Traditional Chinese medicine composition with soothing and oil control effects, preparation method and application thereof
By combining traditional Chinese medicine ingredients such as mulberry bark with enzymatic hydrolysis-ultrasound extraction technology, a safe and gentle oil-control product was prepared. This product solves the problems of existing oil-control products damaging the skin barrier and lacking soothing and anti-inflammatory effects, achieving effective skin oil regulation and healthy care.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- GUANGDONG BAWEI BIOLOGICAL TECH CO LTD
- Filing Date
- 2025-12-29
- Publication Date
- 2026-04-28
AI Technical Summary
Existing oil-control products mostly rely on chemically synthesized ingredients, which can damage the skin barrier and lack the ability to provide long-term soothing and anti-inflammatory care, thus failing to effectively solve the problems of excessive sebum secretion and skin discomfort in oily skin.
A combination of traditional Chinese medicines, including mulberry bark, houttuynia cordata, soapberry, arborvitae leaf, safflower, dictamnus dasycarpus bark, and chrysanthemum, was prepared using enzymatic hydrolysis-ultrasound extraction technology. This combination has a soothing and oil-controlling effect, achieving deep cleansing and long-lasting oil control by inhibiting inflammatory factors and sebum synthesis.
This traditional Chinese medicine composition is safe and gentle, effectively inhibiting sebum secretion, reducing inflammation, providing long-term skin health balance, and possessing excellent soothing and oil-controlling effects.
Smart Images

Figure CN121401174B_ABST
Abstract
Description
Technical Field
[0001] This application relates to the field of cosmetic technology, and in particular to traditional Chinese medicine compositions with soothing and oil-controlling effects, their preparation methods, and applications. Background Technology
[0002] In the field of modern skincare, the needs for oily and combination skincare are becoming increasingly prominent. The core issue lies in the excessive secretion of sebaceous glands, leading to a series of problems such as enlarged pores, dull skin tone, and acne. Currently, most oil-control products on the market rely on chemically synthesized ingredients (such as alcohol, salicylic acid, and zinc salts) or potent exfoliating agents. While these ingredients may provide significant short-term oil control, they often damage the skin barrier, causing dryness and tightness, and even leading to a vicious cycle of skin sensitivity and "oily on the surface but dry underneath." Especially for oily skin that is sensitive due to a damaged barrier, the irritation of traditional strong oil-control products makes long-term, safe use difficult.
[0003] Furthermore, modern research reveals that external stimuli such as mental stress, irregular sleep patterns, and environmental pollution can induce neurogenic inflammation, exacerbating sebum secretion and skin discomfort. Therefore, an ideal oil-control solution must not only effectively reduce oil production but also possess excellent soothing, anti-inflammatory, and barrier-repairing capabilities to achieve a long-term balance of skin health. Many traditional Chinese medicine ingredients are derived from nature, with gentle mechanisms of action, combining efficacy and safety. The development of traditional Chinese medicine compositions aims to provide an oil-control approach that does not rely on strong irritants, making it particularly suitable for sensitive, oily skin requiring long-term care, filling a gap in the market for "soothing oil-control" products.
[0004] CN105012483A discloses a traditional Chinese medicine composition and preparation method for treating seborrheic dermatitis of the scalp, containing ingredients such as rhubarb, scutellaria baicalensis, sophora flavescens, dried plum, and angelica sinensis. Although this composition has good effects in dispelling wind and relieving itching, and combating seborrheic dermatitis, the formulation is too complex. CN119656085B discloses an oil-controlling, anti-inflammatory, and soothing plant composition containing eight ingredients, including centella asiatica extract, licorice extract, gentiana oleifera extract, and willowherb extract. Although this composition has good soothing and oil-controlling effects, the extracts used in the formula are obtained using different extraction processes, making the extraction process too complex.
[0005] Furthermore, existing products with soothing and oil-controlling effects have not undergone corresponding research on the mechanism and target of their soothing and oil-controlling effects, and quality control cannot be effectively carried out during production. Summary of the Invention
[0006] To address the aforementioned shortcomings, the purpose of this application is to provide a traditional Chinese medicine composition with soothing and oil-controlling effects, which can be applied in cosmetics to effectively inhibit the expression of inflammatory factors and mediators and inhibit oil synthesis. It can effectively exert good soothing and oil-controlling effects, and the traditional Chinese medicine composition itself is safe, mild and non-irritating, and can be widely used in the skin care field.
[0007] In the first aspect, this application provides a traditional Chinese medicine composition with soothing and oil-controlling effects, the raw materials of which include, by weight: 1-50 parts of mulberry bark, 1-50 parts of houttuynia cordata, 1-50 parts of soapberry, 1-50 parts of arborvitae leaf, 1-50 parts of safflower, 1-40 parts of dictamnus dasycarpus bark, and 1-40 parts of chrysanthemum.
[0008] The traditional Chinese medicine composition of this application with soothing and oil-controlling effects has excellent soothing and oil-controlling effects, and its raw material composition is relatively simple, and the raw materials are widely available and easy to obtain.
[0009] Furthermore, the Chinese herbal composition with soothing and oil-controlling effects also includes 1-40 parts of Sichuan pepper by weight.
[0010] Furthermore, the Chinese herbal composition with soothing and oil-controlling effects also includes 1-20 parts of excipients by weight.
[0011] Optionally, the excipients include at least one of starch and maltodextrin.
[0012] Secondly, this application provides a method for preparing a traditional Chinese medicine composition with soothing and oil-controlling effects, comprising the following steps:
[0013] Weigh the following raw materials in the indicated weights: 1-50 parts of mulberry bark, 1-50 parts of houttuynia cordata, 1-50 parts of soapberry, 1-50 parts of arborvitae leaf, 1-50 parts of safflower, 1-40 parts of dictamnus dasycarpus bark, and 1-40 parts of chrysanthemum. Crush each raw material separately, sieve it, and mix the resulting powders to obtain fine powder of traditional Chinese medicine.
[0014] The fine powder of the traditional Chinese medicine, water, and enzyme are mixed. The resulting mixture is enzymatically hydrolyzed at a first temperature for a first time, and then enzymatically hydrolyzed at a second temperature for a second time. The mixture is then filtered to obtain a first filtrate and a first filter residue. The first filter residue is mixed with an extraction solvent, and the resulting mixture is ultrasonically treated at a third temperature for a third time. The mixture is then filtered to obtain a second filtrate and a second filter residue. The first filtrate and the second filtrate are combined to obtain an extract. The first temperature is 40℃-70℃, and the first time is 1h-3h. The second temperature is 80℃-90℃, and the second time is 10min-20min. The third temperature is 0℃-80℃, and the third time is 0.5h-4h.
[0015] The extract is concentrated until the weight ratio of the concentrate to the fine powder of the traditional Chinese medicine is 0.8-1.2. The concentrated extract is then settled at a fourth temperature, centrifuged, and the supernatant is collected. The fourth temperature is 0℃-4℃.
[0016] The supernatant is filtered through a membrane, and the filtrate is concentrated until the weight ratio of the concentrated liquid to the fine powder of the traditional Chinese medicine is 0.1-0.5. The concentrated supernatant is then dried with excipients to obtain the traditional Chinese medicine composition with soothing and oil-controlling effects.
[0017] The preparation method of the traditional Chinese medicine composition with soothing and oil-controlling effects of this application is simple. After crushing the raw materials, they are mixed to obtain fine powder of traditional Chinese medicine. The powder is extracted using a highly efficient enzymatic hydrolysis-ultrasonic extraction technology. Combined with simple filtration, sedimentation, centrifugation and other processes, the active ingredients can be effectively extracted, and the composition has excellent soothing and oil-controlling effects.
[0018] Furthermore, the power of the ultrasound is 50W-1500W, and the frequency is 10KHZ-40KHZ.
[0019] Furthermore, the enzyme comprises at least one of cellulase, pectinase, or protease; and / or,
[0020] The enzyme is added at a rate of 3000 U / g to 5000 U / g relative to the fine powder of the traditional Chinese medicine.
[0021] Further, the extraction solvent includes at least one of water and ethanol; and / or,
[0022] The weight-to-volume ratio of the first filter residue to the extraction solvent is 1:10-1:30 (g / mL).
[0023] Furthermore, the preparation method satisfies at least one of the following conditions:
[0024] (1) The mesh size of the sieve is 40-60 mesh;
[0025] (2) In the step of concentrating the extract, the extract is concentrated under the conditions of a pressure of 2KPa-20KPa and a temperature of 40℃-70℃;
[0026] (3) In the step of concentrating the supernatant, the supernatant is concentrated under the conditions of pressure of 2KPa-20KPa and temperature of 40℃-70℃;
[0027] (4) The settling time is 5h-20h;
[0028] (5) The centrifugation speed is 5000 r / min-20000 r / min;
[0029] (6) The membrane used for membrane filtration includes one or more of microfiltration membrane, ultrafiltration membrane or nanofiltration membrane, with the microfiltration membrane having a pore size of 0.1-3 μm, the ultrafiltration membrane having a pore size of 10-50 nm, and the nanofiltration membrane having a pore size of 100-1000 Da.
[0030] Furthermore, in the step of drying the concentrated supernatant, the concentrated supernatant is spray-dried or freeze-dried.
[0031] Optionally, the spray drying conditions include: an inlet temperature of 100℃-130℃ and an outlet temperature of 50℃-80℃.
[0032] Optionally, the freeze-drying conditions include: a pre-freezing temperature of -20°C to -80°C and a pre-freezing time of 3h to 8h; a sublimation pressure of 0Pa to 100Pa and a sublimation time of 10h to 30h.
[0033] Thirdly, this application provides the application of the traditional Chinese medicine composition with soothing and oil-controlling effects described above, or the traditional Chinese medicine composition with soothing and oil-controlling effects prepared by the preparation method described above, in the preparation of cosmetics.
[0034] The raw materials of the traditional Chinese medicine composition in this application are formulated according to the principle of "principal, assistant, adjuvant, and guide": Mulberry bark and houttuynia cordata are the principal herbs. Mulberry bark specifically enters the lung meridian, clearing lung heat and reducing excessive sebum secretion at its source. Houttuynia cordata has heat-clearing and detoxifying effects, and modern pharmacology has confirmed its broad-spectrum antibacterial and anti-inflammatory capabilities, effectively preventing and alleviating inflammation caused by sebum blockage. Together, they are the principal herbs. Gleditsia sinensis and Platycladus orientalis leaves are the assistant herbs. Gleditsia sinensis possesses excellent natural surface activity, gently and thoroughly removing excess oil and dirt from the skin surface and pores. Platycladus orientalis leaves clear heat and cool the blood, tighten pores, and reduce sebum secretion. Together, they achieve deep cleansing and long-lasting oil control. Safflower, Dictamnus dasycarpus, and chrysanthemum are the adjuvant herbs, improving skin blood circulation, promoting metabolism, achieving the effects of dispelling wind and relieving itching, and providing antioxidant protection. Optionally, Sichuan pepper is used as the guide herb, which can guide the medicine upwards to the skin, harmonize the other herbs, moderate their properties, and consolidate the efficacy of the formula. This traditional Chinese medicine composition focuses on soothing and oil control, regulating the secretion of sebum in the skin, while also taking into account multiple effects such as antibacterial, anti-inflammatory, pore tightening, and soothing and calming, thus having excellent soothing and oil-controlling effects.
[0035] The traditional Chinese medicine composition of this application can inhibit the expression of inflammatory factors IL-33 and IL-6, as well as the release of inflammatory mediator NO and the inhibition of lipid synthesis pathways, thereby exerting good soothing and oil-controlling effects.
[0036] The raw materials of the traditional Chinese medicine composition in this application are all derived from medicinal ingredients. They have the advantages of being pure, natural, non-irritating, safe and non-toxic, which can meet the needs of safe skin care and have good prospects for promotion and application.
[0037] The method for preparing the traditional Chinese medicine composition of this application employs a highly efficient enzymatic hydrolysis-ultrasound mixed extraction technology. The complex enzyme is used to destroy the cell wall structure, making the intracellular components easier to dissolve. At the same time, the strong shearing force and cavitation effect generated under the action of ultrasound greatly improve the extraction efficiency and make the active ingredients more completely extracted. Attached Figure Description
[0038] To more clearly illustrate the technical solutions in the specific embodiments of this application or the prior art, the drawings used in the description of the specific embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of this application. For those skilled in the art, other drawings can be obtained from these drawings without creative effort.
[0039] Figure 1 This is a graph showing the change in the average skin redness value in the human test of Example 1 of this application, illustrating the decrease in skin redness value within 15 minutes after using the sample emulsion and the blank emulsion.
[0040] Figure 2 This is a graph showing the change in skin oil content in a human test in Example 1 of this application, illustrating the difference in skin oil content between the sample area and the blank area after 4 hours and 8 hours.
[0041] Figure 3 The Venn diagram, showing the intersection of the active ingredients of the herbal composition in this application with targets related to skin sensitivity and sebum, and potential compound targets, illustrates the intersection of these targets.
[0042] Figure 4 The protein-protein interaction network analysis diagram of the traditional Chinese medicine composition and the overlapping targets of skin sensitivity in this application reveals the connection and regulatory relationship of key targets in the network.
[0043] Figure 5 This is a protein-protein interaction network analysis diagram of the overlapping targets of the traditional Chinese medicine composition and skin sebum in this application, which shows the interaction of key targets in the sebum regulatory network.
[0044] Figure 6The GO functional enrichment map of the core target of skin sensitivity illustrates the main pathways of action of this composition in biological processes, cellular components, and molecular functions; where 1-30 represent: 1-positive regulation of cell migration; 2-positive regulation of cell motility; 3-positive regulation of motility; 4-cellular response to nitrogenous compounds; 5-cellular response to lipids; 6-enzyme-linked receptor protein signaling pathway; 7-regulation of MAPK cascade; 8-response to bacteria; 9-cellular response to hormone stimulation; 10-hematopoiesis; 11-membrane side; 12-membrane raft; 1 3-Membrane microdomain; 14-Vessel cavity; 15-Cytoplasmic vesicle cavity; 16-Perinuclear cytoplasmic region; 17-Secretionary granule cavity; 18-Receptor complex; 19-Transcription regulator complex; 20-Cyclic vacuoles; 21-Phosphotransferase activity, with alcohol groups as receptors; 22-Kinetic activity; 23-Protein kinase activity; 24-Kinetic binding; 25-Protein kinase binding; 26-Protein domain-specific binding; 27-Protein homodimerization activity; 28-Transcription factor binding; 29-Signal receptor regulatory activity; 30-Signal receptor activation activity.
[0045] Figure 7 GO functional enrichment plots of core targets in skin sebum demonstrate the key functional categories of the composition in sebum regulation; 1-30 represent: 1-cellular response to lipids; 2-regulation of inflammatory response; 3-glandular development; 4-cellular response to hormone stimulation; 5-intracellular receptor signaling pathway; 6-negative regulation of cell population proliferation; 7-inflammatory response; 8-regulation of protein localization; 9-response to nutrient levels; 10-regulation of small molecule metabolism; 11-transcriptional regulatory factor complex; 12-receptor complex. 13-Secretion granule lumen; 14-Cytoplasmic vesicle lumen; 15-Vesicle lumen; 16-Membrane raft; 17-Membrane microdomain; 18-Endoplasmic reticulum lumen; 19-Platelet α-granule lumen; 20-Platelet α-granule; 21-Nuclear receptor activity; 22-Ligand-regulated transcription factor activity; 23-Transcription factor binding; 24-Receptor ligand activity; 25-Signal receptor activation activity; 26-Signal receptor regulatory activity; 27-Cytokine receptor binding; 28-Transcription co-regulatory factor binding; 29-Cytokine activity; 30-Protein kinase binding.
[0046] Figure 8 The KEGG pathway enrichment map for the core target of skin sensitivity reveals the key signaling pathways that the herbal composition in this application may be involved in the regulation of skin sensitivity.
[0047] Figure 9 The KEGG pathway enrichment map of the core target of skin sebum shows the main metabolic and signaling pathways that the composition may participate in during sebum regulation. Detailed Implementation
[0048] The present application is further described below with reference to embodiments and examples. It should be understood that these embodiments are for illustrative purposes only and are not intended to limit the scope of the application. Furthermore, it should be understood that after reading the teachings of this application, those skilled in the art can make various alterations or modifications to this application, and these equivalent forms also fall within the protection scope of the appended claims.
[0049] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the application.
[0050] The term "and / or" as used herein includes any one of two or more related listed items, as well as any and all combinations of the related listed items. These arbitrary and all combinations encompass any two related listed items, any more related listed items, or a combination of all related listed items. It should be noted that when at least three items are connected using at least two conjunctions selected from "and / or," it should be understood that, in this application, the technical solution undoubtedly includes solutions connected by "logical AND," and also undoubtedly includes solutions connected by "logical OR." For example, "A and / or B" includes three parallel solutions: A, B, and A+B.
[0051] In this application, terms such as "further" and "preferred" are used for descriptive purposes and to indicate differences in content, but should not be construed as limiting the scope of protection of this application.
[0052] The terms "first," "second," "third," and "fourth" are used for descriptive purposes only and should not be interpreted as indicating or implying relative importance or quantity, nor should they be interpreted as implicitly specifying the importance or quantity of the indicated technical features. Moreover, "first," "second," "third," and "fourth" serve only as a non-exhaustive enumeration and should be understood as not constituting a closed limitation on quantity.
[0053] In this application, the technical features described in an open-ended manner include both closed technical solutions consisting of the listed features and open technical solutions that include the listed features.
[0054] In this application, numerical intervals (i.e., numerical ranges) are involved. Unless otherwise specified, optional numerical distributions within the aforementioned numerical intervals are considered continuous and include the two endpoints (i.e., the minimum and maximum values) of the numerical range, as well as every value between these two endpoints. Unless otherwise specified, when a numerical interval refers only to integers within that interval, it includes the two endpoint integers of the numerical range, as well as every integer between the two endpoints. Furthermore, when multiple ranges are provided to describe features or characteristics, these ranges can be merged. In other words, unless otherwise specified, the ranges disclosed herein should be understood to include any and all subranges to which they are included.
[0055] In this application, weight can be a well-known unit of mass in the pharmaceutical or cosmetic field, such as μg, mg, g, or kg.
[0056] In the first aspect, this application provides a traditional Chinese medicine composition with soothing and oil-controlling effects, the raw materials of which include, by weight: 1-50 parts of mulberry bark, 1-50 parts of houttuynia cordata, 1-50 parts of soapberry, 1-50 parts of arborvitae leaf, 1-50 parts of safflower, 1-40 parts of dictamnus dasycarpus bark, and 1-40 parts of chrysanthemum.
[0057] Preferably, the raw materials of the traditional Chinese medicine composition with soothing and oil-controlling effects include, by weight, 10-40 parts of mulberry bark, 10-40 parts of houttuynia cordata, 10-40 parts of soapberry, 10-40 parts of arborvitae leaf, 10-40 parts of safflower, 10-40 parts of dictamnus dasycarpus bark, and 10-40 parts of chrysanthemum. The weight percentage of each raw material can be independently selected from any value within the specified range (10-40 parts), such as 10 parts, 20 parts, 30 parts, or 40 parts.
[0058] In some embodiments, the raw materials of the traditional Chinese medicine composition having soothing and oil-controlling effects include, by weight: 20 parts of mulberry bark, 20 parts of houttuynia cordata, 20 parts of soapberry, 20 parts of arborvitae leaf, 20 parts of safflower, 20 parts of dictamnus dasycarpus bark, 20 parts of chrysanthemum and 20 parts of Sichuan pepper.
[0059] In some embodiments, the raw materials of the traditional Chinese medicine composition having soothing and oil-controlling effects include, by weight: 40 parts of mulberry bark, 40 parts of houttuynia cordata, 20 parts of soapberry, 20 parts of arborvitae leaf, 10 parts of safflower, 10 parts of dictamnus dasycarpus bark, 10 parts of chrysanthemum and 10 parts of Sichuan pepper.
[0060] In some embodiments, the raw materials of the traditional Chinese medicine composition having soothing and oil-controlling effects include, by weight: 10 parts of mulberry bark, 10 parts of houttuynia cordata, 10 parts of soapberry, 10 parts of arborvitae leaf, 20 parts of safflower, 40 parts of dictamnus dasycarpus bark, 40 parts of chrysanthemum, and 40 parts of Sichuan pepper.
[0061] In some embodiments, the raw materials of the traditional Chinese medicine composition having soothing and oil-controlling effects include, by weight: 20 parts of mulberry bark, 20 parts of houttuynia cordata, 40 parts of soapberry, 40 parts of arborvitae leaf, 10 parts of safflower, 10 parts of dictamnus dasycarpus bark, 10 parts of chrysanthemum, and 10 parts of Sichuan pepper.
[0062] In some embodiments, the raw materials of the traditional Chinese medicine composition having soothing and oil-controlling effects include, by weight: 30 parts of mulberry bark, 10 parts of houttuynia cordata, 10 parts of soapberry, 20 parts of arborvitae leaf, 40 parts of safflower, 10 parts of dictamnus dasycarpus bark, 20 parts of chrysanthemum and 20 parts of Sichuan pepper.
[0063] In some embodiments, the raw materials of the traditional Chinese medicine composition with soothing and oil-controlling effects include, by weight: 10 parts of mulberry bark, 30 parts of houttuynia cordata, 10 parts of soapberry, 30 parts of arborvitae leaf, 20 parts of safflower, 40 parts of dictamnus dasycarpus bark, 10 parts of chrysanthemum and 10 parts of Sichuan pepper.
[0064] In some embodiments, the raw materials of the traditional Chinese medicine composition having soothing and oil-controlling effects include, by weight: 20 parts of mulberry bark, 20 parts of houttuynia cordata, 20 parts of soapberry, 20 parts of arborvitae leaf, 20 parts of safflower, 20 parts of dictamnus dasycarpus bark, 20 parts of chrysanthemum and 20 parts of Sichuan pepper.
[0065] The traditional Chinese medicine composition of this application with soothing and oil-controlling effects has excellent soothing and oil-controlling effects, and its raw material composition is relatively simple, and the raw materials are widely available and easy to obtain.
[0066] Furthermore, the Chinese herbal composition with soothing and oil-controlling effects also includes 1-40 parts of Sichuan pepper by weight.
[0067] Furthermore, the Chinese herbal composition with soothing and oil-controlling effects also includes 1-20 parts of excipients by weight.
[0068] Optionally, the excipients include at least one of starch and maltodextrin.
[0069] Secondly, this application provides a method for preparing a traditional Chinese medicine composition with soothing and oil-controlling effects, comprising the following steps:
[0070] Weigh the following raw materials in the indicated weights: 1-50 parts of mulberry bark, 1-50 parts of houttuynia cordata, 1-50 parts of soapberry, 1-50 parts of arborvitae leaf, 1-50 parts of safflower, 1-30 parts of dictamnus dasycarpus bark, and 1-30 parts of chrysanthemum. Crush each raw material separately, sieve it, and mix the resulting powders to obtain fine powder of traditional Chinese medicine.
[0071] The fine powder of the traditional Chinese medicine, water, and enzyme are mixed. The resulting mixture is enzymatically hydrolyzed at a first temperature for a first time, and then enzymatically hydrolyzed at a second temperature for a second time. The mixture is then filtered to obtain a first filtrate and a first filter residue. The first filter residue is mixed with an extraction solvent, and the resulting mixture is ultrasonically treated at a third temperature for a third time. The mixture is then filtered to obtain a second filtrate and a second filter residue. The first filtrate and the second filtrate are combined to obtain an extract. The first temperature is 40℃-70℃, and the first time is 1h-3h. The second temperature is 80℃-90℃, and the second time is 10min-20min. The third temperature is 0℃-80℃, and the third time is 0.5h-4h.
[0072] The extract is concentrated until the weight ratio of the concentrate to the fine powder of the traditional Chinese medicine is 0.8-1.2. The concentrated extract is then settled at a fourth temperature, centrifuged, and the supernatant is collected. The fourth temperature is 0℃-4℃.
[0073] The supernatant is filtered through a membrane, and the filtrate is concentrated until the weight ratio of the concentrated liquid to the fine powder of the traditional Chinese medicine is 0.1-0.5. The concentrated supernatant is then dried with excipients to obtain the traditional Chinese medicine composition with soothing and oil-controlling effects.
[0074] The preparation method of the traditional Chinese medicine composition with soothing and oil-controlling effects of this application is simple. After crushing the raw materials, they are mixed to obtain fine powder of traditional Chinese medicine. The powder is extracted using a highly efficient enzymatic hydrolysis-ultrasonic extraction technology. Combined with simple filtration, sedimentation, centrifugation and other processes, the active ingredients can be effectively extracted, and the composition has excellent soothing and oil-controlling effects.
[0075] Optionally, the first temperature is 40℃-70℃, for example 40℃, 50℃, 60℃, 70℃, etc., and the first time is 1h-3h, for example 1h, 2h, 3h, etc.
[0076] Optionally, the second temperature is 80℃-90℃, for example 80℃, 85℃, 90℃, etc., and the second time is 10min-20min, for example 10min, 15min, 20min, etc.
[0077] Optionally, the third temperature is 0℃-80℃, for example 0℃, 20℃, 40℃, 60℃, 80℃, etc., and the third time is 0.5h-4h, for example 0.5h, 1h, 2h, 3h, 4h, etc.
[0078] Furthermore, the power of the ultrasound is 50W-1500W, for example 50W, 200W, 500W, 1000W, 1500W, etc., and the frequency is 10KHZ-40KHZ, for example 10KHZ, 20KHZ, 40KHZ, etc.
[0079] Furthermore, the enzyme comprises at least one of cellulase, pectinase, or protease; and / or,
[0080] The enzyme is added at a rate of 3000 U / g to 5000 U / g relative to the fine powder of the traditional Chinese medicine.
[0081] Preferably, the enzyme composition includes cellulase, pectinase, or protease in a weight ratio of 1:(0.8-1.2):(0.8-1.2). This enables better enzymatic release of active ingredients in the fine powder of traditional Chinese medicine.
[0082] Further, the extraction solvent includes at least one of water and ethanol; and / or,
[0083] The weight-to-volume ratio of the first filter residue to the extraction solvent is 1:10 to 1:30 (g / mL), for example, 1g:10mL, 1g:20mL, 1g:30mL, etc. The unit of weight-to-volume ratio, 1:10 g / mL, has the same meaning as 1g:10mL.
[0084] Furthermore, the preparation method satisfies at least one of the following conditions:
[0085] (1) The mesh size of the sieve is 40-60 mesh;
[0086] (2) In the step of concentrating the extract, the extract is concentrated under the conditions of a pressure of 2KPa-20KPa and a temperature of 40℃-70℃;
[0087] (3) In the step of concentrating the supernatant, the supernatant is concentrated under the conditions of pressure of 2KPa-20KPa and temperature of 40℃-70℃;
[0088] (4) The settling time is 5h-20h;
[0089] (5) The centrifugation speed is 5000 r / min-20000 r / min;
[0090] (6) The membrane filtration pore size is one or more of microfiltration membrane, ultrafiltration membrane or nanofiltration membrane, with the microfiltration membrane pore size being 0.1-3μm, the ultrafiltration membrane pore size being 10-50nm, and the nanofiltration membrane pore size being 100-1000Da.
[0091] Furthermore, in the step of drying the concentrated supernatant, the concentrated supernatant is spray-dried or freeze-dried.
[0092] Optionally, the spray drying conditions include: an inlet temperature of 100℃-130℃ and an outlet temperature of 50℃-80℃.
[0093] Optionally, the freeze-drying conditions include: a pre-freezing temperature of -20°C to -80°C and a pre-freezing time of 3h to 8h; a sublimation pressure of 0Pa to 100Pa and a sublimation time of 10h to 30h.
[0094] Thirdly, this application provides the application of the traditional Chinese medicine composition with soothing and oil-controlling effects described above, or the traditional Chinese medicine composition with soothing and oil-controlling effects prepared by the preparation method described above, in the preparation of cosmetics.
[0095] The aforementioned traditional Chinese medicine composition with soothing and oil-controlling effects can be used to prepare soothing and oil-controlling cosmetics. These cosmetics are topical skin preparations made with the aforementioned traditional Chinese medicine composition as the active ingredient, plus conventional pharmaceutical or cosmetic excipients or auxiliary ingredients. In practical use, the soothing and oil-controlling traditional Chinese medicine composition is directly added to the cosmetic base; the amount added can be adjusted according to actual needs, preferably 0.1wt%-1wt%.
[0096] Fourthly, a cosmetic product is also provided, comprising the traditional Chinese medicine composition with soothing and oil-controlling effects described above.
[0097] In some embodiments, the cosmetic comprises 0.1wt%-1wt% of a traditional Chinese medicine composition with soothing and oil-controlling effects and 99wt%-99.9wt% of a matrix. The matrix may be composed of pharmaceutical or cosmetic excipients or auxiliary ingredients.
[0098] The following are some specific examples.
[0099] For experimental parameters not specified in the following specific embodiments, please refer to the guidelines given in this application document first, or refer to experimental manuals or other experimental methods known in the art, or refer to the experimental conditions recommended by the manufacturer.
[0100] The raw materials and reagents involved in the following specific embodiments can be obtained commercially or prepared by those skilled in the art using known methods.
[0101] I. Preparation of Traditional Chinese Medicine Compositions with Soothing and Oil-Controlling Effects
[0102] Example 1
[0103] This embodiment provides a traditional Chinese medicine composition with soothing and oil-controlling effects, which is prepared by extraction from the following raw materials: 20g of mulberry bark, 20g of houttuynia cordata, 20g of soapberry, 20g of arborvitae leaf, 20g of safflower, 20g of dictamnus dasycarpus bark, 20g of chrysanthemum and 20g of Sichuan pepper.
[0104] The preparation steps are as follows:
[0105] S1. Raw material pretreatment: Crush the above raw materials separately using a pulverizer, and pass the resulting powder through a 50-mesh sieve to obtain fine powder; accurately weigh the fine powder of each raw material according to the specified weight and mix them evenly.
[0106] S2. Extraction and Separation: The fine powder of traditional Chinese medicine obtained in S1 is added to an extraction tank, along with deionized water and a mixed enzyme (composed of cellulase, pectinase, and protease in a weight ratio of 1:1:1). The amount of enzyme added is 4000 U / g relative to the weight of the fine powder of traditional Chinese medicine. The resulting mixture is enzymatically hydrolyzed at 55℃ for 2 hours. After that, the temperature is raised to 85℃ and kept at that temperature for 15 minutes. The mixture is then filtered to obtain the first filtrate and the first filter residue. The first filter residue is added to a 50% ethanol aqueous solution at a material-to-liquid ratio of 1:20 (g / mL). The resulting mixture is then ultrasonically extracted at a power of 800W, a frequency of 20kHz, and a temperature of 60℃ for 2 hours. The mixture is then filtered to obtain the second filtrate and the second filter residue. The first and second filtrates are combined to obtain the extract.
[0107] S3. Concentration and Filtration: The extract obtained in S2 is concentrated under reduced pressure at 5 kPa to a weight ratio of 1:1 to the fine powder of traditional Chinese medicine. The liquid is cooled and allowed to settle at 0℃-4℃ for 10 h. Then, it is centrifuged at high speed using a tubular centrifuge at 10000 r / min. The supernatant is collected and filtered through a 0.45 μm microfiltration membrane to obtain the filtrate.
[0108] S4. Drying: The filtrate obtained in S3 is concentrated until the weight ratio of the concentrated liquid to the fine powder of traditional Chinese medicine is 0.5. Maltodextrin with a weight of 0.05 times that of the powder of traditional Chinese medicine is added and stirred evenly. The mixture is then placed in a freeze dryer for pre-freezing at a temperature of -70℃ for 5 hours. After pre-freezing, the mixture is sublimated and dried under a pressure of 2Pa for 15 hours. After drying, the mixture is removed, pulverized, and a traditional Chinese medicine composition with soothing and oil-controlling effects is obtained.
[0109] Example 2
[0110] This embodiment provides a traditional Chinese medicine composition with soothing and oil-controlling effects, which is prepared by extraction from the following raw materials: 40g of mulberry bark, 40g of houttuynia cordata, 20g of soapberry, 20g of arborvitae leaf, 10g of safflower, 10g of dictamnus dasycarpus bark, 10g of chrysanthemum, and 10g of Sichuan pepper. The preparation steps are the same as in Example 1.
[0111] Example 3
[0112] This embodiment provides a traditional Chinese medicine composition with soothing and oil-controlling effects, prepared from the following raw materials: 10g of mulberry bark, 10g of houttuynia cordata, 10g of soapberry, 10g of arborvitae leaf, 20g of safflower, 40g of dictamnus dasycarpus bark, 40g of chrysanthemum, and 40g of Sichuan pepper. The preparation steps are the same as in Example 1.
[0113] Example 4
[0114] This embodiment provides a traditional Chinese medicine composition with soothing and oil-controlling effects, which is prepared by extraction from the following raw materials: 20g of mulberry bark, 20g of houttuynia cordata, 40g of soapberry, 40g of arborvitae leaves, 10g of safflower, 10g of dictamnus dasycarpus bark, 10g of chrysanthemum, and 10g of Sichuan pepper. The preparation steps are the same as in Example 1.
[0115] Example 5
[0116] This embodiment provides a traditional Chinese medicine composition with soothing and oil-controlling effects, prepared from the following raw materials: 30g of mulberry bark, 10g of houttuynia cordata, 10g of soapberry, 20g of arborvitae leaves, 40g of safflower, 10g of dictamnus dasycarpus root bark, 20g of chrysanthemum, and 20g of Sichuan pepper. The preparation steps are the same as in Example 1.
[0117] Example 6
[0118] This embodiment provides a traditional Chinese medicine composition with soothing and oil-controlling effects, prepared from the following raw materials: 10g of mulberry bark, 30g of houttuynia cordata, 10g of soapberry, 30g of arborvitae leaves, 20g of safflower, 40g of dictamnus dasycarpus bark, 10g of chrysanthemum, and 10g of Sichuan pepper. The preparation steps are the same as in Example 1.
[0119] Example 7
[0120] This embodiment provides a soothing and oil-controlling traditional Chinese medicine composition, prepared from the following raw materials: 20g of mulberry bark, 20g of houttuynia cordata, 20g of soapberry, 20g of arborvitae leaf, 20g of safflower, 20g of dictamnus dasycarpus bark, 20g of chrysanthemum, and 20g of Sichuan pepper. The preparation steps are basically the same as in Example 1, except that cellulase is used instead of the mixed enzyme, and its addition amount is maintained at 4000 U / g relative to the weight of the fine powder of traditional Chinese medicine.
[0121] Example 8
[0122] This embodiment provides a traditional Chinese medicine composition with soothing and oil-controlling effects, prepared from the following raw materials: 20g of mulberry bark, 20g of houttuynia cordata, 20g of soapberry, 20g of arborvitae leaf, 20g of safflower, 20g of dictamnus dasycarpus bark, 20g of chrysanthemum, and 20g of Sichuan pepper. The preparation steps are basically the same as in Example 1, except that the amount of mixed enzyme added is reduced to 2000U / g.
[0123] Example 9
[0124] This embodiment provides a traditional Chinese medicine composition with soothing and oil-controlling effects, prepared from the following raw materials: 20g of mulberry bark, 20g of houttuynia cordata, 20g of soapberry, 20g of arborvitae leaf, 20g of safflower, 20g of dictamnus dasycarpus bark, 20g of chrysanthemum, and 20g of Sichuan pepper. The preparation steps are basically the same as in Example 1, except that the enzymatic hydrolysis time is 30 minutes.
[0125] Example 10
[0126] This embodiment provides a traditional Chinese medicine composition with soothing and oil-controlling effects, prepared from the following raw materials: 20g of mulberry bark, 20g of houttuynia cordata, 20g of soapberry, 20g of arborvitae leaves, 20g of safflower, 20g of dictamnus dasycarpus bark, 20g of chrysanthemum, and 20g of Sichuan pepper. The preparation steps are basically the same as in Example 1, except that the enzymatic hydrolysis temperature is 85℃ and the enzymatic hydrolysis time is 4h.
[0127] Comparative Example 1
[0128] This comparative example provides another traditional Chinese medicine composition with soothing and oil-controlling effects, prepared from the following raw materials: 40g of mulberry bark, 20g of houttuynia cordata, 20g of soapberry, 20g of arborvitae leaves, 20g of safflower, and 20g of dictamnus dasycarpus bark. The preparation steps are the same as in Example 1.
[0129] Comparative Example 2
[0130] This comparative example provides another traditional Chinese medicine composition with soothing and oil-controlling effects, prepared from the following raw materials: 30g of soapberry, 30g of arborvitae leaves, 20g of safflower, 20g of dictamnus root bark, 20g of chrysanthemum, and 20g of Sichuan pepper. The preparation steps are the same as in Example 1.
[0131] Comparative Example 3
[0132] This comparative example provides another traditional Chinese medicine composition with soothing and oil-controlling effects, prepared from the following raw materials: 20g of mulberry bark, 20g of houttuynia cordata, 40g of safflower, 20g of dictamnus dasycarpus root bark, 20g of chrysanthemum, and 20g of Sichuan pepper. The preparation steps are the same as in Example 1.
[0133] Comparative Example 4
[0134] This comparative example provides another traditional Chinese medicine composition with soothing and oil-controlling effects, prepared from the following raw materials: 20g mulberry bark, 20g houttuynia cordata, 20g soapberry, 20g arborvitae leaves, 30g chrysanthemum, and 30g Sichuan pepper. The preparation steps are the same as in Example 1.
[0135] Comparative Example 5
[0136] This comparative example provides another traditional Chinese medicine composition with soothing and oil-controlling effects, prepared from the following raw materials: 20g mulberry bark, 30g houttuynia cordata, 20g soapberry, 20g arborvitae leaves, 20g safflower, 20g dictamnus dasycarpus bark, and 20g chrysanthemum. The preparation steps are the same as in Example 1.
[0137] Comparative Example 6
[0138] This comparative example provides another traditional Chinese medicine composition with soothing and oil-controlling effects, prepared from the following raw materials: 30g mulberry bark, 30g soapberry, 20g arborvitae leaves, 30g safflower, 30g dictamnus root bark, and 20g Sichuan pepper. The preparation steps are the same as in Example 1.
[0139] Comparative Example 7
[0140] This comparative example provides another traditional Chinese medicine composition with soothing and oil-controlling effects, prepared from the following raw materials: 20g of mulberry bark, 20g of houttuynia cordata, 20g of soapberry, 20g of burnet root, 20g of safflower, 20g of dictamnus dasycarpus root bark, 20g of chrysanthemum, and 20g of Sichuan pepper. The preparation steps are the same as in Example 1.
[0141] Comparative Example 8
[0142] This comparative example provides another traditional Chinese medicine composition with soothing and oil-controlling effects, prepared from the following raw materials: 20g of mulberry bark, 20g of houttuynia cordata, 20g of soapberry, 20g of arborvitae leaf, 20g of safflower, 20g of sophora flavescens, 20g of chrysanthemum, and 20g of Sichuan pepper. The preparation steps are the same as in Example 1.
[0143] Comparative Example 9
[0144] This comparative example provides another traditional Chinese medicine composition with soothing and oil-controlling effects, prepared from the following raw materials: 20g of mulberry bark, 20g of houttuynia cordata, 20g of soapberry, 20g of arborvitae leaves, 20g of safflower, 20g of dictamnus dasycarpus root bark, 20g of honeysuckle, and 20g of Sichuan pepper. The preparation steps are the same as in Example 1.
[0145] II. Efficacy Testing Experiment
[0146] 1. IL-6 inhibition assay in a macrophage inflammation model.
[0147] The traditional Chinese medicine compositions prepared in Examples 1-10 and Comparative Examples 1-9 were tested as follows:
[0148] (1) Cytotoxicity assay: RAW264.7 cell suspension was adjusted to a concentration and added to 96-well cell plates. The cells were cultured overnight at 37°C with 5% CO2 for assay. The test samples were diluted with cell culture medium to different concentrations and added to cell plates. The cells were cultured at 37°C with 5% CO2 for 20-48 hours. The culture medium was discarded, the cells were washed 1-2 times with PBS, and MTT working solution was added for further culture. After culture, the culture medium was discarded, DMSO was added, and the cells were shaken to mix. The absorbance was measured at 570 nm (with 630 nm as the background). Cytotoxicity was calculated based on the results. Combined with cell morphology, the same concentration of the sample with no obvious cytotoxicity was selected for the next step of the experiment.
[0149] (2) IL-6 assay: RAW264.7 cell suspension was adjusted to a concentration and added to a 96-well cell plate. The cells were cultured overnight at 37°C with 5% CO2 for detection. The test samples were diluted with LPS-containing cell culture medium to a non-cytotoxic concentration before addition. LPS-containing medium served as the negative control (NC), and LPS-free cell culture medium served as the blank control (BC). Positive controls (PC, dexamethasone sodium phosphate) diluted with LPS-containing cell culture medium were used as positive controls. Cells were cultured for 20–24 hours after addition. After the assay, the supernatant was collected and detected according to the IL-6 ELISA kit procedure.
[0150] Result calculation and judgment:
[0151] The downregulation rate of the inflammatory factor IL-6 was calculated according to formula (Ⅰ):
[0152] Downward adjustment rate = (1-T / NC) × 100% (Ⅰ);
[0153] In formula (Ⅰ), T is the average value of IL-6, the inflammatory factor in the experimental group; NC is the average value of IL-6, the inflammatory factor in the negative control group.
[0154] Perform statistical and significance analysis on the data, calculate the P-value, P < 0.05 indicates a significant difference, otherwise there is no statistical difference.
[0155] When the IL-6 level in the negative control group was significantly higher than that in the blank control group (P < 0.05), the experiment was considered successful.
[0156] When the level of the inflammatory factor IL-6 in the sample group was lower than that in the negative control group, and the difference between the two was statistically significant (P < 0.05), the sample could be considered to have a soothing effect.
[0157] Table 1. Experimental results of the downregulation of inflammatory factor IL-6 by traditional Chinese medicine composition.
[0158]
[0159] In Table 1: If P > 0.05, it indicates no significant difference, denoted as "ns"; if P < 0.05, it indicates a significant difference, and if 0.01 < P ≤ 0.05, it is denoted as "*"; if 0.001 < P ≤ 0.01, it is denoted as "**"; if 0.0001 < P ≤ 0.001, it is denoted as "***"; if P ≤ 0.0001, it is denoted as "****".
[0160] The experimental results of the herbal compositions in Examples 1-10 and Comparative Examples 1-9 on the downregulation of the inflammatory factor IL-6 are shown in Table 1 above. BC is the experimental blank control, NC is the experimental negative control, and PC is the positive control. As shown in the table, the IL-6 content in the NC group was significantly higher than that in the blank control group (P < 0.05), indicating that the experiment was successful. The table also shows that when the same safe concentration of the samples from the examples and comparative examples was added, Example 5 showed the best effect, with a downregulation rate of 47.93% for the IL-6 inflammatory factor induced by exogenous stimulation, which was higher than the downregulation rate of the positive control PC, demonstrating a good inhibitory effect. Meanwhile, all the extracts from Examples 1-6, extracted using the preferred specific process parameters of this application, showed an IL-6 downregulation rate of over 30%, which was better than any comparative example (without flavor or with a different flavor), indicating the rationality of the formulation of these eight traditional Chinese medicines and their synergistic effect. Examples 7-10 used extraction parameters outside the specified process range, and while they still showed good inhibition of the inflammatory factor IL-6, the effect was weaker than that of Example 1 with the same formulation, indicating the rationality of the extraction process parameters. These results demonstrate that the traditional Chinese medicine composition with soothing and oil-controlling effects of this application can effectively inhibit the release of the inflammatory factor IL-6, effectively improve skin inflammation, and indirectly improve oil release, exhibiting a good soothing and oil-controlling effect in this pathway.
[0161] 2. Inhibition test of inflammatory factor IL-33.
[0162] IL-33 (Interleukin-33) is an important immunomodulatory cytokine that plays a key role in allergic diseases (such as asthma and atopic dermatitis), autoimmune diseases (such as rheumatoid arthritis), and chronic inflammation. Therefore, IL-33 inflammatory factors were measured in the examples and comparative samples to assess their soothing effects and evaluate the pro-inflammatory role of IL-33 in inhibiting excessive inflammation (such as allergic diseases and chronic inflammation).
[0163] Cytotoxicity assay: RAW264.7 cell suspension was adjusted to different concentrations and added to 96-well cell plates. The cells were incubated overnight at 37°C with 5% CO2 for assay. Test samples were diluted with cell culture medium to different concentrations and added to cell plates, then incubated at 37°C with 5% CO2 for 20–48 h. The culture medium was discarded, and the cells were washed 1–2 times with PBS. MTT working solution was added and the cells were incubated for further incubation. After incubation, the culture medium was discarded, DMSO was added, and the mixture was shaken to mix. The absorbance was measured at 570 nm (with a background of 630 nm). Cytotoxicity was calculated based on the results, and, combined with cell morphology analysis, concentrations of the same sample showing no significant cytotoxicity were selected for further experiments.
[0164] RAW 264.7 cells were used to determine IL-33 levels. Cell suspensions were adjusted to an appropriate concentration and seeded into 96-well plates, incubated overnight at 37°C with 5% CO2. The experiment included a sample group (containing LPS and the traditional Chinese medicine compositions of Examples 1-6 and Comparative Examples 1-6), a negative control (NC, containing LPS), a positive control (PC, containing tranilast and LPS), and a blank control (BC, without LPS). After 24 hours of treatment, the culture medium was slowly washed with PBS, and the cells were repeatedly freeze-thawed with added PBS. The supernatant was then aspirated, centrifuged, and the IL-33 level was detected using a double-antibody sandwich ELISA method: standards / samples, biotinylated detection antibody, HRP-labeled streptavidin, and TMB substrate were added sequentially. After color development, the absorbance at 450 nm was measured. The IL-33 inhibition rate was calculated using the formula: IL-33 inhibition rate = 1 - (sample OD - blank OD) / (NC - BC) × 100%. All experiments were performed in triplicate.
[0165] Table 2 shows the experimental results of the inhibition of the inflammatory factor IL-33 by the traditional Chinese medicine composition.
[0166]
[0167] In Table 2: If P > 0.05, it indicates no significant difference, denoted as "ns"; if P < 0.05, it indicates a significant difference, and if 0.01 < P ≤ 0.05, it is denoted as "*"; if 0.001 < P ≤ 0.01, it is denoted as "**"; if 0.0001 < P ≤ 0.001, it is denoted as "***"; if P ≤ 0.0001, it is denoted as "****".
[0168] The results of the experiments on the downregulation of the inflammatory factor IL-33 content by the traditional Chinese medicine compositions of Examples 1-10 and Comparative Examples 1-9 are shown in Table 2 above. Model validation showed that the intracellular IL-33 secretion level remained stable after repeated freeze-thaw stimulation with LPS, proving the successful modeling. The positive control drug tranilast showed a significant inhibition rate of 92.09%, further verifying the sensitivity of the model to drug response. As shown in the table, when the same safe concentration of the examples and comparative samples was added, Example 3 showed the best effect, with an inhibition rate of 95.69% against the IL-33 inflammatory factor, which was higher than that of the sample control PC. Moreover, the inhibition rates of IL-33 by Examples 1-6 prepared by the specific process of this invention were all above 85%, and the effects of Examples 1-6 were better than any comparative example (without flavor or with changed flavor), indicating that the composition composed of eight traditional Chinese medicines has a synergistic effect and can jointly promote the efficacy. At the same time, the effects of Examples 7-10 were weaker than those of Example 1, which again shows the rationality of the extraction process parameters. The above results indicate that the traditional Chinese medicine composition with soothing and oil-controlling effects of this application can effectively inhibit the release of inflammatory factor IL-33, effectively improve the pro-inflammatory effect of the skin, inhibit skin inflammation, and indirectly improve oil release, thus exhibiting good soothing and oil-controlling effects in this pathway.
[0169] 3. NO inhibition assay in a macrophage inflammation model.
[0170] The traditional Chinese medicine compositions prepared in Examples 1-10 and Comparative Examples 1-9 were tested as follows:
[0171] Cytotoxicity assay: RAW264.7 cell suspension was adjusted to different concentrations and added to 96-well cell plates. The cells were incubated overnight at 37°C with 5% CO2 for assay. Test samples were diluted with cell culture medium to different concentrations and added to cell plates, then incubated at 37°C with 5% CO2 for 20–48 h. The culture medium was discarded, and the cells were washed 1–2 times with PBS. MTT working solution was added, and the cells were incubated for further incubation. After incubation, the culture medium was discarded, DMSO was added, and the mixture was shaken to mix. The absorbance was measured at 570 nm. Cytotoxicity was calculated based on the results, and samples with no significant cytotoxicity were selected for further experiments, taking into account cell morphology.
[0172] NO release assay: RAW264.7 cell suspension was adjusted to a concentration and added to a 96-well cell plate. The cells were cultured overnight at 37°C with 5% CO2 for detection. The test samples were diluted with LPS-containing cell culture medium to a non-cytotoxic concentration before being added. LPS-containing medium served as the negative control (NC), and LPS-free cell culture medium served as the blank control (BC). Cells were cultured for 20–24 h after sample addition. After the reaction, 50 μl of culture medium was placed in a new cell plate, and an equal volume of Griess reagent was added. The mixture was thoroughly mixed and incubated in the dark for 10 min. The OD value was measured at 540 nm.
[0173] NO relative content (%) = OD sample / ODNC × 100%;
[0174] NO inhibition rate (%) = (ODNC - OD sample) / ODNC × 100%;
[0175] In the formula, OD sample refers to the mean OD value of the sample group, and ODNC is the mean OD value of the negative control group.
[0176] The experiment was considered valid when the relative NO content in the blank control group (BC group) was ≤50%. Statistical and significance analysis was performed using GraphPad Prism software, and the P-value was calculated. P < 0.05 indicated a significant difference. When P < 0.05 and the NO inhibition rate was ≥10%, the sample was considered to have a soothing effect.
[0177] Table 3. Experimental results of the inhibition of the inflammatory mediator NO by the traditional Chinese medicine composition.
[0178]
[0179] In Table 3: If P > 0.05, it indicates no significant difference, denoted as "ns"; if P < 0.05, it indicates a significant difference, and if 0.01 < P ≤ 0.05, it is denoted as "*"; if 0.001 < P ≤ 0.01, it is denoted as "**"; if 0.0001 < P ≤ 0.001, it is denoted as "***"; if P ≤ 0.0001, it is denoted as "****".
[0180] The inhibition rates of the herbal compositions in Examples 1-10 and Comparative Examples 1-9 against the inflammatory mediator NO are shown in Table 3. The experiment was considered successful when the relative NO content in the blank control group (BC group) was ≤50%. As shown in the table, Example 5 exhibited the best NO inhibition rate, reaching 74.58%. Furthermore, Examples 1-6, prepared using the specific process of this invention, all showed NO inhibition rates above 60%, demonstrating significant differences compared to the NC group (P < 0.05), indicating good inhibitory effects. Simultaneously, the NO inhibition rates of any of Examples 1-6 were better than those of the comparative examples (without flavor or with changed flavor), indicating that the compositions made from eight herbal medicines were more effective, with each herb synergistically enhancing the efficacy. Meanwhile, the effects of Examples 7-10 were weaker than that of Example 1, indicating that the compositions prepared using the specific process of this application were more effective, further demonstrating the rationality of the extraction process parameters. The above results indicate that the traditional Chinese medicine composition with soothing and oil-controlling effects of this application can effectively inhibit the release of the inflammatory mediator NO, effectively improve skin inflammation and itching, and indirectly inhibit sebum secretion. It has a good soothing and oil-controlling effect in this pathway.
[0181] 4. Human body oil control and soothing test.
[0182] Preparation of soothing and oil-controlling emulsion: The traditional Chinese medicine composition obtained in Example 5 was added to the formula to prepare the emulsion. Table 4 shows the emulsion formula containing the soothing and oil-controlling traditional Chinese medicine composition. The amount of each substance is expressed as a weight percentage.
[0183] Table 4. Formula for Soothing and Oil-Controlling Emulsion.
[0184]
[0185] Preparation method of soothing and oil-controlling emulsion: Mix and heat phase A to 75℃-85℃ until completely dissolved, then set aside; mix and heat phase B to 75℃-85℃ until fully dispersed; add phase A to phase B, homogenize and stir until evenly dispersed; cool to 55℃-65℃, then add phases C1 and C2 sequentially, stir evenly, and continue cooling; cool to below 45℃, then add phase D, stir evenly, and continue cooling to 38℃; stir evenly, and discharge after passing inspection.
[0186] To ensure the rationality of the experiment, a blank emulsion was also set up as a reference. The preparation method was the same as above, except that phase D was not added. The sample emulsion and the blank emulsion were used for inter-group control, and the testing method is as follows.
[0187] Experimental methods and principles: Multiple subjects used the test sample once to measure the average skin redness and skin oil content before and after use, and compared them with the control area to verify the improvement of the average skin redness and skin oil content after using the test sample.
[0188] Test method: Randomized, single-blind, inter-group controlled. After cleansing, an appropriate amount of the test sample (soothing oil-control lotion) was evenly applied to the skin on the left side of the face, and an appropriate amount of the control sample (blank lotion) was evenly applied to the skin on the right side of the face. The concentration of the test sample was (2.0±0.1) mg / cm² on the forehead. 2 The dosage is applied once. The soothing effect was evaluated by the average skin redness immediately after product application (15 minutes) before use, and the oil control effect was evaluated by the skin oil content after product application (4 hours and 8 hours) before use. The change rate of each test index in the sample area and the control area was compared. The number of participants was 15.
[0189] like Figure 1 As shown, after using the emulsion containing 1.0% soothing and oil-controlling traditional Chinese medicine composition, the average redness reduction rate of 15 volunteers was 18.24% after 15 minutes, which was much higher than the 0.79% in the blank group, and there was a significant difference between the groups (P<0.05), indicating that the composition has a good redness-reducing and soothing effect. Figure 2 The results show the skin oil content test results of 15 volunteers. The difference in skin oil content after 4 hours and 8 hours shows that the oil content in the control area increased by 166.00 μg / cm³ after both 4 and 8 hours.2 225.80 μg / cm 2 It is much higher than the 89.23 μg / cm² in the sample area. 2 124.60 μg / cm 2 The difference in skin oil content in the sample area decreased by 46.25% and 44.82% compared to the blank area, indicating that the soothing and oil-controlling lotion can effectively reduce the rate of skin oil growth and has excellent oil-controlling effect. These results demonstrate that the traditional Chinese medicine composition with soothing and oil-controlling effects of this application can effectively reduce skin redness and reduce skin oil growth when applied to cosmetics, exhibiting excellent soothing and oil-controlling effects.
[0190] III. Network pharmacology analysis and verification.
[0191] (1) Collection of potential active ingredients from plants in the soothing and oil-controlling formula.
[0192] Data retrieval and analysis were conducted using the Traditional Chinese Medicine Systems Pharmacology Database and Analysis Platform (TCMSP). Potential active ingredients from mulberry bark, houttuynia cordata, soapberry, arborvitae leaf, safflower, dictamnus dasycarpus bark, chrysanthemum, and Sichuan pepper were collected and screened using a dual screening threshold of oral bioavailability (OB) ≥30% and drug-likeness (DL) ≥0.18.
[0193] (2) Obtain a dataset of target points related to skin soothing and oil control.
[0194] Using the SwissTarget Prediction platform, 557 potential targets for the active ingredient in the composition were identified through screening and integration. Simultaneously, 1814 targets related to sensitive skin and 294 targets related to sebum were retrieved and screened from the GeneCards database. Venn diagrams were used to compare the intersections of the potential targets with the sensitive and sebum targets, revealing 262 common targets with sensitive skin and 51 common targets with skin sebum. Figure 3 ).
[0195] (3) Construct a protein-protein interaction network to identify the key targets of the effective components of traditional Chinese medicine.
[0196] Intersecting target points were imported into the STRING database for analysis, and network topology analysis and visualization were performed using Cytoscape 3.9.1 software. For example... Figure 4 , Figure 5By calculating topological parameters such as node degree and betweenness centrality using software, the importance of targets in the network was ranked. Ultimately, the top-ranking core targets for skin sensitivity were found to be AKT1, TP53, TNF, IL6, and INS, while the top-ranking core targets for skin sebum were PPARG, AKT1, TP53, TNF, IL6, INS, and ESR1. These targets can be preliminarily identified as key targets for regulating skin sensitivity and skin sebum by potential active ingredients for soothing and oil control.
[0197] (4) Enrichment analysis of core targets.
[0198] To systematically elucidate the molecular mechanisms related to the research objectives, functional enrichment analysis was performed on 262 co-expressed targets of skin sensitivity and 51 common targets related to skin sebum identified in the previous screening using the Metascape platform. The results showed that multiple Gene Ontology (GO) functional annotation entries were identified, which could be clearly divided into three modules according to functional categories: biological processes (BP), cellular components (CC), and molecular functions (MF). To further focus on core functional information, the significance level of the enrichment results was used as the screening criterion, and the top 10 highly significant functional entries in the three categories of BP, CC, and MF were finally selected and visualized using charts (…). Figure 6 , Figure 7 This visually displays each item and its enrichment level, providing key functional evidence for further in-depth analysis of molecular mechanisms.
[0199] KEGG pathway enrichment analysis results revealed (e.g.) Figure 8 , Figure 9 The composition may regulate key signaling pathways through multiple targets, thereby clarifying the specific signaling pathways and potential mechanisms of action involved in its soothing and oil-controlling effects. The study identified multiple significantly enriched signaling pathways (P<0.05), which, through multiple pathways, influence the release of inflammatory factors, excessive sebum secretion, and abnormal barrier damage, collectively exerting skin soothing and oil-controlling effects.
[0200] The technical features of the above-described embodiments and examples can be combined in any suitable manner. For the sake of brevity, not all possible combinations of the technical features in the above-described embodiments and examples 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.
[0201] The embodiments described above merely illustrate several implementation methods of this application and should not be construed as limiting the scope of the patent application. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of this application, and these all fall within the protection scope of this application. Furthermore, it should be understood that after reading the above teachings, those skilled in the art can make various alterations or modifications to this application, and the equivalent forms obtained also fall within the protection scope of this application. It should also be understood that technical solutions obtained by those skilled in the art based on the technical solutions provided in this application through logical analysis, reasoning, or limited experimentation are all within the protection scope of the appended claims. Therefore, the protection scope of this patent application should be determined by the appended claims, and the specification can be used to interpret the content of the claims.
Claims
1. A method for preparing a skin-care herbal composition with soothing and oil-controlling effects, characterized in that, Includes the following steps: Weigh the following raw materials in the indicated weight proportions: 1-50 parts of mulberry bark, 1-50 parts of houttuynia cordata, 1-50 parts of soapberry, 1-50 parts of arborvitae leaf, 1-50 parts of safflower, 1-40 parts of dictamnus dasycarpus bark, 1-40 parts of chrysanthemum, and 1-40 parts of Sichuan pepper. Grind each raw material separately, sieve, and mix the resulting powders to obtain fine powder of traditional Chinese medicine. The fine powder of the traditional Chinese medicine, water, and enzyme are mixed. The resulting mixture is enzymatically hydrolyzed at a first temperature for a first time, and then enzymatically hydrolyzed at a second temperature for a second time. The mixture is then filtered to obtain a first filtrate and a first filter residue. The enzyme composition includes at least one of cellulase, pectinase, or protease. The first filter residue is mixed with an extraction solvent. The resulting mixture is ultrasonically treated at a third temperature for a third time, and then filtered to obtain a second filtrate and a second filter residue. The extraction solvent includes water and ethanol. The first filtrate and the second filtrate are combined to obtain an extract. The first temperature is 40℃-70℃, and the first time is 1h-3h. The second temperature is 80℃-90℃, and the second time is 10min-20min. The third temperature is 0℃-80℃, and the third time is 0.5h-4h. The extract is concentrated until the weight ratio of the concentrate to the fine powder of the traditional Chinese medicine is 0.8-1.
2. The concentrated extract is then settled at a fourth temperature, centrifuged, and the supernatant is collected. The fourth temperature is 0℃-4℃. The supernatant is filtered through a membrane, and the filtrate is concentrated until the weight ratio of the concentrated liquid to the fine powder of the traditional Chinese medicine is 0.1-0.
5. The concentrated supernatant is then dried with excipients to obtain the skin care traditional Chinese medicine composition with soothing and oil-controlling effects.
2. The preparation method according to claim 1, characterized in that, The power of ultrasound ranges from 50W to 1500W, and the frequency ranges from 10kHz to 40kHz.
3. The preparation method according to claim 1, characterized in that, The enzyme is added at a rate of 3000 U / g to 5000 U / g relative to the fine powder of the traditional Chinese medicine.
4. The preparation method according to claim 1, characterized in that, The weight-to-volume ratio of the first filter residue to the extraction solvent is 1:10-1:30 g / mL.
5. The preparation method according to any one of claims 1-4, characterized in that, At least one of the following conditions must be met: (1) The mesh size of the sieve is 40-60 mesh; (2) In the step of concentrating the extract, the extract is concentrated under the conditions of pressure of 2kPa-20kPa and temperature of 40℃-70℃; (3) In the step of concentrating the supernatant, the supernatant is concentrated under the conditions of pressure of 2kPa-20kPa and temperature of 40℃-70℃; (4) The settling time is 5h-20h; (5) The centrifugation speed is 5000 r / min-20000 r / min; (6) The membrane used for membrane filtration includes a microfiltration membrane with a pore size of 0.1 μm-3 μm.
6. The preparation method according to any one of claims 1-4, characterized in that, In the step of drying the concentrated supernatant, the concentrated supernatant is spray-dried or freeze-dried. Optionally, the spray drying conditions include: an inlet temperature of 100℃-130℃ and an outlet temperature of 50℃-80℃. Optionally, the freeze-drying conditions include: a pre-freezing temperature of -20°C to -80°C and a pre-freezing time of 3h to 8h; a sublimation pressure of 0Pa to 100Pa and a sublimation time of 10h to 30h.
7. The preparation method according to any one of claims 1-4, characterized in that, The excipients are in the form of 1-20 parts by weight.
8. The preparation method according to claim 7, characterized in that, The excipients include at least one of starch and maltodextrin.
9. A skincare herbal composition with soothing and oil-controlling effects, characterized in that, It is prepared by the preparation method according to any one of claims 1-8.
10. The use of the skin care traditional Chinese medicine composition with soothing and oil-controlling effects prepared by the preparation method according to any one of claims 1-8 in the preparation of cosmetics.
Citation Information
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