A soothing, oil-controlling composition and its preparation method and application

Abstract

This invention discloses a soothing and oil-controlling composition, its preparation method, and its application. The aim is to provide a composition that effectively increases bioavailability, promotes skin penetration of baicalin, reduces the dosage of baicalin, and possesses soothing and oil-controlling properties. It also provides a method for preparing the extract of the composition that improves extraction rate, promotes mutual solubility, is easily implemented on a production line, facilitates large-scale production, and produces a high-clarity and highly stable extract. The technical solution includes 150-200 parts of Scutellaria baicalensis and 40-80 parts of Corydalis yanhusuo; it belongs to the field of cosmetic technology.

Description

Technical Field

[0001] This invention discloses a plant-based composition, specifically a composition with soothing and oil-controlling properties. This invention also discloses a method for preparing the composition and its application, belonging to the field of cosmetic technology. Background Technology

[0002] Scutellaria baicalensis is a plant in the Lamiaceae family, and it is listed in the Chinese Pharmacopoeia and widely used. However, other plants in the same family and genus are also included in the local medicinal material standards. Among them, Scutellaria amoena CHWright is more widely used. Scutellaria amoena CHWright is the dried root of a plant in the Scutellaria genus of the Lamiaceae family. It is a traditional medicinal material from Yunnan Province with a long history of medicinal use and is a medicinal resource for ethnic minorities such as the Yi, Bai, Naxi, Lisu, and Tibetan.

[0003] The main active ingredient in Scutellaria baicalensis is baicalin, along with a large amount of flavonoids and saponins. It not only controls oil and soothes the skin, absorbs ultraviolet rays, and scavenges oxygen free radicals, but also inhibits melanin production. Furthermore, reports have confirmed that the antibacterial effect of Scutellaria baicalensis is significantly superior to that of commonly cultivated Scutellaria baicalensis. In cosmetics, it is an excellent functional cosmetic ingredient; however, because baicalin belongs to the flavonoid glycoside class of compounds, the presence of glycosyl groups in its molecular structure results in poor water and fat solubility, poor absorption, and low bioavailability, thus limiting its application in cosmetics.

[0004] Therefore, the extraction of Scutellaria baicalensis and its application in cosmetics have always been a research hotspot. Currently, the main extraction methods for Scutellaria baicalensis include solvent extraction, ultrasound-assisted extraction, and microwave-assisted extraction. Solvent extraction methods include boiling water, alkaline water, and enzyme or ultrasound extraction; ethanol extraction mainly uses 50%-70% ethanol reflux extraction or microwave-assisted extraction. Water-based extraction methods are safe, environmentally friendly, and inexpensive, but the low solubility of baicalin in water leads to low extraction rates and bioavailability. Enzymatic hydrolysis, ultrasound-assisted extraction, or microwave-assisted extraction can improve the extraction rate, but the recovery rate of baicalin remains low, and the purchase of ultrasound and microwave-assisted extraction equipment is required, which is not conducive to industrial production. Ethanol reflux extraction, ultrasound, or microwave-assisted extraction can improve the extraction rate of baicalin, but ethanol as an extraction solvent is expensive, has high recovery losses, and poses certain risks.

[0005] CN103044507A discloses a method for preparing high-purity baicalin, mainly employing enzymatic hydrolysis and ultrasonic countercurrent extraction technology, using ethanol as a solvent to first obtain an extract, and then recrystallizing it using polyamide-macroporous resin coupling technology to obtain baicalin, achieving a purity of over 98.3%. However, this method is cumbersome, relatively costly, and time-consuming to recrystallize, making it unsuitable for large-scale industrial production. Zhou Fang et al., in their "Optimization of Baicalin Preparation Process," *Hubei Agricultural Sciences*, November 2006, Vol. 45, No. 6, reported an alcohol extraction, acid precipitation, and ethanol recrystallization process. This process involves alcohol extraction of baicalin from Yunnan, followed by acid precipitation and recrystallization with 95% ethanol, achieving a baicalin content (HPLC content) of 86.14% in the extract. However, this method requires a large amount of ethanol for extraction and recrystallization, posing safety risks for large-scale production.

[0006] Therefore, it is particularly necessary to develop a compound composition that can improve the bioactivity of Scutellaria baicalensis, promote the solubility of baicalin, increase the stability and bioavailability of baicalin, reduce the dosage of baicalin, effectively increase solubility and stability, and be easy to mass-produce on a production line, and also have soothing and oil-controlling effects. Summary of the Invention

[0007] The purpose of this invention is to provide a composition that can effectively increase bioavailability, promote the skin penetration of baicalin, reduce the dosage of baicalin, and has soothing and oil-controlling properties.

[0008] The second objective of this invention is to provide a method for preparing a composite extract that can improve extraction rate, promote mutual solubility, is easy to implement on a production line, facilitates large-scale production, and produces a high-clarity and highly stable extract.

[0009] A third objective of this invention is to provide the above-described soothing and oil-controlling composition as a cosmetic additive.

[0010] Therefore, the first technical solution provided by this invention is as follows:

[0011] A composition with soothing and oil-controlling properties, comprising the following components in parts by weight: 150-200 parts of Scutellaria baicalensis and 40-80 parts of Corydalis yanhusuo.

[0012] Furthermore, the above-mentioned soothing and oil-controlling composition also includes 120-200 parts of polyol.

[0013] Furthermore, the above-mentioned soothing and oil-controlling composition also includes 1-10 parts of sodium citrate.

[0014] The second technical solution provided by this invention is a method for preparing the above-mentioned composition with soothing and oil-controlling properties, which includes the following steps in sequence:

[0015] 1) Weigh each component, add 10 to 30 times the total weight of Scutellaria baicalensis and Corydalis yanhusuo in pure water and soak for 30 to 60 minutes. Extract at 85℃ with stirring 1 to 2 times, each time for 1 to 2 hours. Filter the extract and mix them. Let the filtrate stand for 12 hours before use.

[0016] 2) Add 8 to 20 times the total mass of pure water to the residue from step 1), boil and stir to extract 1 to 2 times, each extraction lasting 1 to 2 hours. After filtering the extract, mix the two filtrates and concentrate under reduced pressure at 0.08 to 0.09 MPa and 60 to 70°C to obtain a clear extract with a raw medicinal material concentration of 0.2 to 0.5 g / ml.

[0017] 3) After activating the macroporous resin, wet pack it into a column, collect and combine the eluent, and set aside for later use;

[0018] 4) Concentrate the eluent collected in step 3) under reduced pressure (0.08–0.09 MPa, 60–70°C) to recover alcohol and concentrate to a crude drug concentration of 1 g / ml. Add polyol and sodium citrate to adjust the pH to 4.5–7.0. Add pure water to bring the crude drug concentration to 0.2–0.5 g / ml. Stir and heat to 80°C, hold for 15–30 min. Centrifuge the reconstituted solution at 15,000–17,000 r / min. Filter the resulting centrifuged solution through a 0.2 μm membrane to obtain the final product.

[0019] Furthermore, in the preparation method of the above-mentioned composition with soothing and oil-controlling properties, the filtration in steps 1) and 2) uses a 300-mesh filter cloth.

[0020] Furthermore, in the preparation method of the above-mentioned composition with soothing and oil-controlling properties, the macroporous resin activation treatment method is to soak the resin in 3-4 BV of 95% ethanol for 12 hours, pack the column using a wet method, and wash with 95% ethanol. The washing endpoint is when there is no turbidity when the ethanol and pure water are mixed in equal proportions after washing. Then, the resin is washed with pure water until there is no alcohol odor.

[0021] Furthermore, in the preparation method of the above-mentioned composition with soothing and oil-controlling properties, the sample loading flow rate is 1-3 BV / h when packing the macroporous resin column by wet method; after the sample loading is completed, the column is rinsed with 4-8 BV of pure water at a flow rate of 1-4 BV / h; elution is carried out with 5-12 BV of 40%-80% ethanol at a flow rate of 1-4 BV / h, and the eluent is collected and combined for later use.

[0022] Furthermore, in the preparation method of the above-mentioned composition with soothing and oil-controlling properties, the pH value in step 4) is adjusted using sodium citrate.

[0023] The final technical solution provided by this invention is the application of the above-mentioned soothing and oil-controlling composition as a cosmetic additive.

[0024] Furthermore, the above-mentioned soothing and oil-controlling composition is used as a cosmetic additive, wherein the cosmetic is in the form of an essence or spray.

[0025] Furthermore, in the application of the above-mentioned soothing and oil-controlling composition as a cosmetic additive, the amount of the soothing and oil-controlling composition added is 0.1wt%-20wt%.

[0026] Compared with existing methods, the present invention has the following advantages and beneficial effects:

[0027] 1. The technical solution provided by this invention adopts a compound formulation of Scutellaria baicalensis and Corydalis yanhusuo, which can increase bioavailability. The permeability of Corydalis A and B can reduce the dosage of baicalin. Corydalis B, as an alkaloid, can promote the solubility of baicalin in water and also increase the stability of Scutellaria baicalensis.

[0028] 2. The technical solution provided by this invention also includes sodium citrate, which can effectively promote the skin penetration of baicalin; the Scutellaria baicalensis-Corydalis yanhusuo-citric acid buffer system mutually solubilizes each other, effectively increasing solubility and stability.

[0029] 3. The technical solution provided by this invention adopts a solubilization extraction method for corydaline, which results in a high extraction rate of the target active ingredient and also increases its stability. The boiling water extraction process, vacuum concentration, macroporous resin purification, and polymer membrane filtration system are easy to implement on the production line, which is conducive to large-scale production. At the same time, the output composition extract has high clarity and high stability.

[0030] 4. The technical solution provided by this invention is safe and non-irritating, with no toxic side effects, avoiding allergic reactions during use; it can effectively inhibit the production of inflammatory factors NO and TNF-α, playing an anti-inflammatory and soothing role, and can also play a certain role in inhibiting sebum secretion, and can be used in multi-dosage cosmetic formulations. Specific implementation methods

[0031] The present invention will be further described in detail below with reference to embodiments, but the embodiments of the present invention are not limited thereto.

[0032] Example 1

[0033] The present invention provides a composition with soothing and oil-controlling properties, comprising the following raw materials by weight: 200g of Scutellaria baicalensis and 80g of Corydalis yanhusuo.

[0034] The preparation method of the above-mentioned soothing and oil-controlling composition includes the following steps in sequence:

[0035] 1) Weigh the raw materials, add 20 times the total mass of pure water and soak for 40 minutes. Extract twice at 85℃, each time for 2 hours. Pass the extract through a 300-mesh filter cloth. Mix the filtrates and let the filtrate stand for 12 hours before use.

[0036] 2) Add 12 times the total mass of pure water to the residue from step 1), boil and stir to extract twice, each time for 1.5 hours. Pass the extract through a 300-mesh filter cloth each time. Mix the filtrates and concentrate under reduced pressure at 60℃, with the pressure controlled at 0.09Mpa, until the concentration of raw medicinal material is 0.5g / ml (60-70℃) to obtain a clear extract with appropriate viscosity.

[0037] 3) Select macroporous resin, purify the concentrated extract, and calculate the resin amount based on the adsorption capacity of the macroporous adsorption resin for baicalin. Before use, the macroporous resin should be activated by soaking it in 3 BV of 95% ethanol for 12 hours, followed by wet packing. Wash with 95% ethanol until the ethanol and pure water are mixed in equal proportions and no longer cause turbidity. Elute the resin with pure water until no alcohol odor remains. For wet packing of the macroporous resin, the sample loading flow rate is 3 BV / h. After loading, wash the column with 8 BV of pure water at a flow rate of 1 BV / h; elute with 12 BV of 40% ethanol at a flow rate of 1 BV / h. Collect and combine the eluent for later use.

[0038] 4) Concentrate the eluent collected in step 3) under reduced pressure at 60°C, with the pressure controlled at 0.09 MPa. Recover the alcohol and concentrate the extract to a crude drug concentration of 1 g / ml. Add 280 g of polyol and adjust the pH to 7.0 with 3 g of sodium citrate. Add water to a final volume of 0.5 g / ml, stir, and heat to 80°C. Keep warm for 15 min. Pass the reconstituted solution through a tubular centrifuge at 15000 r / min. Pass the resulting centrifuged liquid through a 0.2 μm membrane to obtain the final product.

[0039] Example 2

[0040] The present invention provides a composition with soothing and oil-controlling properties, comprising the following raw materials by weight: 150g of Scutellaria baicalensis and 80g of Corydalis yanhusuo.

[0041] The preparation method of the above-mentioned soothing and oil-controlling composition includes the following steps in sequence:

[0042] 1) Weigh the raw materials, add 15 times the total mass of pure water and soak for 60 minutes. Extract twice at 85℃, each time for 1.5 hours. Pass the extract through a 300-mesh filter cloth each time. Mix the filtrates and let the filtrate stand for 12 hours before use.

[0043] 2) Add 12 times the total mass of pure water to the residue from step 1), boil and stir to extract once, each extraction lasting 2 hours. Pass the extract through a 300-mesh filter cloth each time. Mix the filtrates and concentrate under reduced pressure at 70℃, with the pressure controlled at 0.08 MPa, until the concentration of raw medicinal materials is 0.2-0.5 g / ml (60-70℃) to obtain a clear extract with appropriate viscosity.

[0044] 3) Select macroporous resin, purify the concentrated extract, and calculate the resin amount based on the adsorption capacity of the macroporous adsorption resin for baicalin. Before use, the macroporous resin should be activated by soaking it in 3 BV of 95% ethanol for 12 hours, followed by wet packing. Wash with 95% ethanol until the ethanol and pure water are mixed in equal proportions and no longer cause turbidity. Elute the resin with pure water until no alcohol odor remains. For wet packing of the macroporous resin, the sample loading flow rate is 3 BV / h. After loading, wash the column with 8 BV of pure water at a flow rate of 1 BV / h. Elute with 12 BV of 40%-80% ethanol at a flow rate of 1 BV / h. Collect and combine the eluent for later use.

[0045] 4) Concentrate the eluent collected in step 3) under reduced pressure at 70°C, with the pressure controlled at 0.08 MPa. Recover the alcohol and concentrate the extract until the concentration of the raw medicinal material is 1 g / ml. Add 287.5 g of polyol and adjust the pH to 6.0 with 2 g of sodium citrate. Add water to bring the volume up to 0.4 g / ml of medicinal material. Stir and heat to 80°C, keep warm for 20 min. Pass the reconstituted solution through a tubular centrifuge at 17000 r / min. Pass the resulting centrifuged liquid through a 0.2 μm membrane to obtain the final product.

[0046] Example 3

[0047] The present invention provides a composition with soothing and oil-controlling properties, comprising the following raw materials by weight: 200g of Scutellaria baicalensis and 40g of Corydalis yanhusuo.

[0048] The preparation method of the above-mentioned soothing and oil-controlling composition includes the following steps in sequence:

[0049] 1) Weigh the raw materials, add 15 times the total mass of pure water and soak for 50 minutes. Extract once at 85℃ with stirring, each extraction lasting 2 hours. Pass the extract through a 300-mesh filter cloth each time. Mix the filtrates and let the filtrate stand for 12 hours before use.

[0050] 2) Add 15 times the total mass of pure water to the residue from step 1), boil and stir to extract twice, each time for 1 hour. Pass the extract through a 300-mesh filter cloth each time. Mix the filtrates and concentrate under reduced pressure at 65℃, with the pressure controlled at 0.08Mpa, until the concentration of raw medicinal material is 0.3g / ml (60-70℃) to obtain a clear extract with appropriate viscosity.

[0051] 3) Select macroporous resin, purify the concentrated extract, and calculate the resin amount based on the adsorption capacity of the macroporous adsorption resin for baicalin. Before use, the macroporous resin should be activated by soaking it in 4 BV of 95% ethanol for 12 hours, followed by wet packing. Wash with 95% ethanol until the ethanol and pure water are mixed in equal proportions and no longer cause turbidity. Elute the resin with pure water until no alcohol odor remains. When wet packing the macroporous resin, the sample loading flow rate is 2 BV / h. After loading, wash the column with 4–8 BV of pure water at a flow rate of 3 BV / h; elute with 8 BV of 60% ethanol at a flow rate of 3 BV / h. Collect and combine the eluent for later use.

[0052] 4) Concentrate the eluent collected in step 3) under reduced pressure at 68℃, with the pressure controlled at 0.08 MPa. Recover the alcohol and concentrate the extract to a crude drug concentration of 1 g / ml. Add 400 g of polyol and adjust the pH to 5.0 with 2.2 g of sodium citrate. Add water to bring the volume to 0.3 g / ml of medicinal material. Stir and heat to 80℃, keep warm for 20 min. Pass the reconstituted solution through a tubular centrifuge at 16000 r / min. Pass the resulting centrifuged liquid through a 0.2 μm membrane to obtain the final product.

[0053] Example 4

[0054] The present invention provides a composition with soothing and oil-controlling properties, comprising the following raw materials by weight: 150g of Scutellaria baicalensis and 40g of Corydalis yanhusuo.

[0055] The preparation method of the above-mentioned soothing and oil-controlling composition includes the following steps in sequence:

[0056] 1) Weigh the raw materials, add 20 times the total mass of pure water and soak for 45 minutes. Extract twice at 85℃, each time for 2 hours. Pass the extract through a 300-mesh filter cloth each time. Mix the filtrates and let the filtrate stand for 12 hours before use.

[0057] 2) Add 15 times the total mass of pure water to the residue from step 1), boil and stir to extract twice, each time for 2 hours. Pass the extract through a 300-mesh filter cloth each time. Mix the filtrates and concentrate under reduced pressure at 65℃, with the pressure controlled at 0.09Mpa, until the concentration of raw medicinal material is 0.4g / ml (60-70℃) to obtain a clear extract with appropriate viscosity.

[0058] 3) Select a macroporous resin to purify the extract concentrate. Calculate the resin amount based on the adsorption capacity of the macroporous adsorption resin for baicalin. Before use, the macroporous resin should be activated by soaking it in 3.5 BV of 95% ethanol for 12 hours, followed by wet packing. Wash with 95% ethanol until the ethanol and pure water are mixed in equal proportions without turbidity. Elute the resin with pure water until there is no alcohol odor. The sample loading flow rate for wet packing of the macroporous resin is 2 BV / h. After loading, wash the column with 6 BV of pure water at a flow rate of 2 BV / Pa. Elute with 8 BV of 60% ethanol at a flow rate of 2 BV / h. Collect and combine the eluent for later use.

[0059] 4) Concentrate the eluent collected in step 3) under reduced pressure at 65°C, with the pressure controlled at 0.08 MPa. Recover the alcohol and concentrate the extract until the concentration of the raw medicinal material is 1 g / ml. Add 475 g of polyol and adjust the pH to 5.0 with 1.7 g of sodium citrate. Add water to bring the volume up to 0.2 g / ml of medicinal material. Stir and heat to 80°C, and keep warm for 25 min. Pass the reconstituted solution through a tubular centrifuge at 16000 r / min. Pass the resulting centrifuged liquid through a 0.2 μm membrane to obtain the final product.

[0060] Example 5

[0061] This embodiment provides an essence with a soothing and oil-controlling composition, comprising the following components by weight: 0.04g disodium EDTA, 0.10g allantoin, 0.2g hydroxyethyl cellulose, 2g glycerin, 0.05g menthol, 2g ethanol, 10g of the soothing and oil-controlling composition provided in Example 1, 0.2g fragrance, 3g propylene glycol, 0.4g PEG-40 hydrogenated castor oil, 0.1g SebumBate deep fat-suppressing agent, 2g Senplant MALT hydrogenated starch hydrolysate, 8g Runsoft PGP cocamidopropyl PG-dimethylammonium chloride phosphate sodium, 0.08g citric acid, 0.2% phenoxyethanol, and the remainder being deionized water.

[0062] Example 6

[0063] This embodiment provides an essence with a soothing and oil-controlling composition, comprising the following components by weight: 0.08g disodium EDTA, 0.05g allantoin, 0.1g hydroxyethyl cellulose, 3g glycerin, 0.03g menthol, 5g ethanol, 15g of the soothing and oil-controlling composition provided in Example 2, 0.1g fragrance, 6g propylene glycol, 0.3g PEG-40 hydrogenated castor oil, 0.1g SebumBate deep fat-inhibiting agent, 2g Senplant MALT hydrogenated starch hydrolysate, 25g Runsoft PGP cocamidopropyl PG-dimethylammonium chloride phosphate sodium, 0.03g citric acid, 0.2% phenoxyethanol, and the remainder being deionized water.

[0064] Example 7

[0065] This embodiment provides an essence with a soothing and oil-controlling composition, comprising the following components by weight: 0.03g disodium EDTA, 0.15g allantoin, 0.5g hydroxyethyl cellulose, 1g glycerin, 0.08g menthol, 1g ethanol, 20g of the soothing and oil-controlling composition provided in Example 4, 0.3g fragrance, 2g propylene glycol, 0.9g PEG-40 hydrogenated castor oil, 0.1g SebumBate deep fat-suppressing agent, 6g Senplant MALT hydrogenated starch hydrolysate, 10g Runsoft PGP cocamidopropyl PG-dimethylammonium chloride phosphate sodium, 0.05g citric acid, 1% phenoxyethanol, and the remainder being deionized water.

[0066] The processes in Examples 5 to 7:

[0067] Add water, disodium EDTA, and allantoin to an emulsifying pot and heat to 70-75°C. Add the evenly dispersed hydroxyethyl cellulose and glycerin, and stir until dissolved into a clear liquid. Continue stirring and cool to 40-45°C. Add menthol and alcohol (phase 1); fragrance (phase 2); PEG-40 hydrogenated castor oil; phenoxyethanol; propylene glycol; skin feel modifier; pH adjuster (citric acid); and 10-30% of Example 1 in sequence. Stir for 10-15 minutes and adjust the pH to 5.5-6.0 (1:9 dilution). After the mixture is evenly mixed, filter and discharge.

[0068] To better demonstrate the development process and effects of the compositions provided in this application, comparative examples from the development process of this application are given below:

[0069] Comparative Example 1

[0070] 200g of Scutellaria baicalensis.

[0071] Comparative Example 2

[0072] Corydalis 80g

[0073] The preparation processes and parameters in Comparative Examples 1 and 2 are the same as those in Examples 1-4, and the missing components do not need to be added.

[0074] Comparative Example 3

[0075] Scutellaria baicalensis 200g, Corydalis yanhusuo 80g.

[0076] Its preparation method is as follows:

[0077] 1) Take the raw material of Scutellaria baicalensis, pulverize it, add 10 times the total amount of 60% ethanol, and extract it three times by reflux in an 80℃ water bath, 2 hours each time. Combine the extracts, concentrate under reduced pressure, and make up to 0.05 g / mL. Take the concentrated extract and perform an acid precipitation test. The acid precipitation temperature is 80℃, the solution pH is 1, and the incubation time is 60 min. Wash the obtained precipitate repeatedly with water until it is colorless, and set aside for later use.

[0078] 2) Crush the medicinal material Corydalis rhizome into powder, add 10 times the total volume of 60% ethanol, and extract three times by reflux in an 80℃ water bath, 2 hours each time. Combine the extracts, concentrate under reduced pressure, and bring the volume to 0.05 g / mL. Perform an acid-base precipitation test on the above extract concentrate. Add 10% glacial acetic acid to the concentrate, stir for 10 min, centrifuge to remove impurities, add NaOH to adjust the pH to greater than 9, let stand for 2 hours, centrifuge to collect the precipitate, wash the precipitate with water until colorless, and set aside.

[0079] 3) Mix the two precipitates with water, polyol, and sodium citrate to a concentration of 1 g / mL (crude drug concentration), and filter through a 0.22-micron filter membrane to obtain the final product.

[0080] Comparative Example 4

[0081] Scutellaria baicalensis 150g, Corydalis yanhusuo 40g.

[0082] Its preparation process includes the following steps:

[0083] Take the coarse powder of the medicinal material (10 mesh), soak it in 12 times the amount of water at 60℃ for 30 minutes, heat it to boiling, reflux and extract for 1 hour, extract twice, filter through a 300-mesh filter cloth, and combine the filtrates; concentrate the filtrate under reduced pressure to 0.5 g / mL, add flocculant to it, keep it warm and let it settle overnight, centrifuge to remove the precipitate, and filter it through a membrane of 0.22 microns to obtain the final product.

[0084] Comparative Example 5: 200g of Scutellaria baicalensis and 90g of Corydalis yanhusuo.

[0085] Comparative Example 6: Scutellaria baicalensis 50g, Corydalis yanhusuo 100g.

[0086] The preparation processes and parameters in Comparative Examples 5 and 6 are the same as those in Examples 1-4.

[0087] The following are the embodiments provided in this application and their comparative experimental data:

[0088] 1. Comparison of active ingredient content detection

[0089] The total corydaline and baicalin content in the extract were detected according to the pharmacopoeia method, and the percentage content in the extract was analyzed.

[0090] Group Total amount of corydaline (%) Baicalin content (%) Total active ingredient (%) Example 1 2.67 5.2 7.87 Example 2 2.13 4.57 6.7 Example 3 2.38 4.97 7.35 Example 4 2.26 4.84 7.1 Comparative Example 1 0 2.56 2.56 Comparative Example 2 1.34 0 1.34 Comparative Example 3 1.29 3.6 4.89 Comparative Example 4 1.45 2.68 4.13 Comparative Example 5 1.71 3.01 4.72 Comparative Example 6 1.52 2.95 4.47

[0091] As can be seen from the percentage of active ingredients, the contents of corydaline and baicalin in the examples are relatively balanced, with the content of active ingredients exceeding 6.7% in both cases. In contrast, the total content of active ingredients in the single-ingredient extracts (Comparative Examples 1 and 2) prepared using the same process is less than 5%. This indicates that the combination of Scutellaria baicalensis and Corydalis yanhusuo can effectively extract and solubilize the active ingredients in the two plants. This combination has a significant technical advantage in enriching active ingredients. Comparative Examples 3 and 4 were prepared using other processes, and their active ingredient contents were lower than those in Examples 1 and 4, indicating that this technology is superior to other conventional processes. Furthermore, Comparative Examples 5 and 6 also used this process, but their proportion of medicinal materials exceeded the range of this composition. However, their active ingredient contents were also lower than those in the examples, indicating that the active ingredients within this range can synergistically solubilize and improve purity.

[0092] 2. Comparison of solubility and stability of active ingredients

[0093] The extract was subjected to heat resistance tests at 60℃ and cold resistance tests at 5℃, and the stability of the sample was observed.

[0094] Table 2. Solubility and stability test results

[0095]

[0096]

[0097] Results Analysis: Examples 1-2 showed stability under heat resistance conditions of 60℃ and cold resistance conditions of 5℃, indicating that the combination of Scutellaria baicalensis and Corydalis yanhusuo exhibits better solubility and stability. Comparative Examples 1-2 showed discoloration in Comparative Example 1 and precipitation in Comparative Example 2, indicating that individual extraction of either herb would result in instability such as discoloration or precipitation; combined extraction increases stability and solubility. Comparative Examples 3-4 showed precipitation at 5℃, indicating that although Scutellaria baicalensis and Corydalis yanhusuo were within the combined range, different processing methods still affected their solubility. Comparative Examples 5-6 showed discoloration and precipitation; although the extraction processes for Scutellaria baicalensis and Corydalis yanhusuo were the same, different ratios also affected their stability and solubility. This indicates that the process and component weight ratios provided by this invention represent optimal conditions, exhibiting the best anti-stability and solubility effects within these conditions.

[0098] 3. Comparison of the anti-inflammatory effects of active ingredients

[0099] After culturing RAW264.7 cells, the cells were diluted to 1×10⁻⁶. 4 Cells were seeded in 24-well plates at a concentration of 100 ng / ml and cultured for 24 hours. A blank control group (without LPS or sample) and all other groups were treated with LPS to induce inflammatory cytokines production. Samples were then added, and after co-culturing for another 24 hours, the cell supernatant was collected for TNF-α and NO detection.

[0100]

[0101]

[0102] Results analysis showed that Examples 1-4 all exhibited good inhibitory effects on NO and TNF-α secretion, with inhibition rates all exceeding 89%. Example 1 showed the best effect, reaching 97.67%, indicating that Examples 1-4 had better soothing and anti-inflammatory effects. Comparative Examples 1-2 showed significantly lower inhibition rates of NO and TNF-α, with Comparative Example 1 showing better inhibition, suggesting that the anti-inflammatory effect may be primarily due to Scutellaria baicalensis, with Corydalis yanhusuo playing a supporting role. Comparative Examples 3-6 showed lower inhibition rates of NO and TNF-α. The extraction and purification process and the weight ratio of each component provided by this invention represent optimal conditions, under which the in vitro anti-inflammatory effect is better.

[0103] 4. Comparison of cell experiments on oil control by active ingredients (experiment on sebaceous gland cell inhibition of sebum secretion)

[0104] Brief description of the testing method

[0105] Sebaceous glands are organs that secrete sebum. SZ95 cells can produce triglycerides, while Oil Red O is an azo dye, a strong lipid solvent and staining agent. It can dissolve lipids in tissues and cells and binds with triglycerides to form small orange-red lipid droplets. After being dissolved in isopropanol, the OD value can be read at a wavelength of 500nm for quantitative analysis of the triglyceride content. At the same time, the amount of Oil Red stained particles can be directly observed under a microscope to evaluate the lipid inhibition effect of the raw material.

[0106] The number of immortalized human sebaceous gland SZ95 cells was adjusted to 3×10 4 Cells were seeded at a concentration of 1 / mL into 24-well plates, 1 mL per well, and incubated for 24 h. After discarding the original culture medium, 1 mL of complete culture medium was added to each well, along with 1 mL of complete culture medium containing 5 mg / mL LA and 1 mL of complete culture medium containing 5 mg / mL LA and 10% of the sample (by mass fraction). Cells were then incubated for another 48 h. The supernatant was discarded, cells were stained with Oil Red O, and dissolved in isopropanol. Three replicates were performed for each group.

[0107]

[0108]

[0109] Results Analysis: Examples 1-4 all showed good effects in inhibiting sebum secretion, with inhibition rates all exceeding 80%. Example 2 showed the best effect, reaching 89.21%. Comparative Example 2 had a better sebum inhibition rate than Comparative Example 1, suggesting that Corydalis rhizome may have a better sebum-controlling effect than Scutellaria baicalensis. Overall, Comparative Examples 1-6 were significantly lower than Examples 1-4. Examples 1-4 had stronger sebum-inhibiting activity, indicating that the combination of the two ingredients increased the solubility of the active ingredients, thereby achieving a synergistic effect.

[0110] Irritation test of active ingredient (chicken embryo chorioallantoic membrane irritation substitution test)

[0111] Brief description of chicken embryo testing methods:

[0112] Based on the similarity between the vascular structure of the mid-stage chorioallantoic membrane (CAM) of fertilized chicken embryos (10-14 days after incubation) and the vascular composition of the human conjunctiva, an ocular irritation test method was used to detect the irritation of samples. 40 μL of the test substance was directly applied to the chicken embryo CAM. A negative control group (physiological saline) and a positive control group (0.01 mol / L SDS) were also included. Images taken before and after 30 minutes of application were compared to observe the degree of chorioallantoic membrane vascular damage (such as ghost vessels, capillary congestion, or hemorrhage). Different degrees of vascular damage were scored to determine the irritant level of the test substance.

[0113] The scoring criteria for vascular effects are as follows:

[0114]

[0115] NC value: The irritant effect of a test substance is compared based on the average score of the vascular injury severity rating (NC value).

[0116]

[0117] According to the test results, all samples in Examples 1-4 showed no irritation.

[0118] sample Test concentration NC score Stimulus grading Example 1 100％ 0.65 Non-irritating Example 2 100％ 1.02 Non-irritating Example 3 100％ 1.49 Non-irritating Example 4 100％ 1.25 Non-irritating

[0119] The results above show that the products provided in Examples 1 to 4 are all non-irritating and have a certain degree of safety.

[0120] 5. Human body testing

[0121] Test product: Example 5, required to effectively control oil, reduce swelling, and reduce redness compared to the control group:

[0122] Sixty volunteers aged 20-30 years with oily and combination skin exhibiting significant redness, swollen acne, and excessive oil production were selected and signed informed consent forms. The volunteers were randomly divided into two groups of 30 each. One group used the blank cream base, while the other group used the product provided in Example 5. After three days of product use, a consumer questionnaire was administered. Volunteers rated the reduction in acne redness, oil production, and redness on three dimensions: reduction in acne swelling, reduction in facial oil production, and reduction in facial redness. The evaluation results are shown in Table 1 below.

[0123] Table 1 Consumer Reviews of Acne Treatment

[0124]

[0125] The test results showed that the blank matrix group could not alleviate the symptoms of oil control, swelling reduction, and redness reduction in the skin after 3 days of use, while Example 5 had a better effect on oil control, swelling reduction, and redness reduction.

Claims

1. A composition having soothing and oil-controlling properties, characterized in that, It includes the following components by weight: Scutellaria baicalensis 150-200 parts, Corydalis yanhusuo 40-80 parts; The soothing and oil-controlling composition is prepared by the following steps: 1) Weigh each component, add 10 to 30 times the total weight of Scutellaria baicalensis and Corydalis yanhusuo in pure water and soak for 30 to 60 minutes. Extract at 85℃ with stirring 1 to 2 times, each time for 1 to 2 hours. Filter the extract and mix them. Let the filtrate stand for 12 hours before use. 2) Add 8 to 20 times the total mass of pure water to the residue from step 1), boil and stir to extract 1 to 2 times, each extraction lasting 1 to 2 hours. After filtering the extract, mix the two filtrates and concentrate under reduced pressure at 0.08 to 0.09 MPa and 60 to 70°C to obtain a clear extract with a raw medicinal material concentration of 0.2 to 0.5 g / ml. 3) After activating the macroporous resin, wet pack it into a column, collect and combine the eluent, and set aside for later use; 4) Concentrate the eluent collected in step 3) under reduced pressure (0.08-0.09 MPa, 60-70°C) to recover the ethanol, and concentrate until the concentration of the crude drug in the extract is 1 g / ml; add polyol and sodium citrate to adjust the pH to 4.5-7.0, add pure water to bring the volume to 0.2-0.5 g / ml, stir and heat to 80°C, keep warm for 15-30 min, and centrifuge the reconstituted solution through a tubular centrifuge at 15000-17000 r / min; pass the resulting centrifuged liquid through a 0.2 μm membrane to obtain the final product. The macroporous resin activation treatment method involves soaking the resin in 3-4 BV of 95% ethanol for 12 hours, wet packing the column, rinsing with 95% ethanol, and the rinsing endpoint being that the ethanol and pure water mixed in equal proportions after rinsing are free of turbidity. The resin is then washed with pure water until there is no alcohol odor.

2. The composition with soothing and oil-controlling properties according to claim 1, characterized in that, It also includes 120-200 parts of polyols.

3. The composition with soothing and oil-controlling properties according to claim 1, characterized in that, It also includes 1-10 parts of sodium citrate.

4. The method for preparing the composition with soothing and oil-controlling properties according to claim 1, characterized in that, The filtration described in steps 1) and 2) uses 300-mesh filter cloth.

5. The method for preparing the composition with soothing and oil-controlling properties according to claim 1, characterized in that, When packing macroporous resin columns using the wet method, the sample loading flow rate is 1~3 BV / h; after sample loading, rinse the column with 4~8 BV of pure water at a flow rate of 1~4 BV / h; elute with 5~12 BV of 40%~80% ethanol at a flow rate of 1~4 BV / h, collect and combine the eluent for later use.

6. The method for preparing the composition with soothing and oil-controlling properties according to claim 1, characterized in that, The pH value mentioned in step 4) is adjusted using sodium citrate.

7. The use of the soothing and oil-controlling composition according to claim 1 as a cosmetic additive.

8. The application of the soothing and oil-controlling composition according to claim 7 as a cosmetic additive, characterized in that, The cosmetic product is in the form of an essence or a spray.

9. The application of the soothing and oil-controlling composition according to claim 7 as a cosmetic additive, characterized in that, The amount of the soothing and oil-controlling composition added is 0.1wt%-20wt%.

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