Plant extract composition with effects of controlling oil and removing acnes, preparation method of plant extract composition and skin care product

Abstract

The invention discloses a plant extract composition with oil-controlling and acne-removing effects, a preparation method thereof and a skin care product, and belongs to the technical field of skin care products, the key point of the technical scheme is that the preparation method of the plant extract composition comprises the following steps: performing solvent extraction and chromatographic purification to obtain a dogwood fruit extract; the raspberry fruit extract is obtained through low-temperature wall breaking extraction and enzymolysis; carrying out solvent extraction and wrapping treatment to obtain a water-soluble schisandra chinensis fruit, radix sophorae flavescentis root and witch hazel composite extract; the preparation method comprises the following steps: uniformly mixing 1-5% of a dogwood extract, 1-3% of a raspberry fruit extract, 2-6% of a composite extract and the balance of auxiliary materials to obtain the plant extraction composition. Through optimization of an extraction process of dogwood fruits, raspberry fruits, Chinese magnoliavine fruits, radix sophorae flavescentis and hamamelis virginiana, after the extracts are prepared, the plant extraction composition is prepared into the plant extraction composition; the effective active matters in the extracts are fully exerted to achieve a synergistic effect, so that the relatively good oil control and acne removal effects are realized.

Description

Technical Field

[0001] The present invention relates to the technical field of skin care products, and particularly to a plant extraction composition with oil control and acne removal effects, a preparation method thereof, and a skin care product. Background Art

[0002] In recent years, studies have found that natural plants contain rich nutrients, such as saponins, polysaccharides, phenolic acids, flavonoids, trace elements, etc., which have certain efficacy in the application of cosmetic formulations and are now widely used in skin care products with effects such as oil control or oil balance, acne removal and soothing, anti-wrinkle and firming, and repair.

[0003] In previous cosmetic research and development, in order to achieve effects such as oil control, acne removal, and anti-wrinkle, chemically synthesized active ingredients were often used. These ingredients can play corresponding roles to a certain extent, but may cause allergic reactions in some users. In addition, there were also some early attempts to apply the active ingredients of natural plants to cosmetics. However, the traditional extraction methods of plant active substances were relatively simple, such as direct crushing extraction or simple soaking with a single solvent. These methods were difficult to fully extract the effective ingredients in plants and could not remove impurities, resulting in a low purity of the extract. There were also some methods using high-temperature extraction, although it could improve the extraction efficiency, but it was easy to damage the thermosensitive effective ingredients in plants.

[0004] However, the existing technical means have obvious defects. Many active substances have poor water solubility, many impurity components, and the properties of the extract are not good, and the purity is low, resulting in the natural active ingredients added to cosmetics not achieving ideal effects and being difficult to simultaneously meet the various requirements of cosmetics such as stability, aesthetics, and efficacy. Summary of the Invention

[0005] In order to solve the problems in the existing technology, the present invention provides a plant extraction composition with oil control and acne removal effects, a preparation method thereof, and a skin care product. Through the optimization of the extraction processes of fructus corni, fructus rubi, fructus schisandrae chinensis, radix sophorae flavescentis, and witch hazel, after reasonable configuration of these extracts, the effective active substances in each extract can be fully exerted, achieving a synergistic effect, and thus realizing good oil control balance and acne removal effects.

[0006] The first aspect of the present invention is to provide a preparation method of a plant extraction composition with oil control and acne removal effects, adopting the following technical scheme: A preparation method of a plant extraction composition with oil control and acne removal effects, comprising the following steps: Obtaining a fructus corni extract by solvent extraction and chromatography purification; Obtaining a fructus rubi extract by low-temperature cell wall breaking extraction and enzymatic hydrolysis; The water-soluble Schisandra chinensis fruit, Sophora flavescens root, and witch hazel composite extract is obtained by solvent extraction and encapsulation treatment. By weight percentage, 1-5% of the cornus officinalis extract, 1-3% of the raspberry fruit extract, 2-6% of the composite extract, and the balance being excipients are mixed evenly to obtain the plant extract composition.

[0007] By adopting the above technical solutions, the cornus officinalis fruit extract obtained by solvent extraction and chromatography purification can improve the purity of the extract; the raspberry fruit extract obtained by low-temperature cell wall breaking extraction and enzymatic hydrolysis is beneficial to releasing the active ingredients in the fruit; the water-soluble Schisandra chinensis fruit, Sophora flavescens root, and witch hazel composite extract obtained by solvent extraction and encapsulation treatment can improve its water solubility and stability; the three extracts are mixed with excipients according to specific weight percentages to obtain the plant extract composition, which can enable the active ingredients in each extract to play a full role and achieve a synergistic effect, thus realizing better oil control balance and acne treatment effects.

[0008] Preferably, the method for obtaining the cornus officinalis fruit extract by solvent extraction and chromatography purification is as follows: S1. The pericarp of cornus officinalis fruit is dried at low temperature, pulverized, and sieved through a 20-40 mesh sieve to obtain the pericarp powder of cornus officinalis fruit. S2. Add an ethanol solution 10-15 times the weight of the pericarp powder of cornus officinalis fruit in step S1, mix evenly, and reflux and extract at 65-75 °C for 2-3 h to obtain a crude extract. S3. Centrifuge and separate the crude extract to obtain a filtrate, concentrate the filtrate under reduced pressure, and then purify the concentrated solution by column chromatography. First, elute with pure water, and the elution volume is 2-3 times the column bed volume. Then, elute with a 40 wt% ethanol solution, collect the purified solution eluted with the ethanol solution, and concentrate under reduced pressure to obtain the cornus officinalis fruit extract.

[0009] By adopting the above technical solutions, drying at low temperature, pulverizing, and sieving through a 20-40 mesh sieve is beneficial for subsequent extraction of the active ingredients of cornus officinalis fruit; reflux extraction with a 10-15 times ethanol solution at 65-75 °C for 2-3 h can fully extract the active ingredients in the cornus officinalis fruit. Then, purify the concentrated solution by column chromatography, first elute with water and then elute with a 40 wt% ethanol solution to remove impurities and obtain a high-purity cornus officinalis fruit extract, which helps the final plant extract composition to have better oil control and acne treatment effects.

[0010] Preferably, in step S2, every 30 min, stir at a speed of 100-300 rpm for 5 min, repeat the extraction once, filter, and combine the crude extracts.

[0011] Preferably, the chromatographic packing material in the column chromatography purification step is one of D-101, AB-8, and HDP600.

[0012] Preferably, the method for low-temperature cell wall breaking extraction and enzymatic hydrolysis to obtain raspberry fruit extract is as follows: S1. After washing and removing the stalks of fresh raspberry fruits, grind the raspberry fruits and water at a weight ratio of 1:(5 - 8) for 10 - 20 min to obtain a slurry; S2. Add a complex enzyme to the slurry for enzymatic hydrolysis for 3 - 4 h at an enzymatic hydrolysis temperature of 45 - 55 °C, and the addition amount of the complex enzyme is 0.01 - 0.05% of the weight of the slurry; S3. Inactivate the enzyme activity of the enzymatically hydrolyzed slurry at 90 - 100 °C for 20 min, then centrifuge, and take the supernatant to pass through a 0.22 μm filter membrane to obtain raspberry fruit extract.

[0013] By adopting the above technical solution, grinding fresh raspberry fruits with water at a specific weight ratio can fully break the fruit cells, which is beneficial to the subsequent extraction of active ingredients. Then, the slurry is enzymatically hydrolyzed with a complex enzyme under suitable temperature and addition amount conditions, which can further decompose the cell wall and improve the dissolution rate of active ingredients; inactivating the enzyme activity of the enzymatically hydrolyzed slurry at high temperature can terminate the enzymatic reaction, ensure the stable quality of the extract, and impurities can be removed after centrifugation and filtration to obtain pure raspberry fruit extract. When mixed with cornel fruit extract, water-soluble schisandra fruit, sophora flavescens root, witch hazel composite extract and excipients, it can make the prepared plant extract composition exert a better oil control and acne removal effect.

[0014] Preferably, the complex enzyme is composed of xylanase, papain and pectinase at a weight ratio of 1:0.5:1.

[0015] Preferably, the method for solvent extraction and encapsulation treatment to obtain water-soluble schisandra fruit, sophora flavescens root, witch hazel composite extract is as follows: S1. Mix schisandra fruit, sophora flavescens root and witch hazel at a weight ratio of 2:1:1, dry and crush them, and pass through a 40 - 60 mesh sieve to obtain a composite plant powder; S2. Mix the composite plant powder and ethanol solution at a weight ratio of 1:(10 - 15), and reflux and extract at 60 - 70 °C for 2 - 3 h; S3. Centrifuge the composite plant extract, concentrate it under reduced pressure to 1 - 2 times the weight of the composite plant powder, then dissolve the composite plant extract and butanediol at a weight ratio of 1:10 at 50 °C to obtain a mixed solution; S4. Prepare a 10 wt% cyclodextrin solution, preheat the cyclodextrin solution at a stirring rate of 300 rpm / min and a temperature of 50 °C, then stir the mixed solution obtained in step S3 and the cyclodextrin solution at a weight ratio of 1:(15 - 20) at a constant temperature for 30 min, then perform high-pressure homogenization and pass through a 0.22 μm filter membrane to obtain schisandra fruit, sophora flavescens root, witch hazel composite extract.

[0016] By adopting the above technical solution, Schisandra chinensis fruit, Sophora flavescens root, and Hamamelis virginiana are mixed and pulverized according to a specific weight ratio, and after being extracted, concentrated, and redissolved with a solvent under specific conditions, they are mixed with a preheated cyclodextrin solution in proportion and filtered by high-pressure homogenization, which can effectively improve the water solubility of the composite extract, overcome the problem of poor water solubility of active substances, enable the natural active ingredients added to cosmetics to better exert the effects of oil control and acne removal, and also improve the stability, aesthetics, and purity of the extract, thereby improving the properties of the extract solution.

[0017] The second aspect of the present invention is to provide a plant extract composition obtained by the above preparation method. By weight percentage, the extract of Cornus officinalis is 1-5%, the extract of Rubus idaeus fruit is 1-3%, the composite extract is 2-6%, and the balance is auxiliary materials. The composite extract is composed of Schisandra chinensis fruit, Sophora flavescens root, and Hamamelis virginiana mixed according to a weight ratio of 2:1:1; the auxiliary materials are composed of pure water, butylene glycol, hexylene glycol, and octanoyl hydroxamic acid mixed according to a weight ratio of (79-90):5:0.8:0.05.

[0018] The third aspect of the present invention is to provide a skin care product, including the following components by weight percentage: glycerol 10-15%, squalane 1-3%, lecithin 0.5-2%, the plant extract composition obtained in the above claim 8 is 1-5%, and the balance is deionized water.

[0019] In summary, the present invention has the following beneficial effects: By extracting Cornus officinalis, Rubus idaeus fruit, Schisandra chinensis fruit, Sophora flavescens root, and Hamamelis virginiana in specific ways respectively, the content of active ingredients in the plants is effectively increased. After reasonably configuring the concentrated extracts, the active ingredients in each extract can be fully exerted, achieving a synergistic effect, and thus realizing better oil control balance and acne removal effects. Detailed Description of the Invention

[0020] The following further elaborates on the present invention in conjunction with embodiments. All reagents without indicating the manufacturer can be obtained as conventional reagent products through commercial purchase.

[0021] Example 1 A skin care product is weighed according to the following weight percentages of components: Glycerol 15%, squalane 3%, lecithin 2%, plant extract composition 5%, and the balance is deionized water. The glycerol, squalane, and lecithin are stirred and dissolved evenly to obtain an oil phase, the plant extract composition and water are stirred and mixed evenly to obtain an aqueous phase, and the aqueous phase and the oil phase are mixed and emulsified evenly at a rotation speed of 4000 r / min to obtain the skin care product; The preparation method of the plant extract composition includes the following steps: (I) Extract of Cornus officinalis fruit S1.1. Low-temperature dry and pulverize the pericarp of Cornus officinalis fruits, and sieve through a 20-mesh sieve to obtain Cornus officinalis fruit pericarp powder; S1.2. Add an ethanol solution with a concentration of 40 wt% and a weight 10 times that of the Cornus officinalis fruit pericarp powder in step S1. After mixing evenly, reflux and extract at 75 °C for 2 h. During extraction, stir at a speed of 100 rpm for 5 min every 30 min, repeat the extraction once, filter, and combine the crude extracts; S1.3. Centrifuge the crude extract at a speed of 8000 r / min for 15 min to separate and obtain the filtrate. Concentrate the filtrate under reduced pressure. The conditions for reduced-pressure concentration are a temperature of 45 °C and a vacuum degree of -0.08 MPa to remove ethanol. Purify the concentrated solution by chromatography column. The packing material for chromatography column purification is D-101. First, elute with pure water, and the elution volume is 2 times the column bed volume. Then, elute with a 40 wt% ethanol solution, collect the purified solution eluted by the ethanol solution, and concentrate under reduced pressure to obtain the Cornus officinalis fruit extract; (2) Raspberry fruit extract S2.1. After washing and removing the stalks of fresh raspberry fruits, mix the raspberry fruits and water at a weight ratio of 1:5 and grind for 10 min to obtain a liquid material; S2.2. Add a complex enzyme to the liquid material for enzymatic hydrolysis for 3 h. The enzymatic hydrolysis temperature is 55 °C, and the addition amount of the complex enzyme is 0.01% of the weight of the liquid material. During enzymatic hydrolysis, stir for 5 min every 30 min. The complex enzyme is composed of xylanase, papain, and pectinase at a weight ratio of 1:0.5:1; S2.3. Inactivate the enzyme activity of the enzymatically hydrolyzed liquid material at 90 °C for 20 min, then centrifuge, and take the supernatant and filter through a 0.22-μm filter membrane to obtain the raspberry fruit extract; (3) Composite extract S3.1. Mix Schisandra chinensis fruits, Sophora flavescens roots, and Hamamelis virginiana at a weight ratio of 2:1:1, dry and pulverize, and sieve through a 40-mesh sieve to obtain a composite plant powder; S3.2. Mix the composite plant powder and an ethanol solution with a concentration of 50 wt% at a weight ratio of 1:10, and reflux and extract at 60 °C for 3 h; S3.3. Centrifuge the composite plant extract at a speed of 9000 r / min for 15 min, filter to remove residues, collect the filtrate, and then concentrate under reduced pressure to 1 time the weight of the composite plant powder. Then, dissolve the composite plant extract and butanediol at a weight ratio of 1:10 at 50 °C to obtain a mixed solution; S3.4. Prepare a 10 wt% cyclodextrin solution, preheat the cyclodextrin solution at a stirring rate of 300 rpm / min and a temperature of 50 °C, then stir the mixed solution obtained in step S3.3 and the cyclodextrin solution at a weight ratio of 1:15 under the condition of 50 °C for 30 min, and then perform high-pressure homogenization. After circulating and treating 2 times at 800 bar, filter through a 0.22 μm filter membrane to obtain the compound extract of Schisandra chinensis fruit, Sophora flavescens root, and Hamamelis virginiana; By weight percentage, mix 2% of the extract of Cornus officinalis, 2% of the extract of Rubus idaeus fruit, 4% of the compound extract, and the balance is auxiliary materials and mix evenly at 50 °C, and then filter through a 0.22 μm filter membrane to obtain the final composition, wherein the auxiliary materials are mixed evenly by pure water, butylene glycol, hexylene glycol, and octanoyl hydroxamic acid according to a weight ratio of 85:5:0.8:0.05 to obtain the plant extract composition.

[0022] Example 2 A skin care product, weigh the components according to the following weight percentages: 15% glycerin, 3% squalane, 2% lecithin, 5% plant extract composition, and the balance is deionized water. Stir glycerin, squalane, and lecithin to dissolve evenly to obtain the oil phase, stir the plant extract composition and water to mix evenly to obtain the water phase, and mix the water phase and the oil phase and emulsify evenly at a rotation speed of 4000 r / min to obtain the skin care product.

[0023] Among them, the preparation method of the plant extract composition includes the following steps: (I) Extract of Cornus officinalis fruit S1.1. Low-temperature dry and pulverize the pericarp of Cornus officinalis fruit and pass through a 40-mesh sieve to obtain the pericarp powder of Cornus officinalis fruit; S1.2. Add an ethanol solution with a concentration of 60 wt% 15 times the weight of the pericarp powder of Cornus officinalis fruit to step S1, mix evenly, and reflux and extract at 65 °C for 3 h. During extraction, stir at a rotation speed of 300 rpm for 5 min every 30 min, repeat the extraction once, filter, and combine the crude extracts; S1.3. Centrifuge the crude extract at a rotation speed of 10000 r / min for 15 min to separate and obtain the filtrate. Concentrate the filtrate under reduced pressure. The conditions for reduced pressure concentration are a temperature of 55 °C and a vacuum degree of -0.09 MPa to remove ethanol. Purify the concentrated solution by chromatography column. The packing material for chromatography column purification is AB-8. First, elute with pure water, and the elution volume is 3 times the column bed volume. Then elute with a 40 wt% ethanol solution, collect the purified solution eluted with the ethanol solution, and concentrate under reduced pressure to obtain the extract of Cornus officinalis fruit; (II) Extract of Rubus idaeus fruit S2.1. After washing and removing the stalks of fresh Rubus idaeus fruit, mix Rubus idaeus fruit and water according to a weight ratio of 1:8 and perform grinding treatment for 20 min to obtain a liquid material; S2.2. Add a composite enzyme to the feed liquid for enzymatic hydrolysis for 4 h. The enzymatic hydrolysis temperature is 45 °C, and the addition amount of the composite enzyme is 0.05% of the weight of the feed liquid. During the enzymatic hydrolysis process, stir for 5 min every 30 min. The composite enzyme is composed of xylanase, papain, and pectinase in a weight ratio of 1:0.5:1. S2.3. Inactivate the enzyme activity of the enzymatically hydrolyzed feed liquid at 100 °C for 20 min, then centrifuge, and take the supernatant to pass through a 0.22-μm filter membrane to obtain raspberry fruit extract. (III) Composite extract S3.1. Mix Schisandra chinensis fruit, Sophora flavescens root, and witch hazel in a weight ratio of 2:1:1, dry and crush them, and pass through a 60-mesh sieve to obtain a composite plant powder. S3.2. Mix the composite plant powder and an ethanol solution with a concentration of 70 wt% in a weight ratio of 1:15, and reflux and extract at 70 °C for 2 h. S3.3. Centrifuge the composite plant extract at a rotational speed of 11,000 r / min for 15 min, filter to remove residues, collect the filtrate, and then concentrate it under reduced pressure to 2 times the weight of the composite plant powder. Then, dissolve the composite plant extract and butanediol in a weight ratio of 1:10 at 50 °C to obtain a mixed solution. S3.4. Prepare a 10 wt% cyclodextrin solution, preheat the cyclodextrin solution at a stirring rate of 300 rpm and a temperature of 50 °C, and then keep the mixed solution obtained in step S3.3 and the cyclodextrin solution at a weight ratio of 1:20 and stir them at a constant temperature of 50 °C for 30 min. Then, perform high-pressure homogenization, circulate and process at 1000 bar for 2 times, and then pass through a 0.22-μm filter membrane to obtain a composite extract of Schisandra chinensis fruit, Sophora flavescens root, and witch hazel. By weight percentage, mix 1% of the Cornus officinalis extract, 1% of the raspberry fruit extract, 2% of the composite extract, and the balance of excipients at 50 °C and mix them evenly, and then filter through a 0.22-μm filter membrane to obtain the final composition. The excipients are composed of pure water, butanediol, hexylene glycol, and octanoyl hydroxamic acid in a weight ratio of 79:5:0.8:0.05 and mixed evenly to obtain the plant extract composition.

[0024] Example 3 A skin care product, which is different from Example 1 in that, by weight percentage, the Cornus officinalis extract in the plant extract is 5%, the raspberry fruit extract is 3%, the composite extract is 6%, and the balance is excipients, and the others are the same as in Example 1.

[0025] Example 4 A skin care product, which is different from Example 1 in that it contains 10% glycerol, 1% squalane, 0.5% lecithin, 1% plant extract composition, and the balance is deionized water, and the others are the same as in Example 1.

[0026] Comparative Example 1 A skin care product, which is different from Example 1 in that, by weight percentage, the raspberry fruit extract in the plant extract is 2%, the compound extract is 4%, and the balance is auxiliary materials, and the others are the same as in Example 1.

[0027] Comparative Example 2 A skin care product, which is different from Example 1 in that, by weight percentage, the cornel fruit extract in the plant extract is 2%, the compound extract is 4%, and the balance is auxiliary materials, and the others are the same as in Example 1.

[0028] Comparative Example 3 A skin care product, which is different from Example 1 in that, by weight percentage, the cornel fruit extract in the plant extract is 2%, the raspberry fruit extract is 2%, and the balance is auxiliary materials, and the others are the same as in Example 1.

[0029] Comparative Example 4 A skin care product, which is different from Example 1 in that the compound extract in the plant extract is obtained by the following preparation method: Schisandra chinensis fruit, Sophora flavescens root, and Witch Hazel are mixed in a weight ratio of 2:1:1, dried and pulverized, and passed through a 60-mesh sieve to obtain a compound plant powder. The compound plant powder is mixed with purified water in a weight ratio of 1:10, refluxed and extracted at 60°C for 3 h. The compound plant extract is centrifuged at a speed of 9000 r / min for 15 min, filtered to remove residues, the filtrate is collected, and then further finely filtered to obtain a clear and transparent extract. The other steps are the same as in Example 1.

[0030] Content and Efficacy Determination Experiment Detect the contents of total flavonoids and total sugars in the plant extract compositions obtained in the above examples and comparative examples, and detect the oil control effect of the skin care products obtained in the above examples and comparative examples on the human face, the determination method for the evaluation of the oil control effect, the acne removal effect, and the evaluation method for the acne removal effect.

[0031] 1. Determination Method for Total Flavonoid Content Using rutin as a reference substance and aluminum nitrate as a chromogenic agent for the colorimetric determination of flavonoids, the absorbance shows a linear relationship with the concentration of rutin. The total flavonoid content is determined by spectrophotometry as follows: Preparation of the standard curve: Using a pipette, accurately pipette 0.00 mL, 0.50 mL, 1.00 mL, 2.00 mL, 3.00 mL, 4.00 mL of the rutin standard solution (equivalent to 0 μg, 75 μg, 150 μg, 300 μg, 450 μg, 600 μg of the standard substance) into 10 mL stoppered test tubes, make up the volume to 5 mL with 70 wt% ethanol. Add 0.30 mL of 5 wt% sodium nitrite solution to each, shake well and let stand for 5 min. Then add 0.30 mL of 10 wt% aluminum nitrate solution to each, shake well and let stand for 6 min. Finally, add 2 mL of 1.0 mol / L sodium hydroxide solution and make up the volume to 10 mL with 70 wt% ethanol. Let stand for 10 min, shake well and measure the absorbance at a wavelength of 510 nm. Taking the absorbance as the ordinate (Y) and the concentration of the standard rutin as the abscissa (X), plot the standard curve to obtain the regression equation and correlation coefficient of the standard curve, Y = 6.0374x + 0.0172, R 2 = 0.9994.

[0032] Sample detection: The volume of the test sample added is 1.0 mL, make up the volume to 5 mL with 70% ethanol. Add 0.30 mL of 5 wt% sodium nitrite solution to each, shake well and let stand for 5 min. Then add 0.30 mL of 10 wt% aluminum nitrate solution to each, shake well and let stand for 6 min. Finally, add 2 mL of 1.0 mol / L sodium hydroxide solution and make up the volume to 10 mL with 70% ethanol. Let stand for 10 min, shake well and measure the absorbance at a wavelength of 510 nm.

[0033] Calculation of results: Calculate according to the plotted standard curve.

[0034] Total flavonoid content = C × N, where C is the flavonoid content (μg / mL) in the test solution calculated according to the regression equation of the standard curve, and N is the dilution factor.

[0035] 2. Determination method of total sugar content Under the action of sulfuric acid, polysaccharides are first hydrolyzed into monosaccharides, and then quickly dehydrated to form furfural derivatives, which then react with phenol to form an orange-yellow compound, and then determined by colorimetry.

[0036] Preparation of standard curve: Accurately weigh 0.2 g of glucose standard sample dried to a constant weight at 105 °C, dissolve it with distilled water and make up the volume to 100.00 mL in a volumetric flask. Pipette 5.00 mL of this solution and make up the volume to 100.00 mL in a volumetric flask again to obtain a standard glucose solution with a concentration of 0.1 g / L. Accurately pipette 0 (blank), 0.10 mL, 0.20 mL, 0.30 mL, 0.40 mL, 0.50 mL, 0.60 mL, 0.70 mL of the standard solution into stoppered test tubes respectively, add ultrapure water to make the volume 1.0 mL, then add 1.0 mL of phenol solution with a volume fraction of 6%, shake well, quickly add 5.0 mL of concentrated sulfuric acid, shake for 5 min, place in a boiling water bath and heat for 15 min, then cool in cold water to room temperature. Measure the absorbance A at 490 nm with a spectrophotometer, repeat 5 times. Use the sugar concentration (C) as the abscissa and the absorbance (A) as the ordinate to plot the standard curve, and obtain the regression equation and correlation coefficient of the standard curve, Y = 11.062x + 0.0118, R 2 = 0.9993.

[0037] Sample detection: Add 1.0 mL of the test sample, then add 1.0 mL of phenol solution with a volume fraction of 6%, shake well, quickly add 5.0 mL of concentrated sulfuric acid, shake for 5 min, place in a boiling water bath and heat for 15 min, then cool in cold water to room temperature. Measure the absorbance A at 490 nm with a spectrophotometer.

[0038] Calculation of results: Calculate according to the plotted standard curve.

[0039] Total sugar content = C × N. Where, C - the total sugar content (g / L) in the test solution calculated according to the regression equation of the standard curve; N - dilution factor.

[0040] 3. Determination method for the oil control effect on the human face and the evaluation of the oil control effect This test developed an internal laboratory method based on the basic definition of the oil control efficacy of cosmetics, used a multi-functional skin tester equipped with a skin oil content test probe Sebumeter® SM 815 to collect skin oil content parameters, and performed a statistical analysis of the objective indicators (skin oil content) in the sample area and the blank control area in the test area 2 h after using the test product.

[0041] Adopt the basic method of human volunteer efficacy test to conduct a human efficacy evaluation test on the oil control efficacy of the sample. There were 6 subjects participating in this test, 0 dropped out, and there were 6 effective subjects. Each person tested one sample of the protocol.

[0042] Step 1. Basic value measurement: Within 3 minutes after the subject cleans the face, use a skin oil measurement probe to measure the sebum amount on the skin surface of the measurement areas on the sample-applied side and the control side respectively. Measure 3 times at different positions within each area, and take the average value as the initial value of the sample-applied side and the control side. Step 2. Apply the sample once at a dosage of (2.0 ± 0.1) mg / cm². Take quantitative samples using a syringe or equivalent, and use a latex finger cot to evenly apply the sample within the specified area, and record the actual sample application amount.

[0043] Step 3. Measure 3 times at different positions within the sample-applied area and the control area at 0 h (before using the product) and 2 h (after using the product) respectively to obtain the sebum amount on the skin surface of each area. The measurement results are expressed as the average value of the 3 measurements.

[0044] 4. Acne treatment effect and evaluation method for acne treatment effect This test adopts the basic method of human volunteer efficacy test. After the volunteers use the test product for 7 days, use the facial imaging VISIA-CR instrument to test the number of red area spots (actually representing the number of acne) and the total spot area (actually representing the red and swollen area of acne) of the control skin before and after, to judge the 7-day acne treatment efficacy of the product.

[0045] Test process Step 1. Qualified subjects use an alkaline soap-based cleansing product to clean the face under the guidance of the staff. After cleaning, wipe it clean with a lint-free absorbent dry paper towel. Sit quietly in a compliant room for at least 30 minutes. During this period, do not drink water or beverages, expose the test area, keep relaxed, and avoid touching the test area.

[0046] Step 2. Then let the volunteers perform image acquisition on the facial imaging VISIA-CR instrument: the number of red area spots and the total spot area are used as the initial measurement values; then distribute the test samples, and the subjects use the samples according to the sample usage instructions; make a phone call follow-up during the subjects' use of the samples to track the basic situation.

[0047] Step 3. After 7 days, return to the laboratory, repeat the previous steps, and perform image acquisition on the facial imaging VISIA-CR instrument; after the test is completed, statistically analyze the test data, and perform calculations and analysis.

[0048] 5. The test results are shown as follows Table 1. Detection results of total flavonoid and total sugar contents Sample Example 1 Example 2 Example 3 Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Total flavonoid content μg / mL 205 172 184 158 145 169 126 Total sugar content g / L 2.35 1.50 1.76 1.15 1.03 1.22 0.95 Table 2. Detection results of the oil control effect of skin care products

[0049] From the test results of the amount of skin oil on the human facial skin in Table 2, it can be seen that after applying the cosmetics containing the plant extract composition in this application, the secretion of skin oil after 2 hours shows a downward trend in the application area compared with the control area. From the perspective of the incremental difference, the difference in Example 1 is the largest, indicating that the plant composition of this application has an oil control effect, and the oil control effect of Example 1 is the best.

[0050] Table 3 Detection Results of the Acne Removal Effect of Skin Care Products

[0051] From the detection results in Table 3, it can be seen that the number of spots and the total area of spots of the tested acne patients in the examples of this application show an obvious decreasing trend. Among them, the change rate of the difference in Example 1 is the most obvious, indicating that the number of acne and the area of the red and swollen area of the tested patients have been significantly improved, achieving a good acne removal effect.

[0052] Therefore, combined with the detection of the flavonoid and total sugar contents in Table 1, the total flavonoid content and the total sugar active substance content in the sample of Example 1 are the highest, indicating that the solution of Example 1 of this application has better advantages. Compared with other comparative examples, it shows that the content of the effective active substances in Example 1 of this application is higher, and the improvement of the active substance content will significantly improve the oil control and acne removal effects.

[0053] The embodiments of this specific implementation manner are all preferred embodiments of the present invention, and do not limit the protection scope of the present invention accordingly. Therefore, all equivalent changes made according to the structure, shape, and principle of the present invention should be covered within the protection scope of the present invention.

Claims

1. A preparation method of a plant extract composition with the efficacy of controlling oil and removing acne, characterized in that: It includes the following steps: Extract the fructus corni extract by solvent extraction and chromatographic purification; Extract the fructus rubi extract by low-temperature cell wall breaking extraction and enzymatic hydrolysis; Extract the water-soluble schizandra fruit, sophora flavescens root, and witch hazel composite extract by solvent extraction and encapsulation treatment; By weight percentage, 1-5% of the fructus corni extract, 1-3% of the fructus rubi extract, 2-6% of the composite extract, and the balance is auxiliary materials, and they are mixed evenly to obtain the plant extract composition.

2. The preparation method of a plant extract composition with oil control and acne removal effects according to claim 1, characterized in that: The method for extracting and chromatographically purifying the fructus corni extract by solvent extraction includes the following: S1. Low-temperature dry and crush the pericarp of fructus corni, and sieve it through a 20-40 mesh sieve to obtain the pericarp powder of fructus corni; S2. Add an ethanol solution 10-15 times the weight of the pericarp powder of fructus corni to step S1, mix evenly, and reflux and extract at 65-75°C for 2-3 h to obtain a crude extract; S3. Centrifuge and separate the crude extract to obtain a filtrate. Concentrate the filtrate under reduced pressure, and then purify the concentrated solution by column chromatography. First, elute with pure water, and the elution volume is 2-3 times the column bed volume. Then, elute with a 40 wt% ethanol solution, collect the purified solution eluted by the ethanol solution, and concentrate it under reduced pressure to obtain the fructus corni extract.

3. The preparation method of a plant extract composition with oil control and acne removal effects according to claim 2, characterized in that: In step S2, stir at a speed of 100-300 rpm for 5 min every 30 min, repeat the extraction once, filter, and combine the crude extracts.

4. The preparation method of a plant extract composition with oil control and acne removal effects according to claim 2, characterized in that: In the column chromatography purification step, the chromatographic packing material is one of D-101, AB-8, and HDP600.

5. The preparation method of a plant extract composition with oil control and acne removal effects according to claim 1, characterized in that: The method for extracting and enzymatically hydrolyzing the fructus rubi extract by low-temperature cell wall breaking includes the following: S1. After washing and removing the stalks of fresh fructus rubi, grind the fructus rubi and water according to a weight ratio of 1:(5-8) for 10-20 min to obtain a feed liquid; S2. Add a composite enzyme to the feed liquid for enzymatic hydrolysis for 3-4 h, the enzymatic hydrolysis temperature is 45-55°C, and the addition amount of the composite enzyme is 0.01-0.05% of the weight of the feed liquid; S3. Inactivate the enzyme activity of the enzymatically hydrolyzed feed liquid at 90-100°C for 20 min, then centrifuge, and take the supernatant and filter it through a 0.22 μm filter membrane to obtain the fructus rubi extract.

6. The preparation method of a plant extract composition with oil control and acne removal effects according to claim 5, characterized in that: The composite enzyme is composed of xylanase, papain, and pectinase according to a weight ratio of 1:0.5:

1.

7. The preparation method of a plant extract composition with oil control and acne removal effects according to claim 1, characterized in that: The method for extracting the water-soluble schizandra fruit, sophora flavescens root, and witch hazel composite extract by solvent extraction and encapsulation treatment includes the following: S1. Mix schizandra fruit, sophora flavescens root, and witch hazel in a weight ratio of 2:1:1, dry and crush them, and sieve them through a 40-60 mesh sieve to obtain a composite plant powder; S2. Mix the composite plant powder and an ethanol solution in a weight ratio of 1:(10-15), and reflux and extract at 60-70°C for 2-3 h; S3. Centrifuge the composite plant extract, concentrate it under reduced pressure to 1-2 times the weight of the composite plant powder, and then re-dissolve the composite plant extract and butanediol in a weight ratio of 1:10 at 50°C to obtain a mixed solution; S4. Prepare a 10 wt% cyclodextrin solution, preheat the cyclodextrin solution at a stirring rate of 300 rpm / min and a temperature of 50 °C, then stir the mixed solution obtained in step S3 and the cyclodextrin solution at a constant temperature with a weight ratio of 1:(15 - 20) for 30 min, and then perform high-pressure homogenization and filter through a 0.22 μm filter membrane to obtain the composite extract of Schisandra chinensis fruit, Sophora flavescens root, and Hamamelis virginiana.

8. A plant extract composition obtained by the preparation method of the plant extract composition with oil control and acne removal effects according to any one of claims 1-7, characterized in that: By weight percentage, 1 - 5% of the extract of Cornus officinalis, 1 - 3% of the extract of Rubus idaeus fruit, 2 - 6% of the composite extract, and the balance is auxiliary materials. The composite extract is a mixture of Schisandra chinensis fruit, Sophora flavescens root, and Hamamelis virginiana in a weight ratio of 2:1:1; the auxiliary materials are a mixture of pure water, butylene glycol, hexylene glycol, and octanoyl hydroxamic acid in a weight ratio of (79 - 90):5:0.8:0.

05.

9. A skin care product, characterized in that, It comprises the following components by weight percentage: 10 - 15% of glycerol, 1 - 3% of squalane, 0.5 - 2% of lecithin, 1 - 5% of the plant extraction composition obtained in claim 8 above, and the balance is deionized water.

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