composition containing multiple plants and antibacterial soothing agents of the present invention; Figure 8 This is a schematic diagram showing the changes in the average redness of acne scars in the experimental group during the anti-inflammatory efficacy test of an acne-removing composition containing multiple plants and antibacterial soothing agents of the present invention; Figure 9 This is a schematic diagram showing the redness of acne marks in the control group during the anti-inflammatory efficacy test of an acne-removing composition containing multiple plants and antibacterial soothing agents of the present invention; Figure 10 This is a schematic diagram showing the change in the average value of acne scar redness in the control group in the anti-inflammatory efficacy test of an acne-removing composition containing multiple plants and antibacterial soothing agents of the present invention; Figure 11This is a schematic diagram of the volume of acne scars in the acne treatment efficacy test of Comparative Example 2 of an acne treatment composition containing multiple plants and antibacterial soothing agents of the present invention; Figure 12 This is a schematic diagram of the change in acne scar volume during the acne treatment efficacy test of Comparative Example 2 of an acne treatment composition containing multiple plants and antibacterial soothing agents of the present invention; Figure 13 This is a schematic diagram of the redness of acne marks in the acne treatment efficacy test of Comparative Example 2 of an acne treatment composition containing multiple plants and antibacterial soothing agents of the present invention; Figure 14 This is a schematic diagram showing the change in the average value of acne scar redness in the acne treatment efficacy test of Comparative Example 2 of the acne treatment composition containing multiple plants and antibacterial soothing agents of the present invention; Figure 15 This is a schematic diagram of the volume of acne scars in the acne treatment efficacy test of Comparative Example 3 of an acne treatment composition containing multiple plants and antibacterial soothing agents of the present invention; Figure 16 This is a schematic diagram of the change in acne scar volume during the acne treatment efficacy test of Comparative Example 3 of the acne treatment composition containing multiple plants and antibacterial soothing agents of the present invention; Figure 17 This is a schematic diagram of the redness of acne marks in the acne treatment efficacy test of Comparative Example 3 of the acne treatment composition containing multiple plants and antibacterial soothing agents of the present invention; Figure 18 This is a schematic diagram showing the change in the average value of acne scar redness in the acne treatment efficacy test of Comparative Example 3 of the acne treatment composition containing multiple plants and antibacterial soothing agents of the present invention; Figure 19 This is a schematic diagram of the volume of acne scars in the acne treatment efficacy test of Comparative Example 4 of the acne treatment composition containing multiple plants and antibacterial soothing agents of the present invention; Figure 20 This is a schematic diagram of the change in acne scar volume during the acne treatment efficacy test of Comparative Example 4 of the acne treatment composition containing multiple plants and antibacterial soothing agents of the present invention; Figure 21 This is a schematic diagram of the redness of acne marks in the acne treatment efficacy test of Comparative Example 4 of the acne treatment composition containing multiple plants and antibacterial soothing agents of the present invention; Figure 22 This is a schematic diagram showing the change in the average value of acne scar redness in the acne treatment efficacy test of Comparative Example 4 of the present invention, an acne treatment composition containing multiple plants and antibacterial soothing agents; Figure 23 This is a schematic diagram of the volume of acne scars in the acne treatment efficacy test of Comparative Example 5 of the acne treatment composition containing multiple plants and antibacterial soothing agents of the present invention; Figure 24 This is a schematic diagram of the change in acne scar volume during the acne treatment efficacy test of Comparative Example 5 of the acne treatment composition containing multiple plants and antibacterial soothing agents of the present invention; Figure 25This is a schematic diagram of the redness of acne marks in the acne treatment efficacy test of Comparative Example 5 of the acne treatment composition containing multiple plants and antibacterial soothing agents of the present invention; Figure 26 This is a schematic diagram of the change in the average value of acne scar redness in the acne anti-efficacy test of Comparative Example 5 of the present invention, an acne anti-composition containing multiple plants and antibacterial soothing agents. DETAILED DESCRIPTION
[0021] The following will clearly and completely describe the technical solutions of the present invention in conjunction with the accompanying drawings. Obviously, the embodiments described are only some of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making any creative efforts are within the scope of protection of the present invention.
[0022] The present invention provides an anti-acne composition containing multiple plants and antibacterial soothing agents, which comprises the following components by weight percentage: Plant extract complex 30-50%, prepared by extracting and concentrating scutellaria root, Acorus calamus, Stephania tetrandra, Sophora flavescens root, Phellodendron amurense bark, Salix alba bark and Salvia miltiorrhiza root with 75% ethanol; 0.5-5% of an antibacterial and soothing agent, selected from at least one of cymene, pyrrolidine, bisabolol, and camellia seed oil; 22-35% alcohol solvent, composed of 2-5% isopentyl glycol and 20-30% butanediol; Hydroxypropyl cyclodextrin 0.5-2%; Tocopherol 0.1-0.2%; The balance is water, which makes up to 100%.
[0023] Specifically, the plant extract complex prepared by extracting and concentrating scutellaria root, calamus tatarinowii, stephania tetrandra, sophora flavescens root, phellodendron amurense bark, willow bark and salvia miltiorrhiza root with 75% ethanol has the effects of inhibiting Propionibacterium acnes, anti-inflammatory and oil control, thereby achieving the effect of removing acne and reducing skin oiliness; the antibacterial and soothing agent selected from cymene, pyrrolidone, bisabolol and camellia seed oil has the effects of antibacterial and soothing sensitive skin, thereby achieving the effect of reducing the occurrence of acne and reducing skin irritation; the alcohol solvent composed of 2-5% isopentyl glycol and 20-30% butylene glycol dissolves and stabilizes the antibacterial and soothing agent, thereby achieving the effect of improving product stability and expanding the scope of application; 0.5-2% hydroxypropyl cyclodextrin encapsulates and stabilizes the active ingredient, thereby achieving the effect of improving product stability and bioavailability; 0.1-0.2% tocopherol enhances product permeability and promotes the absorption of active ingredients, thereby achieving the effect of improving product efficacy and reducing skin irritation.
[0024] The raw material mass ratio of the plant extract complex is: scutellaria root: calamus tatarinowii: stephensi: sophora flavescens root: phellodendron amurense bark: willow bark: salix miltiorrhiza root = (5-10): (5-10): (10-20): (10-20): (15-25): (15-25): (15-25).
[0025] Specifically, Scutellaria baicalensis root extract contains active ingredients such as baicalin, which has significant anti-inflammatory and antioxidant effects. By inhibiting the release of inflammatory mediators, it can reduce skin redness and inflammation, thereby soothing acne-prone skin; Acorus tatarinowii extract contains ingredients such as volatile oil, which has antibacterial and anti-inflammatory activities. By inhibiting the growth of skin pathogens such as Propionibacterium acnes, it can prevent and treat acne, thereby cleansing the skin and reducing the occurrence of acne; Stephania tetrandra extract contains alkaloids such as tetrandrine, which has anti-inflammatory, analgesic and anti-allergic effects. By reducing skin inflammatory reactions and allergic symptoms, it can soothe sensitive skin and reduce skin irritation, thereby improving skin barrier function; Sophora flavescens root extract contains active ingredients such as matrine, which has significant antibacterial, anti-inflammatory and anti-allergic effects. By inhibiting the growth of skin pathogens such as Propionibacterium acnes, it can prevent and treat acne. effect, thereby reducing skin oil secretion and improving oily skin; Phellodendron amurense bark extract contains berberine and other alkaloid ingredients, which have antibacterial, anti-inflammatory and antioxidant effects. By inhibiting the release of inflammatory mediators and anti-oxidative stress, it can reduce skin redness and inflammation, thereby soothing acne-prone skin and improving skin barrier function; White willow bark extract contains salicin and other active ingredients, which have anti-inflammatory, exfoliating and skin renewal effects. By promoting the shedding of old keratinocytes and the generation of new cells, it can improve skin roughness and brighten the skin tone, thereby smoothing the skin and brightening the skin tone; Salvia miltiorrhiza root extract contains tanshinone and other active ingredients, which have anti-inflammatory, antioxidant and blood circulation promoting effects. By promoting skin blood circulation and inhibiting the release of inflammatory mediators, it can reduce skin redness and inflammation, thereby soothing acne-prone skin and improving skin microcirculation.
[0026] The antibacterial and soothing agent comprises at least one of cymene 0.1-2%, pionin 0.1-1.5%, bisabolol 0.2-1% and camellia seed oil 0.1-3%, and the total weight percentage of the selected components is 0.5-5%.
[0027] Specifically, cymene is an ingredient with natural antibacterial properties. It inhibits and kills pathogenic bacteria on the skin surface by destroying the cell membrane structure of bacteria, thereby reducing the occurrence of acne and preventing the deterioration of infection; Pioneer has antifungal and anti-inflammatory activities. By inhibiting fungal growth and reducing skin inflammatory reactions, it prevents and treats skin problems caused by fungi and relieves skin redness and swelling, thereby improving skin health and reducing skin discomfort; Bisabolol is an ingredient extracted from chamomile, which has anti-inflammatory and soothing effects on sensitive skin. By reducing skin inflammation and allergic symptoms, it relieves skin irritation and itching, thereby improving skin comfort and reducing skin redness and swelling; Camellia seed oil is rich in oil Acid and vitamin E have antibacterial and skin barrier repair functions. By nourishing the skin and providing antioxidant protection, they moisturize and promote skin healing, thereby improving dry skin and accelerating the recovery of damaged skin. The antibacterial soothing agent works through the action of at least one ingredient, among which the antibacterial activity of cymene and / or pyrrolidone effectively inhibits the growth of bacteria and fungi on the skin surface, reducing the occurrence of acne and other skin infections; through the anti-inflammatory properties of bisabolol, it reduces skin inflammation, relieves redness, swelling and pain; the soothing effect of bisabolol and camellia seed oil helps reduce skin irritation and allergy symptoms and improve skin comfort; the nourishing and repairing effect of camellia seed oil helps maintain and strengthen the skin barrier, reduce moisture loss, and keep the skin healthy.
[0028] Please see the attached Figure 1 A method for preparing an acne-removing composition containing multiple plants and an antibacterial soothing agent, for use in the above-mentioned acne-removing composition containing multiple plants and an antibacterial soothing agent, the method comprises the following steps: S1. Preparation of plant extract complex: Weigh 5-10 g of Scutellaria root, 5-10 g of Acorus calamus, 10-20 g of Stephania tetrandra, 10-20 g of Sophora flavescens root, 15-25 g of Phellodendron amurense bark, 15-25 g of Salix alba bark, and 15-25 g of Salvia miltiorrhiza root, respectively; grind and pass through a 70-mesh sieve; add 8-12 times the total weight of the raw materials in 75% ethanol; soak at room temperature for 5-8 hours, filter, and collect the filtrate; and concentrate by rotary evaporation at 70-80°C for 30-60 minutes each time, repeat three times, and concentrate to 1 / 4-1 / 3 of the amount of ethanol added. S2. Functional component pretreatment: Mix 0.5-5% of an antibacterial desensitizer, 22-35% of an alcohol solvent, 0.5-2% of hydroxypropyl cyclodextrin, and 0.1-0.2% of tocopherol; heat to 60-70°C and stir to dissolve; place in an ice-water bath and ultrasonicate for 1-3 minutes; S3. Synthesis of composition: Take 30-50% of the filtrate obtained from S1 and mix it with the S2 solution; heat it in a water bath to 50-60°C and stir for 3-5 minutes; add water to 100%, place it in an ice water bath; ultrasonically treat it for 8-12 minutes; and stir it for 5-10 minutes to obtain the product.
[0029] Specifically, by weighing specific proportions of Scutellaria root, Acorus tatarinowii, Stephania tetrandra, Sophora flavescens root, Phellodendron amurense bark, Salix babylonica bark, and Salvia miltiorrhiza root, and crushing them through a 70-mesh sieve, the effective ingredients in the plants are extracted, thereby providing natural anti-inflammatory and antibacterial activity for the acne-removing composition; 75% ethanol, which is 8-12 times the total weight of the raw materials, is added and soaked at room temperature for 5-8 hours to dissolve and extract the effective ingredients in the plant raw materials, thereby enhancing the efficacy of the acne-removing composition; after filtration, the filtrate is collected and concentrated by rotary evaporation at 70-80°C, each evaporation lasts 30-60 minutes, repeated three times, and concentrated to 1 / 4-1 / 3 of the amount of ethanol added, thereby reducing the amount of solvent and increasing the concentration of the effective ingredients, thereby making the acne-removing composition more efficient and stable; 0.5-5% of antibacterial soothing agent, 22-35% of alcohol solvent, 0.5-2% of hydroxypropyl cyclodextrin, and 0.1-0.2% of tocopherol are mixed and heated to 60-70°C and stirred. The mixture is stirred and dissolved to uniformly disperse and dissolve the components, thereby ensuring the uniformity and stability of the acne-removing composition; the mixture is ultrasonically treated in an ice-water bath for 1-3 minutes to further refine the dispersion system and improve the compatibility of the components, thereby enhancing the permeability and bioavailability of the acne-removing composition; 30-50% of the filtrate obtained in S1 is mixed with the S2 solution, and the mixture is heated in a water bath to 50-60°C and stirred for 3-5 minutes to effectively combine the plant extract with the functional components, thereby achieving a synergistic effect of removing acne and soothing the skin; after adding water to 100%, the mixture is ultrasonically treated in an ice-water bath for 8-12 minutes to further refine the dispersion system, improve the stability and bioavailability, thereby making the acne-removing composition more gentle and easy for the skin to absorb; the final acne-removing composition is obtained by stirring for 5-10 minutes, which ensures that the components are fully mixed and uniformly formed into a stable suspension, thereby improving the user experience and efficacy of the product.
[0030] Please see the attached Figure 1 ,The rotary evaporation in S1 was carried out in three stages: the first stage was evaporation at a constant temperature of 65-70°C for 30 minutes, the second stage was evaporation at a constant temperature of 75-80°C for 40 minutes, and the third stage was evaporation at a constant temperature of 70-75°C for 50 minutes.
[0031] Specifically, by performing preliminary evaporation at a relatively low temperature of 65-70°C, the ethanol solvent is gently removed, thereby avoiding the damage of heat-sensitive components in the plant extract caused by high temperature, thereby maintaining the integrity and biological activity of the active ingredients in the extract; on the basis of the first stage, the temperature is increased to 75-80°C for further evaporation, which accelerates the solvent removal and improves the concentration efficiency, while maximally retaining the effective ingredients in the extract within a controllable temperature range, thereby obtaining a high-concentration plant extract rich in active ingredients; after the second stage of high-efficiency concentration, the temperature is appropriately lowered to 70-75°C for the final stage of evaporation, which plays a role in finely controlling the extract concentration and ensuring the extract quality, while avoiding the deterioration or activity loss of the extract that may be caused by long-term high-temperature treatment, thereby obtaining a plant extract with good stability and high biological activity.
[0032] Please see the attached Figure 1 In S3, the ultrasonic treatment adopts an intermittent mode: working for 2 seconds and then resting for 1 second in a cycle operation, and the power density of the ultrasonic treatment is 50-80W / L.
[0033] Specifically, by cyclically operating for 2 seconds and then 1 second of rest, the excessive energy input is reduced while maintaining the ultrasonic treatment effect, thereby avoiding damage to sensitive ingredients, and thus protecting the active ingredients in the plant extracts and antibacterial soothing agents from being destroyed by high temperature or prolonged ultrasound; this intermittent mode helps to control the increase in local temperature, reduce the impact of heat generated by ultrasonic treatment on the stability of the ingredients, and thus maintain the overall stability and effectiveness of the acne-removing composition; the power density is set within the range of 50-80W / L, which can provide sufficient energy for effective dispersion and mixing, while avoiding decomposition or denaturation of ingredients caused by excessive energy input, thereby ensuring the uniform distribution and biological activity of the components in the acne-removing composition; appropriate power density helps to achieve a finer dispersed system, improve the solubility and bioavailability of the ingredients, and thus enhance the efficacy and transdermal absorption capacity of the acne-removing composition.
[0034] Please see the attached Figure 1 , the amount of 75% ethanol added to S1 is 10 times the total dry weight of the raw materials.
[0035] Specifically, by using 75% ethanol in an amount that is 10 times the total dry weight of the raw material, it is possible to ensure that the active ingredients in the plant raw material are fully extracted. As a good solvent, ethanol can effectively dissolve a variety of active ingredients in plants, such as flavonoids, phenolic compounds, etc., thereby increasing the concentration and biological activity of the active ingredients in the extract; a large amount of 75% ethanol can increase the contact area with the plant raw material, improve the extraction efficiency, and allow more active ingredients to be dissolved during the soaking process, thereby improving the quality of the extract; the high proportion of 75% ethanol helps to dissolve the fat-soluble and water-soluble components in the plant raw material, thereby making the extract contain a more comprehensive range of active ingredients, providing a more comprehensive therapeutic effect for the acne-removing composition; after using a large amount of 75% ethanol for extraction, although more time is required for rotary evaporation concentration, this also means that the final extract will have a higher concentration, which is convenient for subsequent concentration and preparation processes, thereby improving the stability and effect of the final product.
[0036] Please see the attached Figure 1 The temperature of the S2 dissolution process is controlled at 68±2°C; the ice water bath temperature is 0-5°C, the ice water bath treatment time does not exceed 5 minutes, and the ultrasonic frequency is 20-40kHz.
[0037] Specifically, by controlling the temperature at 68±2°C, it is possible to ensure that the functional components are fully dissolved at an appropriate temperature. This temperature range can not only ensure the solubility of the components, but also avoid the decomposition or inactivation of the components that may be caused by excessively high temperatures, thereby maintaining the stability and effectiveness of the acne-removing composition; placing the pretreated solution in an ice water bath at 0-5°C can quickly reduce the temperature of the solution and reduce the effect of heat on the stability of the components. At the same time, controlling the ice water bath treatment time to no more than 5 minutes can avoid the precipitation or precipitation of components that may be caused by low-temperature treatment for too long, thereby ensuring the uniformity and stability of the acne-removing composition; using an ultrasonic frequency of 20-40kHz for treatment can generate sufficient mechanical vibration and cavitation effects to promote the uniform dispersion and mixing of the functional components. Ultrasonic treatment helps to refine the dispersed system, improve the solubility and bioavailability of the components, and thereby enhance the efficacy and transdermal absorption capacity of the acne-removing composition.
[0038] Please see the attached Figure 1 , S3 water bath heating uses a constant temperature water bath, and the stirring rate is 200-400 rpm; the water adding process adopts a gradient water addition method: 60% of the total water volume is added for the first time, and the remaining water is added after stirring for 3 minutes.
[0039] Specifically, constant temperature water bath heating and appropriate stirring rate help to achieve sufficient mixing of the S1 filtrate and the S2 solution, thereby improving the uniformity and stability of the acne-removing composition; uniform temperature and mild stirring conditions help to protect the active ingredients in the acne-removing composition and avoid damage caused by overheating or vigorous stirring; the gradient water addition method helps to enhance the interaction between water molecules and active ingredients, improve solubility and bioavailability, and enhance the efficacy of the acne-removing composition.
[0040] Please see the attached Figure 1 , the rotary evaporation in S1 was carried out under a vacuum condition of -0.098 MPa.
[0041] Specifically, under vacuum conditions, the boiling point of the liquid will decrease, which means that evaporation can be carried out at a lower temperature, reducing thermal damage to heat-sensitive plant extract components, thereby maintaining the integrity and biological activity of the active ingredients in the extract; the vacuum environment can accelerate the evaporation rate of the solvent, improve the concentration efficiency, shorten the concentration time, and at the same time reduce the problem of extract quality degradation caused by long-term heating; vacuum rotary evaporation can reduce the oxidative effect of oxygen on the extract, reduce the risk of oxidative deterioration, and help maintain the color, aroma and stability of the active ingredients of the extract.
[0042] Example 1: 1. This embodiment provides a method for preparing an anti-acne composition containing multiple plants and antibacterial soothing agents, comprising the following steps: (1) Preparation of a plant extract complex: Raw material ratio: Scutellaria root 8g, Acorus calamus 8g, Stephania tetrandra 15g, Sophora flavescens root 15g, Phellodendron amurense bark 20g, Salix alba bark 20g, Salvia miltiorrhiza root 20g; Crushing and screening: after crushing, pass through 80 mesh sieve; Extraction process: Add 75% ethanol (10 times the total weight of the raw materials), 900g, and soak at room temperature for 6 hours; Concentration step: Rotary evaporation at 75°C and -0.098 MPa was performed in three stages: The first stage: constant temperature evaporation at 70℃ for 35 minutes; The second stage: constant temperature evaporation at 75℃ for 45 minutes; The third stage: constant temperature evaporation at 72°C for 55 minutes; The mixture was concentrated to 1 / 3 of the amount of ethanol added, and the final filtrate volume was 160 g.
[0043] (2) Pretreatment of functional components: Antibacterial and soothing agents: cymene 1.0%, pyridine 1.0%, bisabolol 0.8%, camellia seed oil 1.2%, total 4.0%; alcohol solvent: isopentyl glycol 3.0%, butanediol 25.0%; Other ingredients: Hydroxypropyl cyclodextrin 1.5%, tocopherol 0.15%; Dissolution process: Heat to 68°C and stir to dissolve, transfer to a 0-5°C ice water bath, and ultrasonicate at 30kHz for 2 minutes.
[0044] (III) Synthesis of composition: Mixing and heating: 40% of the filtrate was mixed with the pretreatment solution and stirred at 300 rpm in a 55°C water bath for 4 minutes; Gradient water replenishment: add 60% of the total water for the first time, stir for 3 minutes and add the remaining water to 100%; Ultrasonic treatment: Place in an ice water bath and sonicate for 10 minutes at 60W / L power, 2 seconds on / 1 second off mode; Final stirring: stirring at room temperature for 8 minutes to obtain the anti-acne composition.
[0045] 2. Antibacterial performance test: Inhibition zone method (please refer to the attached Figure 2 ) (1) Detection method: Bacterial species: Propionibacterium acnes (ATCC6919); step: Prepare modified GAM medium, 6 g / 100 mL water, sterilize at 121°C for 30 minutes; The bacterial suspension was adjusted to 1.5×10 8 CFU / mL; Take 100 μL of coating medium, punch wells and add the composition of Example 1, 20 μL / well; The cells were incubated anaerobically at 37°C for 72 h, and the diameter of the inhibition zone was measured.
[0046] (II) The judgment criteria are shown in Table 1: Table 1: (3) Results: Example 1: The diameter of the inhibition zone is 17.2±0.3 mm, and the effect level is high efficiency.
[0047] 3. Anti-inflammatory Efficacy Test: Antera3D Redness Area Analysis (I) Testing Method: Sample: 30 volunteers aged 18-25 years, with inflammatory acne around the lips of 3-5 mm in diameter; Grouping: Take 5 g of the composition of Example 1, stir and dissolve it with 95 g of purified water to obtain a test sample, and then apply it to the desired area.
[0048] step: Use Antera3D to take photos of the acne area at 0h / 24h / 48h; The reddening area change rate was analyzed and calculated using the formula: (initial area - current area) / initial area × 100%.
[0049] (II) The results are shown in Table 2: Table 2: time Redness reduction rate in the experimental group 24h 7.0%±0.9% 48h 14.8%±1.6% (III) Conclusion: After 48 hours, the redness area in the experimental group was significantly reduced, confirming that the composition can quickly relieve inflammation.
[0050] 4. Acne Treatment Efficacy Test: Antera3D Volume Analysis (I) Testing Method: Sample: Same batch of volunteers, same group of acne; step: Antera3D analyzes changes in acne volume; The volume change rate is calculated as follows: (initial volume - current volume) / initial volume × 100%.
[0051] (II) The results are shown in Table 3: Table 3: (III) Conclusion: After 48 hours, the volume of acne was significantly reduced by 18.1% (P<0.01), confirming that the composition can achieve high efficiency in acne removal through a triple synergistic mechanism (antibacterial, anti-inflammatory, and oil control).
[0052] Example 2: 1. This embodiment provides a method for preparing an anti-acne composition containing multiple plants and antibacterial soothing agents, comprising the following steps: (1) Preparation of a plant extract complex: Raw material ratio: Scutellaria root 5g, Acorus calamus 5g, Stephania tetrandra 10g, Sophora flavescens root 10g, Phellodendron amurense bark 15g, Salix alba bark 15g, Salvia miltiorrhiza root 15g; Crushing and screening: after crushing, pass through 70 mesh sieve; Extraction process: Add 75% ethanol (10 times the total weight of the raw materials), 900g, and soak at room temperature for 7 hours; Concentration step: Rotary evaporation at 75°C and -0.098 MPa was performed in three stages: The first stage: constant temperature evaporation at 68°C for 30 minutes; The second stage: constant temperature evaporation at 78°C for 40 minutes; The third stage: constant temperature evaporation at 72°C for 50 minutes; The mixture was concentrated to 1 / 3 of the amount of ethanol added, and the final filtrate volume was 160 g.
[0053] (2) Pretreatment of functional components: Antibacterial and soothing agents: cymene 1.2%, piornine 0.8%, bisabolol 0.5%, camellia seed oil 1.5%, total 4%; Alcohol solvent: isopentyl glycol 3%, butanediol 25%; Other ingredients: Hydroxypropyl cyclodextrin 1.2%, tocopherol 0.15%; Dissolution process: Heat to 65°C and stir to dissolve, transfer to a 0-5°C ice water bath, and ultrasonicate at 30kHz for 2 minutes.
[0054] (III) Synthesis of composition: Mixing and heating: 40% of the filtrate was mixed with the pretreatment solution and stirred at 300 rpm in a 55°C water bath for 4 minutes; Gradient water replenishment: add 60% of the total water for the first time, stir for 3 minutes and add the remaining water to 100%; Ultrasonic treatment: Place in an ice water bath and sonicate for 10 minutes at 60W / L power, 2 seconds on / 1 second off mode; Final stirring: stirring at room temperature for 8 minutes to obtain the anti-acne composition.
[0055] 2. Antibacterial performance test: Inhibition zone method (I) Test method: 1. Bacteria species: Propionibacterium acnes (ATCC6919); 2. Steps: Prepare modified GAM medium, 6 g / 100 mL water, sterilize at 121°C for 30 minutes; The bacterial suspension was adjusted to 1.5×10 8 CFU / mL; Take 100 μL of coating medium, punch wells and add the composition of Example 2, 20 μL / well; The cells were incubated anaerobically at 37°C for 72 h, and the diameter of the inhibition zone was measured.
[0056] (II) The judgment criteria are shown in Table 4: Table 4: Diameter of inhibition zone (mm) Effect Level <6 invalid 6~10 Inefficiency 10~14 Medium-effective >15 Efficient Results: Example 2: The diameter of the inhibition zone was 16.8±0.4 mm, and the effect level was highly effective.
[0057] 2. Anti-inflammatory Efficacy Test: Antera3D Redness Area Analysis (I) Testing Method: 1. Sample: 30 volunteers (18-25 years old) with inflammatory acne around the lips (3-5 mm in diameter); 2. Grouping: Take 5 g of the composition of Example 2, stir and dissolve it with 95 g of purified water to obtain a test sample, and then apply it to the desired area; 3. Steps: Use Antera3D to photograph the acne area at 0h / 24h / 48h; The reddening area change rate was analyzed and calculated using the formula: (initial area - current area) / initial area × 100%.
[0058] (II) The results are shown in Table 5: Table 5: time Example 2 group redness reduction rate 24h 6.2%±0.8% 48h 13.5%±1.7% III. Acne-Removal Efficacy Test: Antera3D Volume Analysis (I) Testing Method: The same group of volunteers and acne were analyzed by Antera3D for changes in acne volume; The volume change rate is calculated as follows: (initial volume - current volume) / initial volume × 100%.
[0059] (II) The results are shown in Table 6: Table 6: time Volume reduction rate of Example 2 group 24h 8.7%±0.9% 48h 16.1%±2.1% Example 3 1. This embodiment provides a method for preparing an anti-acne composition containing multiple plants and antibacterial soothing agents, comprising the following steps: (1) Preparation of a plant extract complex: Raw material ratio: Scutellaria root 10g, Acorus calamus 10g, Stephania tetrandra 20g, Sophora flavescens root 20g, Phellodendron amurense bark 25g, Salix alba bark 25g, Salvia miltiorrhiza root 25g; Crushing and screening: after crushing, pass through a 40-mesh sieve; Extraction process: Add 75% ethanol (8 times the total weight of the raw materials, 720g) and soak at room temperature for 5 hours; Concentration step: Rotary evaporation at 70°C and -0.098 MPa was performed in three stages: The first stage: constant temperature evaporation at 65℃ for 30 minutes; The second stage: constant temperature evaporation at 75℃ for 40 minutes; The third stage: constant temperature evaporation at 70℃ for 50 minutes; The mixture was concentrated to 1 / 4 of the amount of ethanol added, and the final filtrate volume was 180 g.
[0060] (2) Pretreatment of functional components: Antibacterial and soothing agents: cymene 0.5%, pyridine 0.5%, bisabolol 0.3%, camellia seed oil 0.2%, total amount 1.5%.
[0061] Alcohol solvent: isopentyl glycol 2.0%, butanediol 20.0%; Other ingredients: Hydroxypropyl cyclodextrin 0.5%, tocopherol 0.1%; Dissolution process: Heat to 65°C and stir to dissolve, transfer to a 0-5°C ice water bath, and ultrasonicate at 20 kHz for 1 minute.
[0062] (III) Synthesis of composition: Mixing and heating: 30% of the filtrate was mixed with the pretreatment solution and stirred at 200 rpm in a 50°C water bath for 3 minutes; Gradient water replenishment: add 60% of the total water for the first time, stir for 3 minutes and add the remaining water to 100%; Ultrasonic treatment: Place in an ice water bath and sonicate for 8 minutes at 50 W / L power, 2 seconds on / 1 second off mode; Final stirring: Stir at room temperature for 5 minutes to obtain the acne-removing composition.
[0063] 2. Antibacterial performance test: Inhibition zone method (I) Test method: Species: Propionibacterium acnes (ATCC6919) step: Prepare modified GAM medium, 6 g / 100 mL water, sterilize at 121°C for 30 minutes; The bacterial suspension was adjusted to 1.5×10 8 CFU / mL; Take 100 μL of coating medium, punch wells and add the composition of Example 3, 20 μL / well; The cells were incubated anaerobically at 37°C for 72 h, and the diameter of the inhibition zone was measured.
[0064] (II) The judgment criteria are shown in Table 7: Table 7: Diameter of inhibition zone (mm) Effect Level <6 invalid 6~10 Inefficiency 10~14 Medium-effective >15 Efficient (3) Results: Example 3: The diameter of the inhibition zone is 15.5±0.2 mm, and the effect level is high efficiency; 3. Anti-inflammatory Efficacy Test: Antera3D Redness Area Analysis (I) Testing Method: Sample: 30 volunteers aged 18-25 years with inflammatory acne around the lips with a diameter of 3-5 mm. Grouping: Take 5 g of the composition of Example 3, stir and dissolve it with 95 g of purified water to obtain a test sample, and then apply it to the desired area; step: Use Antera3D to take photos of the acne area at 0h / 24h / 48h; The reddening area change rate was analyzed and calculated using the formula: (initial area - current area) / initial area × 100%.
[0065] (II) The results are shown in Table 8: Table 8: time Redness reduction rate in the experimental group 24h 5.5%±0.7% 48h 12.3%±1.5% (III) Conclusion: After 48 hours, the redness area in the experimental group was significantly reduced, confirming that the composition can quickly relieve inflammation.
[0066] 4. Acne Treatment Efficacy Test: Antera3D Volume Analysis (I) Testing Method: Sample: Same batch of volunteers, same group of acne; step: Antera3D analyzes changes in acne volume; The volume change rate is calculated as follows: (initial volume - current volume) / initial volume × 100%.
[0067] (II) The results are shown in Table 9: Table 9: time Volume reduction rate of the experimental group 24h 7.8%±0.8% 48h 16.7%±2.0% (III) Conclusion: After 48 hours, the volume of acne was significantly reduced by 16.7%, confirming that the composition can achieve high efficiency in acne removal through a triple synergistic mechanism (antibacterial, anti-inflammatory, and oil control).
[0068] The comparison of efficacy data of Examples 1, 2, and 3 is shown in Table 10: Table 10: Summary: This comparison confirms that Example 1 is significantly superior to Example 2 and Example 3 in terms of antibacterial, anti-inflammatory, and acne-removing effects, and is the optimal implementation scheme.
[0069] Comparative Example 1 This comparative example provides a method for preparing an acne-removing composition containing multiple plants and an antibacterial soothing agent, comprising the following steps: (1) The root of Scutellaria baicalensis was replaced with the root of Paeonia lactiflora, 5 g, and the other plant materials remained unchanged, as in Example 1; (2) Preparation process: 1. Preparation of plant extract complex: Weigh 5g of peony root, 5g of Acorus calamus, 15g of Stephania tetrandra, 15g of Sophora flavescens root, 20g of Phellodendron amurense bark, 20g of Salix alba bark, and 20g of Salvia miltiorrhiza root.
[0070] Grind through 70 mesh sieve.
[0071] Add 75% ethanol (900 g) which is 10 times the total weight of the raw materials and soak at room temperature for 7 hours.
[0072] After filtration, the residue was extracted repeatedly once and the filtrates were combined.
[0073] The mixture was rotary evaporated at 75°C and -0.098 MPa: first stage 68°C / 30 min, second stage 78°C / 40 min, third stage 72°C / 50 min, and concentrated to 160 g of filtrate.
[0074] 2. Functional component pretreatment: Mix 1.2% of cymene, 0.8% of pyridine, 0.5% of bisabolol and 1.5% of camellia seed oil to a total amount of 4%.
[0075] Isopentyl glycol 3%, butylene glycol 25%, hydroxypropyl cyclodextrin 1.2%, and tocopherol 0.15% were added.
[0076] Heat to 65°C, stir and dissolve, transfer to a 0-5°C ice-water bath, and sonicate at 30 kHz for 2 minutes.
[0077] 3. Synthesis of composition: Take 40% of the above filtrate and mix it with the pretreatment solution.
[0078] The mixture was stirred at 300 rpm in a 55°C water bath for 4 minutes.
[0079] Gradient water replenishment: add 60% of the total water for the first time, stir for 3 minutes and add the remaining water to 100%.
[0080] Transfer to an ice water bath and sonicate for 10 minutes at a power of 60 W / L and a working time of 2 seconds and a rest time of 1 second.
[0081] The mixture was stirred at room temperature for 8 minutes to obtain an acne-removing composition.
[0082] Ⅰ. Processing steps of the anti-acne composition: 1. Phase A treatment: Add all ingredients of Phase A to a beaker, including water, natto gum, 1,3-propylene glycol, p-hydroxyacetophenone, and ammonium acryloyldimethyltaurate / VP copolymer; Heat to 80±2℃, homogenize at 8000rpm for 4 minutes, within the range of 3-5min, and keep warm for 10 minutes to allow the colloid to fully swell.
[0083] 2. Cooling control: Remove the beaker from the heat source and cool it down to 45±1°C with a water bath while stirring at 300 rpm.
[0084] 3. Addition of phase B: The anti-acne composition of Example 1 and 1,2-hexanediol were added in sequence and mixed evenly; Slowly add phase A into the beaker at a flow rate of ≤5g / s, and immediately stir at 500rpm for 5 minutes until the system becomes homogeneous and transparent.
[0085] 4. Filling and storage: Filter through a 200-mesh sieve while hot, let stand at room temperature to defoam, and fill into a light-proof container; Storage conditions: Store in a cool place below 25°C, avoid freezing.
[0086] 5. The formula is shown in Table 11: Table 11: Notes: Mixing order: The anti-acne composition must be added last to avoid direct contact with preservatives and inactivation; after adding the anti-acne composition and stirring evenly, add 1,2-hexanediol.
[0087] II. Containing the composition of Comparative Example 1, the formula is the same as that of Example 1, except that the active ingredient is replaced by the acne-removing composition of Comparative Example 1.
[0088] The formula is shown in Table 12: Table 12: (III) Experimental data: (Please refer to the attached Figure 2 ) 1. Antibacterial performance test: Inhibition zone diameter: 12.5±0.3mm.
[0089] Effect level: medium.
[0090] Compared with Example 1: significantly lower than Example 1.
[0091] 2. Anti-inflammatory efficacy testing (1) Efficacy test: 1. Test efficacy: anti-inflammatory.
[0092] 2. Instrument model: Miravex Antera 3D.
[0093] 3. Test method: 3.1 Subject Screening Number of participants: 30 healthy volunteers; Location: Inflammatory acne around the lips (2-4mm in diameter, obvious redness and swelling); 3.2 Grouping: Experimental group: Apply the serum of Example 1 to the left acne; Control group: Apply control serum to the right pimple.
[0094] A. Use Antera3D multifunctional 3D skin imager to photograph the skin around the lips of the subjects, and select two growing pimples as the experimental group and control group respectively.
[0095] B. After the shooting is completed, the experimental sample (anti-acne soothing essence (Example 1)) and the control sample (anti-acne soothing essence (Comparative Example 1)) are applied to the acne skin surface of the experimental group and the control group respectively (once in the morning and once in the evening every day), and then the Antera3D multi-functional 3D skin imager is used to take pictures once a day (i.e., day 0, day 1, and day 2). After the three pictures are taken, the results before and after application of the test area around the lips of the experimenter are analyzed and compared to obtain the results.
[0096] C. The anti-inflammatory effect of this experiment is mainly judged by visual observation and machine testing. Visual observation determines the anti-inflammatory effect by determining whether there is any change in the color of the acne, and machine testing determines the anti-inflammatory effect by measuring the redness of the acne.
[0097] (2) Test results: (Please refer to the attached Figure 7 -Attached Figure 10 ) A. Naked eye: Apply the experimental sample and the control sample to the acne on the skin around the lips of the experimenter. After the second shoot, the redness was not much different from the original skin.
[0098] B. Machine test: After the experimental group applied the experimental sample to the pimples for three times and took photos, the redness of the pimples decreased by 11.84% compared with the initial value, and the range of redness was reduced, which showed a significant anti-inflammatory effect. After the control group applied the control sample to the pimples for three times and took photos, the redness of the pimples increased by 9.04% compared with the initial value, which showed no anti-inflammatory effect.
[0099] 1. Quantitative data (Antera3D) are shown in Table 13: Table 13: Group 48h redness reduction rate Δa* value change Significance (P value) Experimental group 11.84% -3.42±0.51 <0.01 control group +9.04% +2.73±0.63 - Note: Δa* value indicates color change: positive value indicates aggravation of inflammation, negative value indicates resolution.
[0100] 2. Visual observation is shown in Table 14: Table 14: Group 0h status 48h status Experimental group Deep red spots Light pink, 50% smaller control group Deep red spots Fuchsia, 30% wider range (3) Experimental summary: The machine test results show that after applying the experimental sample to the pimples in the experimental group for three times, the redness of the pimples decreased, indicating a significant anti-inflammatory effect. However, after applying the control sample to the pimples in the control group for three times, the redness increased instead of decreasing, indicating that the control sample failed to suppress inflammation and had a poor anti-inflammatory effect.
[0101] In summary: The above experimental results show that the product (Anti-Acne Soothing Essence (Example 1)) has excellent anti-inflammatory effects.
[0102] 3. Acne removal efficacy test (I) Efficacy test: 1. Test efficacy: anti-acne.
[0103] 2. Instrument model: Miravex Antera 3D.
[0104] 3. Test method: 3.1 Subject Screening Number of participants: 30 healthy volunteers (18-35 years old); Location: Inflammatory acne around the lips (2-4mm in diameter, containing pus heads); 3.2 Grouping: Experimental group: Apply the serum of Example 1 to the left acne; Control group: Apply control serum to the right pimple.
[0105] A. Use Antera3D multifunctional 3D skin imager to photograph the skin around the lips of the subjects, and select two growing pimples as the experimental group and control group respectively.
[0106] B. After the shooting is completed, the experimental sample (anti-acne soothing essence (Example 1)) and the control sample (anti-acne soothing essence (Comparative Example 1)) are applied to the acne skin surface of the experimental group and the control group respectively (once in the morning and once in the evening every day), and then the Antera3D multi-functional 3D skin imager is used to take pictures once a day (i.e., day 0, day 1, and day 2). After the three pictures are taken, the results before and after application of the test area around the lips of the experimenter are analyzed and compared to obtain the results.
[0107] C. The acne removal effect of this experiment is mainly judged by naked eye observation and machine testing. Naked eye observation determines the acne removal effect by determining whether there is any change in the size of the acne, and machine testing determines the acne removal effect by measuring the change in the volume of the acne.
[0108] 2. Test results: (Please refer to the attached Figure 3 -Attached Figure 6 ) Reference standard: ISO24442:2011 "Test method for clinical anti-acne efficacy of cosmetics".
[0109] A. Naked eyes: After applying the experimental and control samples to acne spots around the subject's lips, the subjects were photographed three times. Visual observation revealed that the experimental group's acne was slightly smaller than the original, while the control group's acne had no significant change in size compared to the original.
[0110] B. Machine test: After three shots of the experimental group's acne with the experimental sample, the volume of the acne decreased by 15.73% compared with the initial value, which was a significant decrease; after three shots of the control group's acne with the control sample, the volume of the acne increased by 11.81% compared with the initial value.
[0111] 1. Quantitative data (Antera3D) are shown in Table 15: Table 15: Group 48h volume reduction rate Changes in the major / minor diameter ratio Significance (P value) Experimental group 15.73% 1.8 reduced to 1.2 <0.001 control group -11.81% 1.7 to 2.3 - Note: Negative values indicate increased volume 2. The results of visual observation are shown in Table 16: Table 16: Group 48h status Size changes Symptom improvement Experimental group The pimples are dry and the pus heads disappear Significantly reduced (down 2 levels) Redness and swelling subsided, no tenderness control group Abscess enlarges and oozes Basically unchanged (±0 level) Increased redness and swelling, and obvious tenderness 3. Experimental Summary: Visual observation and machine testing revealed that after three exposures, the experimental group, treated with the experimental sample, showed a decrease in both size and volume, indicating that the experimental sample inhibited acne growth and was effective in removing acne. However, after three exposures, the control group, treated with the control sample, showed no significant change in size, while its volume increased, indicating that the control sample failed to inhibit acne growth and was ineffective in removing acne.
[0112] In summary: The above experimental results show that the product (Anti-Acne Soothing Essence (Example 1)) has an excellent acne-removing effect.
[0113] Comparative Example 2: This comparative example provides a method for preparing an acne-removing composition containing multiple plants and an antibacterial soothing agent, comprising the following steps: (1) Salvia miltiorrhiza root was replaced with 20 g of Pueraria lobata root, and the other plant materials remained unchanged, as in Example 1.
[0114] (2) Preparation process: 1. Preparation of plant extract complex: Weigh 5g of Scutellaria root, 5g of Acorus gramineus, 15g of Stephania tetrandra, 15g of Sophora flavescens root, 20g of Phellodendron amurense bark, 20g of Salix alba bark, and 20g of Pueraria root.
[0115] Grind through 70 mesh sieve.
[0116] Add 900 g of 75% ethanol, which is 10 times the total weight of the raw materials, and soak at room temperature for 7 hours.
[0117] After filtration, the residue was extracted repeatedly once and the filtrates were combined.
[0118] The mixture was rotary evaporated at 75°C and -0.098 MPa: first stage 68°C / 30 min, second stage 78°C / 40 min, third stage 72°C / 50 min, and concentrated to 160 g of filtrate.
[0119] 2. Functional component pretreatment: Mix 1.2% of cymene, 0.8% of pyridine, 0.5% of bisabolol and 1.5% of camellia seed oil to a total amount of 4%.
[0120] Isopentyl glycol 3%, butylene glycol 25%, hydroxypropyl cyclodextrin 1.2%, and tocopherol 0.15% were added.
[0121] Heat to 65°C, stir and dissolve, transfer to a 0-5°C ice-water bath, and sonicate at 30 kHz for 2 minutes.
[0122] 3. Synthesis of composition: Take 40% of the above filtrate and mix it with the pretreatment solution.
[0123] The mixture was stirred at 300 rpm in a 55°C water bath for 4 minutes.
[0124] Gradient water replenishment: add 60% of the total water for the first time, stir for 3 minutes and add the remaining water to 100%.
[0125] Transfer to an ice water bath and sonicate for 10 minutes at a power of 60 W / L and a working time of 2 seconds and a rest time of 1 second.
[0126] The mixture was stirred at room temperature for 8 minutes to obtain an acne-removing composition.
[0127] (3) Experimental data: Antibacterial performance test: Inhibition zone diameter: 11.8±0.4mm.
[0128] Effect level: medium.
[0129] Compared with Example 1: significantly lower than Example 1.
[0130] Anti-inflammatory efficacy test: Redness reduction rate after 48 hours: -12.20%.
[0131] Compared with Example 1: significantly lower than Example 1.
[0132] Acne-removing efficacy test: Volume reduction rate after 48h: -12.1%.
[0133] Compared with Example 1: significantly lower than Example 1.
[0134] (IV) Conclusion Substitution of salvia root resulted in decreased oil control and anti-acne effects, confirming its key role in the formulation.
[0135] Comparative Example 3: This comparative example provides a method for preparing an acne-removing composition containing multiple plants and an antibacterial soothing agent, comprising the following steps: (1) The bark of Phellodendron amurense was replaced with 20 g of olive leaves, and the other plant materials remained unchanged, as in Example 1.
[0136] (2) Preparation process: 1. Preparation of plant extract complex: Weigh 5g of Scutellaria root, 5g of Acorus calamus, 15g of Stephania tetrandra, 15g of Sophora flavescens root, 20g of Olea europaea leaf, 20g of Salix alba bark, and 20g of Salvia miltiorrhiza root.
[0137] Grind through 70 mesh sieve.
[0138] Add 900 g of 75% ethanol, which is 10 times the total weight of the raw materials, and soak at room temperature for 7 hours.
[0139] After filtration, the residue was extracted repeatedly once and the filtrates were combined.
[0140] The mixture was rotary evaporated at 75°C and -0.098 MPa: first stage 68°C / 30 min, second stage 78°C / 40 min, third stage 72°C / 50 min, and concentrated to 160 g of filtrate.
[0141] 2. Functional component pretreatment: Mix 1.2% of cymene, 0.8% of pyridine, 0.5% of bisabolol and 1.5% of camellia seed oil to a total amount of 4%.
[0142] Isopentyl glycol 3%, butylene glycol 25%, hydroxypropyl cyclodextrin 1.2%, and tocopherol 0.15% were added.
[0143] Heat to 65°C, stir and dissolve, transfer to a 0-5°C ice-water bath, and sonicate at 30 kHz for 2 minutes.
[0144] 3. Synthesis of composition: Take 40% of the above filtrate and mix it with the pretreatment solution.
[0145] The mixture was stirred at 300 rpm in a 55°C water bath for 4 minutes.
[0146] Gradient water replenishment: add 60% of the total water for the first time, stir for 3 minutes and add the remaining water to 100%.
[0147] Transfer to an ice water bath and sonicate for 10 minutes at a power of 60 W / L and a working time of 2 seconds and a rest time of 1 second.
[0148] The mixture was stirred at room temperature for 8 minutes to obtain an acne-removing composition.
[0149] (3) Experimental data: 1. Antibacterial performance test: Inhibition zone diameter: 10.2±0.3mm.
[0150] Effect level: medium.
[0151] Compared with Example 1: significantly lower than Example 1.
[0152] 2. Anti-inflammatory efficacy test: Redness reduction rate after 48 hours: -19.63%.
[0153] Compared with Example 1: significantly lower than Example 1.
[0154] 3. Anti-acne efficacy test: Volume reduction rate after 48 hours: -108.76%.
[0155] Compared with Example 1: significantly lower than Example 1.
[0156] (IV) Conclusion Substitution of Phellodendron amurense bark significantly reduced the antibacterial and anti-acne effects, confirming its central role in the formula.
[0157] Comparative Example 4: This comparative example provides a method for preparing an acne-removing composition containing multiple plants and an antibacterial soothing agent, comprising the following steps: (1) Isopentyl glycol was replaced by 2% glycerol, and the other solvents remained unchanged, as in Example 1.
[0158] (2) Preparation process: 1. Preparation of plant extract complex: Scutellaria root 8g, Acorus gramineus 8g, Stephania tetrandra 15g, Sophora flavescens root 15g, Phellodendron amurense bark 20g, Salix alba bark 20g, Salvia miltiorrhiza root 20g.
[0159] Grind through 70 mesh sieve.
[0160] Add 900 g of 75% ethanol, which is 10 times the total weight of the raw materials, and soak at room temperature for 7 hours.
[0161] After filtration, the residue was extracted repeatedly once and the filtrates were combined.
[0162] The mixture was rotary evaporated at 75°C and -0.098 MPa: first stage 68°C / 30 min, second stage 78°C / 40 min, third stage 72°C / 50 min, and concentrated to 160 g of filtrate.
[0163] 2. Functional component pretreatment: Mix 1.2% of cymene, 0.8% of pyridine, 0.5% of bisabolol and 1.5% of camellia seed oil to a total amount of 4%.
[0164] Add 2% glycerol, 25% butylene glycol, 1.2% hydroxypropyl cyclodextrin, and 0.15% tocopherol.
[0165] Heat to 65°C, stir and dissolve, transfer to a 0-5°C ice-water bath, and sonicate at 30 kHz for 2 minutes.
[0166] 3. Synthesis of composition: Take 40% of the above filtrate and mix it with the pretreatment solution.
[0167] The mixture was stirred at 300 rpm in a 55°C water bath for 4 minutes.
[0168] Gradient water replenishment: add 60% of the total water for the first time, stir for 3 minutes and add the remaining water to 100%.
[0169] Transfer to an ice water bath and sonicate for 10 minutes at a power of 60 W / L and a working time of 2 seconds and a rest time of 1 second.
[0170] The mixture was stirred at room temperature for 8 minutes to obtain an acne-removing composition.
[0171] (3) Experimental data: 1. Antibacterial performance test: Inhibition zone diameter: 11.3±0.4mm.
[0172] Effect level: medium.
[0173] Compared with Example 1: significantly lower than Example 1.
[0174] 2. Anti-inflammatory efficacy test: Redness reduction rate after 48 hours: -18.72%.
[0175] Compared with Example 1: significantly lower than Example 1.
[0176] 3. Acne removal efficacy test: Volume reduction rate after 48 hours: -23.75%.
[0177] Compared with Example 1: significantly lower than Example 1.
[0178] (IV) Conclusion Substitution of isoprene glycol resulted in a decrease in overall efficacy, confirming its important role in the formulation.
[0179] Comparative Example 5: This comparative example provides a method for preparing an acne-removing composition containing multiple plants and an antibacterial soothing agent, comprising the following steps: (1) Tocopherol was replaced by 0.1% hydrogenated lecithin, and the other solvents remained unchanged, as in Example 1.
[0180] (2) Preparation process: 1. Preparation of plant extract complex: Scutellaria root 8g, Acorus gramineus 8g, Stephania tetrandra 15g, Sophora flavescens root 15g, Phellodendron amurense bark 20g, Salix alba bark 20g, Salvia miltiorrhiza root 20g.
[0181] Grind through 70 mesh sieve.
[0182] Add 900 g of 75% ethanol, which is 10 times the total weight of the raw materials, and soak at room temperature for 7 hours.
[0183] After filtration, the residue was extracted repeatedly once and the filtrates were combined.
[0184] The mixture was rotary evaporated at 75°C and -0.098 MPa: first stage 68°C / 30 min, second stage 78°C / 40 min, third stage 72°C / 50 min, and concentrated to 160 g of filtrate.
[0185] 2. Functional component pretreatment: Mix 1.2% of cymene, 0.8% of pyridine, 0.5% of bisabolol and 1.5% of camellia seed oil to a total amount of 4%.
[0186] Add 3% isopentyl glycol, 25% butylene glycol, 1.2% hydroxypropyl cyclodextrin, and 0.1% hydrogenated lecithin.
[0187] Heat to 65°C, stir and dissolve, transfer to a 0-5°C ice-water bath, and sonicate at 30 kHz for 2 minutes.
[0188] 3. Synthesis of composition: Take 40% of the above filtrate and mix it with the pretreatment solution.
[0189] The mixture was stirred at 300 rpm in a 55°C water bath for 4 minutes.
[0190] Gradient water replenishment: add 60% of the total water for the first time, stir for 3 minutes and add the remaining water to 100%.
[0191] Transfer to an ice water bath and sonicate for 10 minutes at a power of 60 W / L and a working time of 2 seconds and a rest time of 1 second.
[0192] The mixture was stirred at room temperature for 8 minutes to obtain an acne-removing composition.
[0193] (3) Experimental data: 1. Antibacterial performance test: Inhibition zone diameter: 10.8±0.3mm.
[0194] Effect level: medium.
[0195] Compared with Example 1: significantly lower than Example 1.
[0196] 2. Anti-inflammatory efficacy test: Redness reduction rate after 48 hours: -27.90%.
[0197] Compared with Example 1: significantly lower than Example 1.
[0198] 3. Anti-acne efficacy test: Volume reduction rate after 48 hours: -139.70%.
[0199] Compared with Example 1: significantly lower than Example 1.
[0200] (IV) Conclusion Substitution of tocosolan significantly reduced the anti-inflammatory and anti-acne effects, confirming its necessity in the formulation.
[0201] The experimental data comparison table of Comparative Examples 1-5 is shown in Table 17: Table 17: Summary: By comparing the experimental data of Examples 1-5, the comprehensive optimality of Example 1 in the three dimensions of antibacterial, anti-inflammatory and acne treatment was further verified, providing an important reference basis for formula development.
[0202] Note: In all efficacy test results, positive values (+) represent symptom improvement, such as reduced redness area and volume; negative values (-) represent symptom worsening, such as increased redness and volume.
[0203] While embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions, and variations may be made to these embodiments without departing from the principles and spirit of the invention, and that the scope of the invention is defined by the appended claims and their equivalents.
Claims
1. An anti-acne composition containing multiple plants and antibacterial soothing agents, characterized in that: The following components are included by weight percentage: Plant extract complex 30-50%, made by extracting and concentrating Scutellaria root, Acorus calamus, Stephania tetrandra, Sophora flavescens root, Phellodendron amurense bark, Salix alba bark and Salvia miltiorrhiza root with 75% ethanol; 0.5-5% antibacterial and soothing agent, at least one selected from cymene, pyrrolidone, bisabolol, and camellia seed oil; 22-35% alcohol solvent, composed of 2-5% isopentyl glycol and 20-30% butanediol; Hydroxypropyl cyclodextrin 0.5-2%; Tocosolan 0.1-0.2%; The balance is water, which makes up to 100%.
2. The acne-removing composition containing multiple plants and antibacterial soothing agents according to claim 1, characterized in that: The raw material mass ratio of the plant extract complex is: scutellaria root: calamus tatarinowii: stephensi: sophora flavescens root: phellodendron amurense bark: willow bark: salix miltiorrhiza root = (5-10): (5-10): (10-20): (10-20): (15-25): (15-25): (15-25).
3. The acne-removing composition containing multiple plants and antibacterial soothing agents according to claim 1, characterized in that: The antibacterial and soothing agent comprises at least one of cymene 0.1-2%, pionin 0.1-1.5%, bisabolol 0.2-1%, and camellia seed oil 0.1-3%, and the total weight percentage of the selected components is 0.5-5%.
4. A method for preparing an anti-acne composition containing multiple plants and antibacterial soothing agents, characterized in that: The acne-removing composition containing multiple plants and antibacterial soothing agents according to any one of claims 1 to 3, wherein the method comprises the following steps: S1. Preparation of plant extract complex: Weigh 5-10 g of Scutellaria root, 5-10 g of Acorus calamus, 10-20 g of Stephania tetrandra, 10-20 g of Sophora flavescens root, 15-25 g of Phellodendron amurense bark, 15-25 g of Salix alba bark, and 15-25 g of Salvia miltiorrhiza root respectively; grind and pass through a 70-mesh sieve; add 8-12 times the total weight of the raw materials in 75% ethanol; soak at room temperature for 5-8 hours, filter, and collect the filtrate; and concentrate by rotary evaporation at 70-80°C for 30-60 minutes each time, repeat three times, and concentrate to 1 / 4-1 / 3 of the amount of ethanol added. S2. Functional component pretreatment: Mix 0.5-5% of an antibacterial desensitizer, 22-35% of an alcohol solvent, 0.5-2% of hydroxypropyl cyclodextrin, and 0.1-0.2% of tocopherol; heat to 60-70°C and stir to dissolve; place in an ice water bath and ultrasonicate for 1-3 minutes; S3. Synthesis of composition: Take 30-50% of the filtrate obtained from S1 and mix it with the S2 solution; heat it in a water bath to 50-60°C and stir for 3-5 minutes; add water to 100% and place it in an ice water bath; ultrasonically treat it for 8-12 minutes; and stir it for 5-10 minutes to obtain the product.
5. The method for preparing an anti-acne composition containing multiple plants and antibacterial soothing agents according to claim 4, characterized in that: The rotary evaporation in S1 is carried out in three stages: the first stage is evaporation at a constant temperature of 65-70° C. for 30 minutes, the second stage is evaporation at a constant temperature of 75-80° C. for 40 minutes, and the third stage is evaporation at a constant temperature of 70-75° C. for 50 minutes.
6. The method for preparing an anti-acne composition containing multiple plants and antibacterial soothing agents according to claim 4, characterized in that: The ultrasonic treatment in S3 adopts an intermittent mode: the operation is cyclical, with a power density of 50-80 W / L, after working for 2 seconds and resting for 1 second.
7. The method for preparing an anti-acne composition containing multiple plants and antibacterial soothing agents according to claim 4, characterized in that: The amount of 75% ethanol added to the S1 is 10 times the total dry weight of the raw materials.
8. The method for preparing an anti-acne composition containing multiple plants and antibacterial soothing agents according to claim 4, characterized in that: The temperature of the S2 dissolution process is controlled at 68±2°C; the ice water bath temperature is 0-5°C, the ice water bath treatment time does not exceed 5 minutes, and the ultrasonic frequency is 20-40kHz.
9. The method for preparing an anti-acne composition containing multiple plants and antibacterial soothing agents according to claim 4, characterized in that: The water bath heating in S3 adopts a constant temperature water bath, and the stirring rate is 200-400 rpm; the water adding process adopts a gradient water addition method: 60% of the total water volume is added for the first time, and the remaining water is added after stirring for 3 minutes.
10. The method for preparing an anti-acne composition containing multiple plants and antibacterial soothing agents according to claim 4, characterized in that: The rotary evaporation in S1 was carried out under a vacuum condition of -0.098 MPa.
Citation Information
Patent Citations
Natural plant acne treatment gel and preparation method of natural plant acne treatment gel
CN107550775A
Acne-removing traditional Chinese medicine composition, application thereof and acne-removing balancing essence containing composition
CN111588815A
Plant acne-removing agent and preparation method and application thereof
CN112516034A
Acne-removing gel composition containing various plant essences
CN113318019A
Plant extract composite bacteriostatic agent and application thereof
CN113509413A