Application of Acanthopanax trifoliatus leaf and stem extract in preparation of oil control product
The oil-control product prepared from the leaf and stem extract of Bletilla striata solves the problems of irritation and short-term effects of chemical ingredients in existing cosmetics, achieves a safe and effective oil-control effect, and meets consumers' demand for natural cosmetics.
Patent Information
- Application Number
- CN202510894085.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-06-30
- Publication Date
- 2025-09-12
AI Technical Summary
Existing oil-control cosmetics are mostly chemically synthesized substances, which are irritating and have short-term effects. They cannot effectively control sebum secretion. In addition, the use of natural acid substances in cosmetics is limited, making it difficult to meet consumers' demand for green and safe oil control.
The oil-control products are prepared by water extraction using the extract of the leaves and stems of the white taro. They include creams, lotions, gels and other dosage forms. They utilize the effect of reducing the oil secretion of sebaceous gland cells and are suitable for all skin types. They are gentle and non-irritating.
The extract from the leaves and stems of white taro can significantly reduce the oil secretion of sebaceous gland cells, has a significant oil control effect, is safe, and is suitable for different skin types. The product is mild and non-irritating, meeting consumers' demand for natural cosmetics.
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Figure CN120617110A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of natural extracts, and in particular to application of a bambusa serrata leaf and stem extract in the preparation of an oil-control product. Background Art
[0002] As living standards improve, people's demands for skin care are becoming increasingly demanding. People with oily skin urgently need cosmetics that effectively control oil secretion to improve their skin condition, satisfy their pursuit of beauty, and meet their daily skin care needs. Excessive oil production not only affects appearance but can also lead to a variety of skin problems. Excessive oil can easily contaminate environmental pollutants, clog pores, and cause skin diseases such as seborrheic dermatitis. Furthermore, oily skin can make it appear rough and enlarge pores, affecting its overall texture and radiance, causing psychological stress for consumers and reducing their quality of life.
[0003] The formation of oily skin is mainly related to the vigorous secretion of sebaceous glands. The secretion of sebaceous glands is regulated by many factors, among which androgens play a key role. Testosterone is converted into dihydrotestosterone under the action of 5α-reductase. Dihydrotestosterone can promote the excessive proliferation of sebaceous gland cells and promote the secretion of oil by sebaceous gland cells. In addition, sebaceous gland secretion is also related to factors such as sebaceous gland size, lifestyle habits (such as high-sugar, high-fat diet, staying up late, etc.), body parts (such as the T-zone has more sebaceous glands and more vigorous oil secretion), season (sebum secretion is relatively high in summer), age (sebaceous gland secretion rate is higher between the ages of 15 and 35) and gender (the average sebum value of men is higher than that of women).
[0004] In the cosmetics industry, commonly used oil-control products include oil-absorbing powders, surfactants, and acids. Common oil-absorbing powders, such as silica, titanium dioxide, and talc, fill pores with fine particles and absorb excess oil, thereby reducing surface shine. Their advantages include immediate shine reduction and ease of use. However, their disadvantages are that they only temporarily reduce shine and fail to fundamentally address excessive oil secretion. Excessive use can clog pores and cause other skin problems, such as acne. Some surfactants can remove sebum from the skin's surface through cleansing, providing a certain degree of oil control. However, some surfactants can be irritating, disrupting the skin's barrier function, leading to moisture loss and dryness. Long-term use can also cause adverse reactions such as skin allergies. Acids, such as azelaic acid, effectively inhibit 5α-reductase at relatively low concentrations, achieving an oil-control effect. However, acids significantly affect the pH of cosmetics, limiting their inclusion in cosmetic formulas. This, to a certain extent, limits their ability to fully exert their oil-control effects.
[0005] As living standards improve, consumers are increasingly choosing cosmetics containing natural ingredients, believing them to be greener, safer, and gentler. Researching and developing plant-based oil-control ingredients can provide the cosmetics industry with more natural and effective options, satisfying consumer demand for natural cosmetics and enhancing consumer trust and acceptance of these products.
[0006] Therefore, there is an urgent need to develop a green, oil-controlling natural product. Summary of the Invention
[0007] The purpose of the present invention is to overcome the shortcomings of the existing technology and provide the application of the leaf and stem extract of white balsam pear in the preparation of oil-control products, which can provide a better solution for people with oily skin and expand the application of the leaf and stem extract of white balsam pear in skin oil-control cosmetics.
[0008] To achieve the above object, the technical solution adopted by the present invention is:
[0009] In a first aspect, the present invention provides a use of an extract from the leaves and stems of Bletilla striata in preparing an oil-control product.
[0010] The present invention confirms through experiments that the leaf and stem extract of Bletilla striata has the effect of reducing the oil secretion of human sebaceous gland cells. At the same time, through human body tests, it is found that the leaf and stem extract of Bletilla striata has the oil-control effect, is safe, mild and non-irritating, and is suitable for consumers with various skin types and who have oil-control needs.
[0011] As a preferred embodiment of the application of the present invention, the oil-control product includes oil-control cosmetics and / or oil-control daily necessities.
[0012] As a preferred embodiment of the application of the present invention, the dosage form of the oil control product includes at least one of creams, lotions, aqueous solutions, gels, oils, powders, block powders or solids, patches, films and freeze-dried products.
[0013] As a preferred embodiment of the application of the present invention, the Bletilla striata leaf and stem extract is mainly prepared by water extraction.
[0014] As a preferred embodiment of the application of the present invention, the water extraction method comprises the following steps:
[0015] (1) extracting the leaves and / or stems of the white hyacinth with water at 96-100° C. for 1.5-3 hours, filtering to obtain a filtrate and a filter residue, wherein the obtained filtrate is the first extract;
[0016] (2) extracting the filter residue obtained in step (1) with water under reflux at 96-100° C. for 1-2 hours, filtering to obtain a filtrate and filter residue, wherein the obtained filtrate is the second extract;
[0017] (3) combining the first extract obtained in step (1) and the second extract obtained in step (2), concentrating and filtering to obtain a filtrate, and concentrating, sterilizing, and drying the filtrate to obtain a Bletilla striata leaf and stem extract.
[0018] As a preferred embodiment of the application of the present invention, in step (1), the ratio of the leaves and / or stems of the bletilla striata to water is: leaves and / or stems of the bletilla striata: water = 1 g: (10-20) mL.
[0019] As a preferred embodiment of the application of the present invention, in step (1), the ratio of the leaves and / or stems of the scutellaria baicalensis to water is the leaves and / or stems of the scutellaria baicalensis: water = 1 g: 15 mL.
[0020] As a preferred embodiment of the application of the present invention, in step (2), the ratio of the filter residue to water is filter residue: water = 1 g: (10-15) mL.
[0021] As a preferred embodiment of the application of the present invention, in step (2), the ratio of the filter residue to water is filter residue: water = 1 g: 10 mL.
[0022] As a preferred embodiment of the application of the present invention, in step (1), the reflux extraction time is 2 hours.
[0023] As a preferred embodiment of the application of the present invention, in step (2), the reflux extraction time is 1.5 h.
[0024] As a preferred embodiment of the application of the present invention, the filtration is performed using a filter membrane with a pore diameter of 0.22 μm.
[0025] As a preferred embodiment of the application of the present invention, the performance parameter of the extract from the leaves and stems of the scutellaria baicalensis is that the pH value of the aqueous solution of the 1 wt % extract from the leaves and stems of the scutellaria baicalensis is 4.0-6.5.
[0026] As a preferred embodiment of the application of the present invention, the performance parameter of the extract from the leaves and stems of the scutellaria baicalensis is that the moisture content of the extract from the leaves and stems of the scutellaria baicalensis is ≤7.0%.
[0027] As a preferred embodiment of the application of the present invention, the performance parameter of the extract from the white balsam pear leaf and stem is that the acid-insoluble ash content of the extract from the white balsam pear leaf and stem is ≤0.5%.
[0028] As a preferred embodiment of the application of the present invention, the weight of the extract from the leaves and stems of Bletilla striata accounts for 0.01-1% of the total weight of the oil-control product.
[0029] In a second aspect, the present invention provides an oil-control emulsion comprising the following components in parts by weight: 0.2-0.4 parts of acrylates / C10-30 alkyl acrylate crosspolymer, 2-4 parts of butylene glycol, 0.4-0.6 parts of p-hydroxyacetophenone, 2-4 parts of glycerin, 0.1-0.3 parts of xanthan gum, 0.4-0.6 parts of PCA zinc, 1.8-2.2 parts of cetearyl alcohol, 1.2-1.8 parts of cetyl phosphate, 1.8-2.2 parts of polydimethylsiloxane, 2.8-3.2 parts of caprylic / capric triglyceride, 0.08-0.12 parts of phenoxyethanol / ethylhexylglycerin, 0.1-0.5 parts of white peony leaf stem extract, and 80-99.5 parts of water.
[0030] As a preferred embodiment of the oil-control emulsion of the present invention, it includes the following components in parts by weight: 0.3 parts of acrylates / C10-30 alkyl acrylate crosspolymer, 3 parts of butylene glycol, 0.5 parts of p-hydroxyacetophenone, 3 parts of glycerin, 0.2 parts of xanthan gum, 0.5 parts of PCA zinc, 2 parts of cetearyl alcohol, 1.5 parts of cetyl phosphate, 2 parts of polydimethylsiloxane, 3 parts of caprylic / capric triglyceride, 0.1 parts of phenoxyethanol / ethylhexylglycerin, 0.2 parts of white peony leaf stem extract and 80-99.5 parts of water.
[0031] As a preferred embodiment of the oil-control emulsion of the present invention, the oil-control emulsion further comprises 0.01-0.05 parts by weight of daily-use fragrance.
[0032] As a preferred embodiment of the oil-control emulsion of the present invention, the pH value of the oil-control emulsion is 5.0-6.5.
[0033] In a third aspect, the present invention provides a process for preparing the above-mentioned oil-control emulsion, comprising the following steps:
[0034] (1) Mixing acrylic acid (esters) / C10-30 alkyl acrylate crosspolymer, butylene glycol, and p-hydroxyacetophenone with water, adding glycerin, xanthan gum, and PCA zinc, and heating to 75-80° C. for 25-30 minutes to obtain a premix a;
[0035] (2) mixing cetearyl alcohol, cetyl phosphate, dimethicone, and caprylic / capric triglyceride at 75-80° C. to obtain a premix b;
[0036] (3) mixing the premix a obtained in step (1) and the premix b obtained in step (2), homogenizing for 3-5 minutes, cooling to 45° C., adding phenoxyethanol / ethylhexylglycerin and daily fragrance, and mixing to obtain a premix c;
[0037] (4) The premix c obtained in step (3) was mixed with water and a pH regulator, and the pH was adjusted to 5.0-6.5. Water and the extract of the white sedge leaf and stem were added, and the mixture was stirred for 10-15 minutes to obtain an oil-control lotion.
[0038] Compared with the prior art, the present invention has the following beneficial effects:
[0039] The present invention confirms through experiments that the leaf and stem extract of Bletilla striata has the effect of reducing the oil secretion of human sebaceous gland cells. At the same time, through human body tests, it is found that the leaf and stem extract of Bletilla striata has the oil-control effect, is safe, mild and non-irritating, and is suitable for consumers with various skin types and who have oil-control needs. BRIEF DESCRIPTION OF THE DRAWINGS
[0040] Figure 1 This is the HPLC characteristic spectrum of the Bletilla striata leaf and stem extract obtained in Example 1 of the present invention;
[0041] Figure 2 This is the HPLC characteristic spectrum of the Bletilla striata leaf and stem extract obtained in Example 2 of the present invention;
[0042] Figure 3 This is the HPLC characteristic spectrum of the Bletilla striata leaf and stem extract obtained in Example 3 of the present invention;
[0043] Figure 4 This is a stacked diagram of the HPLC characteristic spectra obtained from the leaf and stem extracts of Examples 1-3 of the present invention;
[0044] Figure 5 The effect of different concentrations of the extracts from the leaves and stems of Bletilla striata on the viability of SZ95 cells in Experimental Example 1 of the present invention;
[0045] Figure 6 The effect of the leaf and stem extract of S. leucoderma on the oil secretion of SZ95 cells in Experimental Example 1 of the present invention, wherein A is the result of SZ95 staining under a fluorescence microscope, and B is the result of oil secretion detection of SZ95 cells with different treatments;
[0046] Figure 7 These are the results of human body tests on the oil-control efficacy of the oil-control lotion obtained in Example 4 of Experimental Example 2 of the present invention. In the figure, "ns" indicates no significant difference compared with the same treatment group before use, and "*" indicates a significant difference compared with the same treatment group before use (P < 0.05). DETAILED DESCRIPTION
[0047] In order to better illustrate the purpose, technical solutions and advantages of the present invention, the present invention will be further described below in conjunction with specific embodiments.
[0048] Unless otherwise specified, other materials and reagents used in the examples can be obtained from commercial sources.
[0049] The techniques not described in detail in the following examples, comparative examples and effect examples are all commonly used techniques in the art. Please refer to "Molecular Biology Experiment Manual" (Ma Wenli, People's Military Medical Publishing House), "Molecular Biology Experiment (Second Edition)" (Zhejiang University Press), and "Cell Biology Experiment" (Yang Hongbing, Hou Lixia, Zhang Yuxi, Higher Education Press).
[0050] The Bletilla striata used in the following examples, comparative examples and effect examples has been identified as Bletilla striata of the genus Acanthopanax in the family Araliaceae by the Guangdong Provincial Institute of Traditional Chinese Medicine Testing Center.
[0051] The CAS number of chlorogenic acid is 327-97-9, and the CAS number of isochlorogenic acid A is 89919-62-0.
[0052] SZ95 human sebaceous gland cells were purchased from Wuhan Punosai Biotechnology Co., Ltd. Unless otherwise specified, they were cultured in DMEM medium at 37°C and 5% CO2.
[0053] Anti-fluorescence quenching sealing fluid was purchased from Shanghai Biyuntian Biotechnology Co., Ltd. with the product number of P0126-25ml.
[0054] Example 1
[0055] This embodiment provides a method for preparing a leaf and stem extract of Bletilla striata, comprising the following steps:
[0056] S1. Extract the leaves and / or stems of Bletilla striata with water at a ratio of 1 g of leaves and / or stems of Bletilla striata and 15 mL of water at reflux at 100° C. for 2 h, and filter to obtain a filtrate and a filter residue, wherein the filtrate is the first extract;
[0057] S2. Extract the filter residue obtained in step S1 with water at 100° C. under reflux for 1.5 h in a ratio of 1 g of the filter residue obtained in step S1 to 10 mL of water. Filter to obtain a filtrate and a filter residue. The obtained filtrate is the second extract.
[0058] S3. The first extract obtained in step S1 and the second extract obtained in step S2 are combined, concentrated, and filtered using a 0.22 μm filter membrane. The retentate is discarded, and the filtrate is retained. The filtrate is concentrated, sterilized at high temperature, and spray-dried to obtain a white balsam pear leaf and stem extract. The yield of the white balsam pear leaf and stem extract is 8.64%, that is, 8.64 g of white balsam pear leaf and stem extract can be extracted from every 100 g of white balsam pear leaves and / or stems. The yields in the following Examples 2 and 3 have the same meaning.
[0059] The prepared Bletilla striata leaf and stem extract was characterized:
[0060] 1. The extract from the leaves and stems of the common balsam pear is in the form of a yellow-brown to yellow-brown powder, which is allowed to have agglomeration and has the characteristic odor of the raw material (the leaves and / or stems of the common balsam pear); the extract from the leaves and stems of the common balsam pear is prepared into a 1 wt% aqueous solution, and the pH value is measured to be 4.0-6.5; the moisture content of the extract from the leaves and stems of the common balsam pear is measured using a rapid moisture meter and is ≤7.0%; 1 g of the extract from the leaves and stems of the common balsam pear is mixed with 99 mL of water, and the extract from the leaves and stems of the common balsam pear is completely dissolved, with no impurities visible to normal vision and no charred debris; the acid-insoluble ash is measured according to the third method of the national standard GB 5009.4-2016 and is ≤0.5%.
[0061] 2. The characteristic spectrum of the extract from the leaves and stems of the white peony was tested, and chlorogenic acid and isochlorogenic acid A were used as reference substances for liquid chromatography detection.
[0062] Accurately weigh 22.29 mg of chlorogenic acid reference substance into a 25 mL volumetric flask, dissolve it with methanol and dilute to the mark, shake well to obtain a chlorogenic acid reference substance solution with a concentration of 873.8 μg / mL, and store it in a -8 °C refrigerator until use.
[0063] Accurately weigh about 21.83 mg of isochlorogenic acid A reference substance into a 25 mL volumetric flask, dissolve it with methanol and dilute to the mark, shake well to obtain an isochlorogenic acid A reference substance solution with a concentration of 829.5 μg / mL, and store it in a -8 °C refrigerator for later use.
[0064] Accurately weigh 0.5 g of the extract from the leaves and stems of the white taro obtained in Example 1 and place it in a 25 mL volumetric flask. Accurately add 20 mL of 70% methanol solution and ultrasonically treat (37 kHz, 1100w) for 30 min. Cool to room temperature, adjust to volume, shake well, and then filter with a 0.22 μm organic phase filter membrane. The filtrate is sampled and tested.
[0065] The chromatographic column was Hungpu AQ 5μm*4.6mm*250mm, the column temperature was 35°C, the flow rate was 1mL / min, the injection volume was 20μL, the detection wavelength was 280nm, and the mobile phase and elution gradient were shown in Table 1.
[0066] Table 1 Liquid chromatography mobile phase and elution gradient
[0067] Time / min Acetonitrile (%) 0.1v / v% formic acid-water (%) 0 7 93 8 15 85 33 25 75 35 40 60 42 80 20 50 80 20 51 7 93 60 7 93
[0068] The obtained leaf and stem extract of the white balsam pear was subjected to liquid chromatography detection according to the above method to determine the chromatographic peak of the leaf and stem extract of the white balsam pear, and to obtain the HPLC standard characteristic spectrum of the leaf and stem extract of the white balsam pear ( Figure 1 ), and the relative retention times of other characteristic chromatographic peaks were calculated using chlorogenic acid and isochlorogenic acid A as reference peaks. The results are shown in Table 2.
[0069] Table 2 Retention time of HPLC standard characteristic spectrum of the extract of Bletilla striata leaf and stem obtained in Example 1
[0070] Peak number Absolute retention time (min) Relative retention time (min) Remark S 12.772 1.00 Chlorogenic acid, reference peak 1 6.029 0.47 2 12.202 0.96 3 14.778 1.16 4 16.920 1.32 5 23.485 1.84 6 23.843 1.87 7 27.880 2.18 8 28.349 2.22 9 30.080 2.36 Isochlorogenic acid A 10 32.729 2.56
[0071] like Figure 1 As shown in Table 2, the characteristic peaks of the Bletilla striata leaf and stem extract obtained in Example 1 are 10 in total, and the separation degree of each characteristic peak is good, indicating that the characteristic spectrum of the Bletilla striata leaf and stem extract can be effectively constructed using the above method.
[0072] Example 2
[0073] This embodiment provides a method for preparing a leaf and stem extract of Bletilla striata, comprising the following steps:
[0074] S1. Extract the leaves and / or stems of Bletilla striata with water at a ratio of 1 g of leaves and / or stems of Bletilla striata and 15 mL of water at 98° C. under reflux for 1.5 h, and filter to obtain a filtrate and a filter residue. The obtained filtrate is the first extract;
[0075] S2. Extract the filter residue obtained in step S1 with water at 98°C under reflux for 1 hour in a ratio of 1 g of the filter residue obtained in step S1 to 10 mL of water. Filter to obtain a filtrate and a filter residue. The obtained filtrate is the second extract.
[0076] S3. The first extract obtained in step S1 and the second extract obtained in step S2 are combined, concentrated, and filtered using a 0.22 μm filter membrane. The retentate is discarded and the filtrate is retained. The filtrate is concentrated, sterilized at high temperature, and spray-dried to obtain a scutellaria baicalensis leaf and stem extract. The yield of the scutellaria baicalensis leaf and stem extract is 8.02%.
[0077] The obtained leaf and stem extract of Bletilla striata was subjected to HPLC detection according to the method described in Example 1 to obtain the HPLC standard characteristic spectrum ( Figure 2 ), and the relative retention times of other characteristic chromatographic peaks were calculated using chlorogenic acid and isochlorogenic acid A as reference peaks. The results are shown in Table 3.
[0078] Table 3 Retention time of HPLC standard characteristic spectrum of the extract of Bletilla striata leaf and stem obtained in Example 2
[0079] Peak number Absolute retention time (min) Relative retention time (min) Remark S 12.782 1.00 Chlorogenic acid, reference peak 1 6.029 0.47 2 12.182 0.95 3 14.783 1.16 4 16.928 1.32 5 23.480 1.84 6 23.833 1.86 7 27.890 2.18 8 28.323 2.22 9 30.091 2.35 Isochlorogenic acid A 10 32.725 2.56
[0080] like Figure 2 As shown in Table 3, the characteristic peaks of the Bletilla striata leaf and stem extract obtained in Example 2 are 10 in total, and the separation degree of each characteristic peak is good, indicating that the characteristic spectrum of the Bletilla striata leaf and stem extract can be effectively constructed using the above method.
[0081] Example 3
[0082] This embodiment provides a method for preparing a leaf and stem extract of Bletilla striata, comprising the following steps:
[0083] S1. Extract the leaves and / or stems of Bletilla striata with water at a ratio of 1 g of leaves and / or stems of Bletilla striata and 15 mL of water at 96° C. under reflux for 2 h, and filter to obtain a filtrate and a filter residue. The obtained filtrate is the first extract;
[0084] S2. Extract the filter residue obtained in step S1 with water at 96°C under reflux for 1 hour in a ratio of 1 g of the filter residue obtained in step S1 to 10 mL of water. Filter to obtain a filtrate and a filter residue. The obtained filtrate is the second extract.
[0085] S3. The first extract obtained in step S1 and the second extract obtained in step S2 are combined, concentrated, and filtered using a 0.22 μm filter membrane. The retentate is discarded and the filtrate is retained. The filtrate is concentrated, sterilized at high temperature, and spray-dried to obtain a scutellaria baicalensis leaf and stem extract. The yield of the scutellaria baicalensis leaf and stem extract is 7.43%.
[0086] The obtained leaf and stem extract of Bletilla striata was subjected to HPLC detection according to the method described in Example 1 to obtain the HPLC standard characteristic spectrum ( Figure 3 ), and the relative retention times of other characteristic chromatographic peaks were calculated using chlorogenic acid and isochlorogenic acid A as reference peaks. The results are shown in Table 4.
[0087] Table 4 HPLC standard characteristic spectrum retention time of the white sedge leaf and stem extract obtained in Example 2
[0088] Peak number Absolute retention time (min) Relative retention time (min) Remark S 12.776 1.00 Chlorogenic acid, reference peak 1 6.027 0.47 2 12.212 0.96 3 14.777 1.16 4 16.924 1.32 5 23.475 1.84 6 23.830 1.87 7 27.872 2.18 8 28.321 2.22 9 30.081 2.35 Isochlorogenic acid A 10 32.709 2.56
[0089] like Figure 3 As shown in Table 4, the characteristic peaks of the Bletilla striata leaf and stem extract obtained in Example 3 are 10 in total, and the separation degree of each characteristic peak is good, indicating that the characteristic spectrum of the Bletilla striata leaf and stem extract can be effectively constructed using the above method.
[0090] The HPLC standard characteristic spectra of the extracts of the leaves and stems of the white clover obtained in Examples 1-3 were stacked ( Figure 4 ) It can be seen that there are 10 common characteristic peaks of the white peony leaf and stem extract.
[0091] Experimental Example 1
[0092] To verify the oil-control efficacy of the extract from the leaves and stems of Bletilla striata, in vitro testing was conducted using SZ95 human sebaceous gland cells (hereinafter referred to as SZ95 cells) as the experimental subjects. The specific protocol is as follows:
[0093] 1. SZ95 cells were cultured at 6×10 3The cells were inoculated at a density of 100 μL in DMEM medium containing 10% FBS and 1% PS. After culturing for 12 hours, they were cultured with 100 μL of different concentrations of white balsam leaf and stem extract for 24 hours (white balsam leaf and stem extract: 0.05, 0.1, 0.2, 0.3125 mg / mL, diluted with DEME medium). The culture medium was then discarded, and 100 μL of fresh culture medium containing 10 μL MTT (5 mg / mL) was added and cultured at 37°C for another 4 hours. The supernatant was discarded, and 100 μL DMSO was added to dissolve the formed blue crystals. The absorbance was measured at 590 nm. The results are shown in the table. Figure 5 .
[0094] like Figure 5 As shown in the results, when the concentration of ETS-LE was 0.05 mg / mL, it had no significant effect on the proliferation of SZ95 cells. Even when the concentration was increased to 0.2 mg / mL, the viability of these cell lines remained at 89%, demonstrating that ETS-LE has low cytotoxicity. Based on this, 0.2 mg / mL was selected as the working concentration of ETS-LE in subsequent in vitro cell experiments.
[0095] 2. SZ95 cells were divided into four groups: blank group (Control), model group and sample group (0.2 mg / mL ETS-LE); blank group: cells + culture medium; model group: cells + culture medium + 5α-DHT (0.5 μg / mL); sample group: cells + culture medium + 5α-DHT (0.5 μg / mL) + ETS-LE (0.2 mg / mL), 5α-DHT refers to 5α-dihydrotestosterone.
[0096] SZ95 cells (4×10 5 Cells were plated into 6-well plates (100 cells / well). Using aseptic techniques, cells were inoculated with culture medium and cultured in a cell culture incubator at 37°C, 5% CO2. The cells were then digested with 0.25% (w / v) trypsin and subcultured for 12 hours until the cells adhered. The culture medium was then discarded, and fresh culture medium was added to the blank control group, 5α-DHT (0.5 μg / mL) was added to the model group, and a 5α-DHT-diluted extract of the white clover leaf and stem was added to the sample group (final concentration of 5α-DHT was 0.5 μg / mL, and final concentration of the white clover leaf and stem extract was 0.2 mg / mL). The cells were cultured for another 24 hours. The supernatant was again discarded, and the cells were washed three times with pre-chilled PBS for 3 minutes each. Each well was fixed with 1 mL of 4% v / v paraformaldehyde at room temperature for 10 minutes. After fixation, the cells were stained with Nile red (100 μg / mL) for 10 minutes in a 37°C incubator protected from light. The staining solution was aspirated and then washed with PBS 3 times, 5 minutes each time, and anti-fluorescence quenching sealing medium was added to each well. The staining was photographed under a fluorescence microscope. The results are shown in the figure. Figure 6 .
[0097] like Figure 6 As shown in -A, according to the morphological observation results, it can be seen that compared with the blank (Control) group, the sebum secretion of the model group increased significantly, and the sebum secretion model was successfully established; compared with the model group, the sample group treated with the white sedge leaf stem extract showed a decrease in oil secretion. The relative oil content of each group is shown in Figure 6 -B shows that compared with the blank group, the relative oil content of the model group increased, with a significant difference (P<0.001); compared with the model group, the relative oil content of the sample group treated with the white sedge leaf stem extract decreased by 19%, which was significant (P<0.05), indicating that the white sedge leaf stem extract has the effect of inhibiting the oil secretion of SZ95 cells, suggesting that the white sedge leaf stem extract has the effect of controlling oil.
[0098] Example 4
[0099] This embodiment provides an oil-control emulsion and a preparation method thereof. The components and amounts of the oil-control emulsion are shown in Table 5. The preparation method comprises the following steps:
[0100] (1) Mixing acrylic acid (esters) / C10-30 alkyl acrylate crosspolymer, butylene glycol, and p-hydroxyacetophenone with water, adding glycerin, xanthan gum, and PCA zinc, and heating to 75-80° C. for 25-30 minutes to obtain a premix a;
[0101] (2) mixing cetearyl alcohol, cetyl phosphate, dimethicone, and caprylic / capric triglyceride at 75-80° C. to obtain a premix b;
[0102] (3) mixing the premix a obtained in step (1) and the premix b obtained in step (2), homogenizing for 3-5 minutes, cooling to 45° C., adding phenoxyethanol / ethylhexylglycerin and daily fragrance, and mixing to obtain a premix c;
[0103] (4) The premix c obtained in step (3) was mixed with water and a pH regulator, and the pH was adjusted to 5.0-6.5. Water and the extract of the white sedge leaves and stems obtained in Example 1 were added, and the mixture was stirred for 10-15 minutes to obtain an oil-control lotion.
[0104] Table 5 Components and dosage of oil control emulsion
[0105]
[0106] Experimental Example 2
[0107] The oil-control emulsion obtained in Example 4 was tested on human subjects, and the specific scheme is as follows:
[0108] (1) The test recruited 5 healthy East Asian subjects aged 29 to 39 years old, who self-assessed that their facial skin was oily and had no other diseases that could affect the evaluation results. All 5 subjects completed the sample trial as required, with an average age of 34.4±4.8 years.
[0109] (2) Five subjects cleansed their faces the night before the test and did not use any products on their faces until they visited the laboratory the next day.
[0110] (3) After the visit, the skin was stabilized at a temperature of 21±1°C and a humidity of 50±10% for 30 minutes, and the base oil content of the left and right cheeks was measured using a skin oil tester.
[0111] (4) Apply 2 pumps of the sample to one side of the face at a time and apply evenly until absorbed, following the principle of randomized control.
[0112] (5) Use the skin oil tester 1 hour and 2 hours after using the sample. SM815) test the left and right cheek oil, the test results are shown in Table 6 and Figure 7 There was no significant difference in the fat content between the blank control groups or between the sample groups at different time points compared with that before use, which is indicated by "ns". There was a significant difference in the fat content between the blank groups or between the sample groups at different time points compared with that before use, which was indicated by "*" if P<0.05.
[0113] Table 6 Human test results of oil control efficacy before and after using oil control lotion
[0114]
[0115] like Figure 7 As shown in Table 6, compared with before use, the amount of oil on the skin surface was significantly reduced 1 hour or 2 hours after using the oil-control lotion; compared with before use, there was no significant difference in the amount of oil on the skin surface of the blank control group 1 hour or 2 hours after use. It can be seen that the oil-control lotion containing the extract of 1 white calendula leaf stem has a certain oil-control effect.
[0116] Experimental Example 3
[0117] The oil-control emulsion obtained in Example 4 was investigated, and the specific solution is as follows:
[0118] Healthy individuals aged 18-60 with oily skin are recruited as subjects. They are required to voluntarily participate in and actively cooperate with this trial. They are not required to participate in drug clinical trials or other product trial trials during the test period. They are required to ensure that only designated samples are used in the test area during the test period.
[0119] Thirty-two qualified subjects were screened, with zero dropouts. All 32 subjects, aged 21 to 48, completed the trial as instructed, achieving a 100% efficacy rate. Instructions for using the oil-control lotion: After cleansing the face, apply the product using the usual amount, gliding along the skin's texture from the inside out. Gently pat and massage until fully absorbed. Use once daily, morning and evening.
[0120] Consumers followed the instructions for using the oil-control lotion for three days and then completed a questionnaire to evaluate the results. The results were scored on a scale of 1 to 5: 1 for strongly disagree, 2 for disagree, 3 for indifference, 4 for agreement, and 5 for strongly agree. A score of 4 or higher was considered effective, otherwise it was considered ineffective. The formula for calculating the effectiveness is as follows:
[0121]
[0122] Where n5: number of people who scored 5 points, n4: number of people who scored 4 points, and n5: number of people who rated yes. 总 : The total number of people who scored 5, 4, 3, 2, and 1.
[0123] The results were evaluated using the binomial test. If the questionnaire data showed an efficacy rate > 50% and a P value < 0.05, the trial was considered effective. A P value < 0.5 and an efficacy rate > 50% indicated statistical significance, indicated by an "S." The survey results are shown in Table 7.
[0124] Table 7 Consumer survey results of oil-control lotion
[0125]
[0126]
[0127] As shown in Table 7, after the subjects used the oil-control lotion for 3 days, 87.50% of the volunteers felt that the excessive secretion of facial skin was reduced after using the product; 90.63% of the volunteers felt that the oiliness of facial skin became less obvious after using the product; 87.50% of the volunteers felt that the product had an oil-control effect; 90.63% of the volunteers felt that the oiliness of facial skin improved after use; 93.75% of the volunteers felt that the product was suitable for their skin type; and 87.50% of the volunteers felt that the product was satisfactory overall. In summary, the oil-control lotion containing the leaf and stem extract of the present application has a relatively excellent oil-control effect. In addition, consumers believe that the oil-control lotion containing the leaf and stem extract of the leaf and stem ...
[0128] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit the scope of protection of the present invention. Although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that the technical solutions of the present invention may be modified or replaced by equivalents without departing from the essence and scope of the technical solutions of the present invention.
Claims
1. Application of Bletilla striata leaf and stem extract in the preparation of oil control products.
2. The use according to claim 1, characterized in that The bletilla striata leaf and stem extract is mainly prepared by water extraction.
3. The use according to claim 2, characterized in that The water extraction method comprises the following steps: (1) extracting the leaves and / or stems of the white hyacinth with water at 96-100° C. for 1.5-3 hours, filtering to obtain a filtrate and a filter residue, wherein the obtained filtrate is the first extract; (2) extracting the filter residue obtained in step (1) with water under reflux at 96-100° C. for 1-2 hours, filtering to obtain a filtrate and filter residue, wherein the obtained filtrate is the second extract; (3) combining the first extract obtained in step (1) and the second extract obtained in step (2), concentrating and filtering to obtain a filtrate, and concentrating, sterilizing, and drying the filtrate to obtain a Bletilla striata leaf and stem extract.
4. The use according to claim 3, characterized in that Including at least one of the following (I) to (II): (I) In step (1), the ratio of the leaves and / or stems of the white hyacinth to water is: leaves and / or stems of the white hyacinth: water = 1 g: (10-20) mL; (II) In step (2), the ratio of the filter residue to water is filter residue: water = 1 g: (10-15) mL.
5. The use according to claim 3, characterized in that Including at least one of the following (III) to (IV): (III) In step (1), the reflux extraction time is 2 h; (IV) In step (2), the reflux extraction time is 1.5 h.
6. The use according to claim 3, characterized in that In step (3), the filtration is performed using a filter membrane with a pore diameter of 0.22 μm.
7. The use according to claim 1, characterized in that The performance parameters of the extract from the leaves and stems of the white calendula are at least one of the following (a) to (c): (a) the pH value of the 1 wt% aqueous solution of the Bletilla striata leaf and stem extract is 4.0-6.5; (b) the water content of the extract from the leaves and stems of the scutellaria baicalensis is ≤7.0%; (c) The acid-insoluble ash content of the extract from the white calamus leaf and stem is ≤0.5%.
8. The use according to claim 1, characterized in that The weight of the Bletilla striata leaf and stem extract accounts for 0.01-1% of the total weight of the oil-control product.
9. An oil-control lotion, characterized in that: The invention comprises the following components in parts by weight: 0.2-0.4 parts of acrylates / C10-30 alkyl acrylate crosspolymer, 2-4 parts of butylene glycol, 0.4-0.6 parts of p-hydroxyacetophenone, 2-4 parts of glycerin, 0.1-0.3 parts of xanthan gum, 0.4-0.6 parts of PCA zinc, 1.8-2.2 parts of cetearyl alcohol, 1.2-1.8 parts of cetyl phosphate, 1.8-2.2 parts of polydimethylsiloxane, 2.8-3.2 parts of caprylic / capric triglyceride, 0.08-0.12 parts of phenoxyethanol / ethylhexylglycerin, 0.1-0.5 parts of white calendula leaf stem extract and 80-99.5 parts of water.
10. The oil-control emulsion according to claim 9, characterized in that: The invention comprises the following components in parts by weight: 0.3 parts of acrylates / C10-30 alkyl acrylate crosspolymer, 3 parts of butylene glycol, 0.5 parts of p-hydroxyacetophenone, 3 parts of glycerin, 0.2 parts of xanthan gum, 0.5 parts of PCA zinc, 2 parts of cetearyl alcohol, 1.5 parts of cetyl phosphate, 2 parts of polydimethylsiloxane, 3 parts of caprylic / capric triglyceride, 0.1 parts of phenoxyethanol / ethylhexylglycerin, 0.2 parts of white calendula leaf stem extract and 80-99.5 parts of water.