A kind of squalene gel and preparation method thereof
By using squalene and specially made bark bark extract in gynecological gels, the shortcomings of traditional gels in fineness and antibacterial properties are solved, achieving better user experience and vaginal health protection.
Patent Information
- Application Number
- CN202110462329.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2021-04-27
- Publication Date
- 2025-02-18
- Estimated Expiration
- 2041-04-27
AI Technical Summary
Traditional gynecological gels have shortcomings in terms of delicateness and skin adhesion, and long-term use of chemical antibacterial agents will destroy vaginal microecological balance and cause irritation.
Using squalene gel, raw materials include skin conditioning agents, squalene, lactic acid bacteria fermentation products, thickeners, pH adjusters, cooling agents, oil-water mixed solvents and water, to prepare bald bark extract through specific process conditions. A and B, synergistically improve the fineness and antibacterial properties of the gel.
It improves the fineness and antibacteriality of the gel, increases moisturizing properties, and regulates the vaginal microecological balance and reduces the irritation to the skin.
Abstract
Description
Technical Field
[0001] The invention relates to daily chemical products for female hygiene and health, and in particular to squalene gel and a preparation method thereof. Background Art
[0002] Gynecological vaginal inflammation is a common disease among women. These inflammations are mainly caused by some bacterial infections. The commonly used treatment methods for this type of disease are oral or topical antibiotics. Topical antibiotics mainly include some lotions, but because lotions cannot fully stay in the external vagina during use and cannot achieve a good antibacterial effect, gel preparations have been developed. Because gel preparations can stay in the diseased area for a long time and can better exert their antibacterial properties, gel preparations have been widely developed.
[0003] However, the antibacterial property of traditional gel preparations is not good. In order to increase its antibacterial performance, some chemical antibacterial agents such as nanosilver are added to some gels to increase the gel's ability to kill harmful bacteria. However, since the female vagina is a relatively sensitive part, long-term use of these chemical antibacterial agents will, on the one hand, destroy the microecological balance of the vagina, and on the other hand, cause certain irritation to the vagina. Therefore, the applicant has developed a gynecological gel with specific plant components as antibacterial ingredients, and applied for relevant patents (patent number CN111419730A). The gynecological gel has good antibacterial properties and low irritation, but in subsequent use, it was found that the user experience was not very good, mainly due to the fineness of the gel and its adhesion to the skin. Summary of the invention
[0004] In order to solve the above technical problems, the first aspect of the present invention provides a squalene gel, the raw materials including, by weight percentage, 7-10% skin conditioner, 1-2% squalene, 1-1.5% lactic acid bacteria fermentation product, 0.0.6-1.3% thickener, 0.5-0.7% pH adjuster, 0.1-0.2% cooling agent, 0.5-1.5% oil-water mixed solvent, and water supplemented to 100%.
[0005] As a preferred technical solution of the present invention, the skin conditioner includes plant active ingredients and plant essential oils.
[0006] As a preferred technical solution of the present invention, the skin conditioner includes plant active ingredients, plant essential oils, and moisturizers.
[0007] As a preferred technical solution of the present invention, the plant active ingredients are a combination of Stemona japonica extract, Honeysuckle flower extract, Phellodendron chinense bark extract, Cnidium monnieri extract, Sophora flavescens extract, Pulsatilla scabra extract, Salvia miltiorrhiza extract, Camellia seed extract, and Coix lachryma-jobi seed extract, and the weight ratio thereof is (1-3): (2-4): (1-3): (2-4): (4-6): (1-3): (4-6): (2-4): (3-5).
[0008] As a preferred technical solution of the present invention, the Phellodendron amurense bark extract includes Phellodendron amurense bark extract A, and the Phellodendron amurense bark extract A is obtained by alcohol extraction.
[0009] As a preferred technical solution of the present invention, the Phellodendron amurense bark extract also includes Phellodendron amurense bark extract B, and the Phellodendron amurense bark extract B is extracted by an alkali extraction method.
[0010] As a preferred technical solution of the present invention, the humectant is a small molecule polyol.
[0011] As a preferred technical solution of the present invention, the thickener includes a combination of ammonium acryloyldimethyltaurate / VP copolymer and acrylic acid (ester) / C10-30 alkyl acrylate cross-linked polymer.
[0012] As a preferred technical solution of the present invention, the thickener further comprises polyethylene glycol-240 / HDI copolymer bis-decyltetradecyl alcohol polyether-20.
[0013] The second aspect of the present invention provides a method for preparing squalene gel, comprising the following preparation steps:
[0014] (1) Add the thickener to 40 wt% water, soak for 25 min, heat to 60° C. and stir to obtain material A;
[0015] (2) stirring the pH regulator and 1 wt% water to obtain material B;
[0016] (3) melting the cooling agent and adding it to 5 wt% water, stirring evenly, and then adding an oil-water mixed solvent to obtain material C;
[0017] (4) adding 15 wt % water and lactic acid bacteria fermentation product to material C to obtain material D;
[0018] (5) Add material A and the remaining water to the main pot, stir evenly at 70°C, then cool to 45°C, add the remaining raw materials, material B, and material D, stir evenly, and vacuum homogenize to obtain squalene gel.
[0019] Beneficial effects:
[0020] 1. The two specific Phellodendron bark extracts prepared in the present invention have a synergistic effect with each other, thereby improving the disadvantage of poor fineness of previous gel products, and the antibacterial property of the prepared gel is also comparable to that of previous gel products;
[0021] 2. The present invention can achieve good antibacterial and anti-inflammatory effects through the synergistic effect between the specific combination of plant active ingredients, and the addition of moisturizers also makes the gel have good moisturizing properties;
[0022] 3. Although the addition of moisturizer makes the gel have good moisturizing properties, it also causes the gel to over-solidify, resulting in poor adhesion of the gel to the skin. The present invention improves this shortcoming by selecting a specific thickener, while further increasing the fineness of the gel. DETAILED DESCRIPTION
[0023] The content of the present invention can be further understood by combining the following detailed description of the preferred implementation method of the present invention and the embodiments included. Unless otherwise stated, all technical and scientific terms used in this article have the same meaning as those of ordinary skill in the art to which the present invention belongs. If the definition of a specific term disclosed in the prior art is inconsistent with any definition provided in the present invention, the definition of the term provided in the present invention shall prevail.
[0024] As used herein, unless the context clearly indicates otherwise, features that are not limited to the singular or plural form are also intended to include features in the plural form. It should also be understood that the term "prepared by..." as used herein is synonymous with "comprising", "including", "including", "having", "including" and / or "comprising", when used in this specification, represents the stated composition, step, method, product or device, but does not exclude the presence or addition of one or more other compositions, steps, methods, products or devices. In addition, when describing embodiments of the present invention, the use of "preferred", "preferably", "more preferably", etc. refers to embodiments of the present invention that may provide certain beneficial effects in certain cases. However, other embodiments may also be preferred in the same or other cases. In addition, the expression of one or more preferred embodiments does not imply that other embodiments are not available, nor is it intended to exclude other embodiments from the scope of the present invention.
[0025] In order to solve the above technical problems, the first aspect of the present invention provides a squalene gel, the raw materials including, by weight percentage, 7-10% skin conditioner, 1-2% squalene, 1-1.5% lactic acid bacteria fermentation product, 0.0.6-1.3% thickener, 0.5-0.7% pH adjuster, 0.1-0.2% cooling agent, 0.5-1.5% oil-water mixed solvent, and water supplemented to 100%.
[0026] In a preferred embodiment, a squalene gel, the raw materials include, by weight percentage, 8.73% skin conditioner, 1.54% squalene, 1.23% lactic acid bacteria fermentation product, 1% thickener, 0.6% pH adjuster, 0.15% cooling agent, 1% oil-water mixed solvent, and water supplemented to 100%.
[0027] The skin conditioner is the main reason for the gel to exert its antibacterial effect. In order to ensure that the gel has safety and bactericidal efficacy, in one embodiment, the skin conditioner includes plant active ingredients and plant essential oils.
[0028] Because the gel of the present invention is mainly used on the female genitals, it is also necessary for the gel to have a certain moisturizing property during use. In a preferred embodiment, the skin conditioner includes plant active ingredients, plant essential oils, and moisturizers in a weight ratio of (2-4): (0.5-0.7): (4-6), preferably 3.07:0.66:5.
[0029] The synergistic effect between the specific combination of plant active ingredients can achieve excellent antibacterial and anti-inflammatory effects. In one embodiment, the plant active ingredients are a combination of Stemona japonica extract, Lonicera japonica extract, Phellodendron chinense bark extract, Cnidium monnieri extract, Sophora flavescens extract, Pulsatilla scabra extract, Salvia miltiorrhiza extract, Camellia japonica seed extract, and Coix lachryma-jobi seed extract, and the weight ratio is (1-3): (2-4): (1-3): (2-4): (4-6): (1-3): (4-6): (2-4): (3-5), preferably 2:3:2:3:5:2:5:3:4.
[0030] In one embodiment, the Phellodendron amurense bark extract includes Phellodendron amurense bark extract A.
[0031] In one embodiment, the Phellodendron chinense bark extract A is obtained by alcohol extraction.
[0032] In one embodiment, the preparation of the Phellodendron amurense bark extract A at least comprises:
[0033] (1) drying the Phellodendron amurense and grinding it in a grinder, and passing the obtained powder through a 50-80 mesh sieve to obtain substance A;
[0034] (2) dissolving substance A in 95% by volume ethanol at a material-liquid ratio of (10-20):1 (V / W) to obtain substance B;
[0035] (3) At room temperature, ultrasonically treating substance B at 100-200 W ultrasonic power for 10-15 min to obtain substance C;
[0036] (4) reflux substance C at 68-75° C. for 1-2 h and then filter to obtain filtrate D;
[0037] (5) Concentrating the filtrate D to one third of its volume to obtain a concentrated solution E;
[0038] (6) adding (2-5) times the volume of concentrated solution E and 95% ethanol to the concentrated solution E, mixing evenly, allowing to settle at 4° C. for 24 h, and then centrifuging at 2500-4000 rpm for 5-10 min to collect the solid, which is substance F;
[0039] (7) Dry the substance F to a constant weight to obtain the Phellodendron amurense bark extract A.
[0040] The material-liquid ratio (10-20): 1 (V / W) refers to the ratio of the volume of ethanol with a volume fraction of 95% to the mass of substance A.
[0041] In a preferred embodiment, the preparation steps of the Phellodendron amurense bark extract A are:
[0042] (1) Drying the Phellodendron amurense and grinding it in a grinder, and passing the resulting powder through a 60-mesh sieve to obtain substance A;
[0043] (2) dissolving substance A in 95% by volume ethanol at a material-liquid ratio of 15:1 (V / W) to obtain substance B;
[0044] (3) At room temperature, substance B was sonicated at 150 W ultrasonic power for 12 min to obtain substance C;
[0045] (4) Reflux the substance C at 70° C. for 1.5 h and then filter to obtain a filtrate D;
[0046] (5) Concentrating the filtrate D to one third of its volume to obtain a concentrated solution E;
[0047] (6) Add 3 times the volume of concentrated solution E and 95% ethanol to the concentrated solution E, mix well, let stand for precipitation at 4°C for 24 h, centrifuge at 3000 r / min for 8 min, and retain the solid, which is substance F;
[0048] (7) Dry the substance F to a constant weight to obtain the Phellodendron amurense bark extract A.
[0049] In the present invention, a Phellodendron bark extract A with specific active ingredients is prepared by specific process conditions. The applicant has found through research that a specific ratio of plant active ingredients and lactic acid bacteria fermentation products can synergistically inhibit harmful bacteria and promote the growth of probiotics, which is beneficial to the growth of beneficial bacteria and has a good effect on maintaining and repairing the balance of local microecology. In previous studies, the fineness of the gel prepared from the purchased plant extracts made the consumer experience poor when using it. In order to solve this problem, the applicant has found through a lot that it may be because the baicalin and berberine in the purchased Phellodendron bark extract, especially berberine, have poor solubility in the system of the present invention, resulting in the poor fineness of the prepared gel when it is used. The applicant found that the synergistic effect of the two specific Phellodendron bark extracts used in the present invention made the prepared gel have better fineness when used. This may be because the amount of insoluble solids of alkaloids such as baicalin and berberine in the Phellodendron bark extract A extracted using the extraction method of the present invention is reduced, and the active ingredients (polysaccharides) in the Phellodendron bark extract A have certain antibacterial properties through synergistic effects with other plant extracts in the system. At the same time, the Phellodendron bark extract A may also achieve the purpose of regulating skin inflammation through the interaction with different membrane receptors.
[0050] In a preferred embodiment, the Phellodendron amurense bark extract further includes Phellodendron amurense bark extract B.
[0051] In one embodiment, the Phellodendron chinense bark extract B is obtained by alkali extraction.
[0052] In one embodiment, the weight ratio of the Phellodendron amurense bark extract A to the Phellodendron amurense bark extract B is (1.2-2):(0.6-0.9), preferably 1.65:0.78.
[0053] In one embodiment, the preparation steps of the Phellodendron amurense bark extract B at least include:
[0054] (1) drying the Phellodendron amurense and grinding it in a grinder, and passing the obtained powder through a 50-80 mesh sieve to obtain material A;
[0055] (2) dissolving material A in a sodium hydroxide aqueous solution having a mass fraction of 0.8% to 1.3% according to a material-liquid ratio of (15-24): 1 (V / W) to obtain material B;
[0056] (3) at 35-50° C., subjecting material B to ultrasonic treatment at an ultrasonic power of 260-320 W for 12-18 min to obtain material C;
[0057] (4) stirring material C at 75-85° C. for 3-5 h to obtain material D;
[0058] (5) Centrifuge material D at 3500-4500 r / min for 10-20 min, and retain the supernatant as material E;
[0059] (6) Concentrating material E to one third of its volume to obtain material F;
[0060] (7) Add 95% ethanol (2-4 times the volume of material F) to material F and mix well. Let it settle at 4°C for 24 hours and centrifuge at 2500-3500 r / min for 5-10 minutes to collect the solid, which is material G.
[0061] (8) Dry material G to constant weight to obtain Phellodendron amurense bark extract B.
[0062] Among them, the material-liquid ratio (15-24): 1 (V / W) refers to the ratio of the volume of the sodium hydroxide aqueous solution with a mass fraction of 0.8%-1.3% to the mass of material A.
[0063] In a preferred embodiment, the preparation steps of the Phellodendron amurense bark extract B are:
[0064] (1) Drying the dried Phellodendron chinense medicinal material and grinding it in a grinder, and passing the obtained powder through a 60-mesh sieve to obtain material A;
[0065] (2) dissolving material A in a 1% by mass sodium hydroxide aqueous solution at a material-liquid ratio of 20:1 (V / W) to obtain material B;
[0066] (3) At 40°C, material B was ultrasonically treated at an ultrasonic power of 300 W for 15 min to obtain material C;
[0067] (4) stirring material C at 80° C. for 4 h to obtain material D;
[0068] (5) Centrifuge material D at 4000 r / min for 15 min, and retain the supernatant as material E;
[0069] (6) Concentrating material E to one third of its volume to obtain material F;
[0070] (7) Add 95% ethanol in a volume fraction of 3 times the volume of material F to material F and mix well. Allow to settle at 4°C for 24 hours and centrifuge at 3000 r / min for 8 minutes to collect the solid, which is material G.
[0071] (8) Dry material G to constant weight to obtain Phellodendron amurense bark extract B.
[0072] At present, there are plant extracts on the market that are used as active ingredients for anti-inflammatory and sterilization of female genitals, but the antibacterial property of the prepared products is not strong and cannot achieve a good antibacterial effect. In the present invention, the prepared Phellodendron bark extract A is used to synergize with other components in the system to increase the anti-inflammatory property of the gel and improve the disadvantage of poor fineness of the gel. However, the antibacterial property of the prepared gel is slightly lower than that of the gel prepared in patent CN111419730A. This may be because the alkaloid active substances in the Phellodendron bark extract A are reduced, resulting in a decrease in its antibacterial performance. The applicant intends to It was found that the synergistic effect of the Phellodendron chinense bark extract B prepared in the present invention and the Phellodendron chinense bark extract A not only can make the antibacterial activity of the gel reach the same antibacterial level as the gel prepared in patent CN111419730A, but also make the gel more suitable for the female vagina, further regulating the microecological balance of the vagina. The applicant speculates that this may be because the Phellodendron chinense bark extract B contains acidic active ingredients such as fatty acids, which can synergize with the Phellodendron chinense bark extract A and other active ingredients in the system to supplement the original antibody activity of the vagina and increase the defense against external bacteria, thereby increasing the antibacterial activity of the gel.
[0073] In one embodiment, the Chinese medicinal material Phellodendron chinense is purchased from Shunwangcheng Chinese medicinal material market; the honeysuckle flower extract is purchased from Shanghai Xier Biotechnology Co., Ltd. under the brand name of honeysuckle extract; the creeping Stemona extract is purchased from Ganzhou Baizhentang Biological Co., Ltd. under the brand name of Stemona extract; the Cnidium monnieri extract is purchased from Shanghai Xier Biotechnology Co., Ltd. under the brand name of Cnidium monnieri extract; the Sophora flavescens extract is purchased from Shanghai Xier Biotechnology Co., Ltd. under the brand name of Sophora flavescens extract; the Pulsatilla striata extract is purchased from Shaanxi Tianzhirun Biotechnology Co., Ltd. under the brand name of Pulsatilla striata extract; the Salvia miltiorrhiza extract is purchased from Shanghai Xier Biotechnology Co., Ltd. under the brand name of Salvia miltiorrhiza extract; the camellia seed extract is purchased from Ganzhou Baizhentang Biological Co., Ltd. under the brand name of tea seed extract; the Coix seed extract is purchased from Shanghai Ou Rong Biotechnology Development Center under the brand name of coix seed oil.
[0074] In order to make the gel have a rapid antibacterial effect when used, in one embodiment, the plant essential oil is a combination of tea tree essential oil, patchouli essential oil, lemon essential oil, and melaleuca essential oil, and the weight ratio thereof is (8-12):(2.3-4):(1.2-2.5):(8-12), preferably 10:3:2:10.
[0075] In one embodiment, tea tree essential oil was purchased from Wuhan Huaxiang Kejie Biotechnology Co., Ltd.; patchouli essential oil was purchased from Jinan Yunuo Chemical Co., Ltd.; lemon essential oil was purchased from Wuhan Huaxiang Kejie Biotechnology Co., Ltd.; and melaleuca essential oil was purchased from Jiangxi Global Natural Flavors Co., Ltd.
[0076] In one embodiment, the moisturizing agent is a small molecule polyol, which may be propylene glycol, butylene glycol, hexylene glycol, glycerol, etc. The preferred small molecule polyol is propylene glycol, and its CAS number is 57-55-6.
[0077] Squalene contains six isoprene double bonds. In the system of the present invention, squalene can enhance the metabolic activity of leukocytes, prevent functional cells from being hypoxic and causing pathological changes that lead to some inflammatory diseases, and can also synergize with the plant extracts and plant essential oils in the system to reduce the irritation of some substances in the plant extracts.
[0078] In one embodiment, squalene is purchased from Guangzhou Limeida Import and Export Trading Co., Ltd.
[0079] In one embodiment, the thickener includes a combination of ammonium acryloyldimethyltaurate / VP copolymer and acrylic acid (esters) / C10-30 alkyl acrylate cross-linked polymer, and the weight ratio thereof is 1:(1-2), preferably 1:1.5.
[0080] In a preferred embodiment, the thickener further comprises polyethylene glycol-240 / HDI copolymer bis-decyltetradecyl alcohol polyether-20.
[0081] In a preferred embodiment, the weight of the polyethylene glycol-240 / HDI copolymer bis-decyltetradecyl alcohol polyether-20 is 4-6% by weight of the moisturizer, preferably 5%.
[0082] In one embodiment, ammonium acryloyldimethyltaurate / VP copolymer is purchased from Shanghai Zhirou Chemical Co., Ltd. with the brand name AVC; acrylic acid (ester) / C10-30 alkyl acrylate cross-linked polymer is purchased from Shanghai Zhaoheng Industrial Co., Ltd. with the brand name Carbopol Ultrez 20; polyethylene glycol-240 / HDI copolymer bis-decyltetradecyl alcohol polyether-20 is purchased from Shanghai Zhaoheng Industrial Co., Ltd. with the brand name Adeka NOL GT-730.
[0083] After using the gel prepared in patent CN111419730A, the feedback was that the gel had poor adhesion to the skin. After extensive research, the applicant found that adding a certain amount of polyethylene glycol-240 / HDI copolymer bis-decyltetradecyl alcohol polyether-20 to the system can increase the viscosity of the gel. This may be because the viscosity of propylene glycol itself is relatively large. In order to achieve good moisturizing properties, more propylene glycol is added to the system, resulting in excessive solidification of the gel, which reduces the viscosity of the gel, making the gel less sticky to the skin. Polyethylene glycol- The addition of 240 / HDI copolymer bis-decyltetradecyl alcohol polyether-20 makes it synergistic with ammonium acryloyldimethyltaurate / VP copolymer and acrylic acid (ester) / C10-30 alkyl acrylate cross-linked polymer during the preparation process of the gel to make propylene glycol olefinic in the system, and the structural chain of decyltetradecyl alcohol and the structural chain of C10-30 alkyl alcohol synergistically increase the thixotropic properties of the system, allowing the system to recover quickly. At the same time, the three thickeners work synergistically in the system to make the gel have better film-forming properties, further increasing the fineness of the gel.
[0084] In order to maintain an appropriate pH value so that the gel can protect the female vulva and reproductive tract, in one embodiment, the pH regulator is at least one of sodium hydroxide, tromethamine, arginine, and meglumine; preferably, the pH regulator is tromethamine, and its CAS number is 77-86-1.
[0085] In order to make the gel have a certain cool and comfortable feeling when used, in one embodiment, the cooling agent is a combination of borneol and menthol, and the weight ratio thereof is 1:(0.08-0.15), preferably 1:0.1.
[0086] In one embodiment, the borneol is purchased from Shanghai Xier Biotechnology Co., Ltd.; the menthol is purchased from Shanghai Xier Biotechnology Co., Ltd.
[0087] In order to make the oil phase and the water phase in the system well compatible, a certain amount of oil-water mixed solvent is added in the present invention. The specific content of the oil-water mixed solvent is not specifically limited. The oil-water mixed solvent used in the present invention is PEG-40 hydrogenated castor oil, which is purchased from Shanghai Xierui Industrial Development Co., Ltd. with a brand name of CO 40.
[0088] In one embodiment, the lactic acid bacteria fermentation product is purchased from Hangzhou Ma'an New Materials Co., Ltd. with the brand name BioMAPS.
[0089] The water is not particularly limited and may be distilled water, deionized water, purified water, etc. Deionized water is used in the present invention.
[0090] The second aspect of the present invention provides a method for preparing squalene gel, comprising the following preparation steps:
[0091] (1) Add the thickener to 40 wt% water, soak for 25 min, heat to 60° C. and stir to obtain material A;
[0092] (2) stirring the pH regulator and 1 wt% water to obtain material B;
[0093] (3) melting the cooling agent and adding it to 5 wt% water, stirring evenly, and then adding an oil-water mixed solvent to obtain material C;
[0094] (4) adding 15 wt % water and lactic acid bacteria fermentation product to material C to obtain material D;
[0095] (5) Add material A and the remaining water to the main pot, stir evenly at 70°C, then cool to 45°C, add the remaining raw materials, material B, and material D, stir evenly, and vacuum homogenize to obtain squalene gel.
[0096] Specific embodiments of the present invention are given below, but the present invention is not limited by the embodiments.
[0097] In addition, unless otherwise specified, the raw materials in the present invention can be obtained from commercial sources.
[0098] Example
[0099] Example 1
[0100] A squalene gel, the raw materials of which include, by weight percentage, 8.73% of a skin conditioner, 1.54% of squalene, 1.23% of a lactic acid bacteria fermentation product, 1% of a thickener, 0.6% of a pH regulator, 0.15% of a cooling agent, 1% of an oil-water mixed solvent, and deionized water supplemented to 100%.
[0101] The skin conditioning agent comprises plant active ingredients, plant essential oils and moisturizers, and the weight ratio thereof is 3.07:0.66:5; the plant active ingredients are a combination of Stemona scabra extract, Honeysuckle flower extract, Phellodendron chinense bark extract, Cnidium monnieri extract, Sophora flavescens extract, Pulsatilla scabra extract, Salvia miltiorrhiza extract, Camellia seed extract and Coix lachryma-jobi extract, and the weight ratio thereof is 2:3:2:3:5:2:5:3:4; the Phellodendron chinense bark extract comprises Phellodendron chinense bark extract A; the Phellodendron chinense bark extract A is extracted by an alcohol extraction method;
[0102] The preparation steps of the Phellodendron bark extract A are as follows: (1) drying the Phellodendron bark medicinal material and then putting it into a grinder to grind it, and the obtained powder is sieved through a 60-mesh sieve to obtain substance A; (2) dissolving substance A in 95% ethanol by volume according to a solid-liquid ratio of 15:1 (V / W) to obtain substance B; (3) subjecting substance B to ultrasonic treatment at 150W ultrasonic power for 12 minutes at room temperature to obtain substance C; (4) subjecting substance C to reflux reaction at 70°C for 1.5 hours and then filtering to obtain filtrate D; (5) concentrating filtrate D to one-third of its volume to obtain concentrated solution E; (6) adding 95% ethanol by volume in an amount of 3 times the volume of concentrated solution E to the concentrated solution E to mix evenly, allowing the solution to settle at 4°C for 24 hours, and centrifuging at 3000 r / min for 8 minutes to retain the solid, which is substance F; (7) drying substance F to constant weight to obtain Phellodendron bark extract A;
[0103] The Phellodendron bark extract also includes Phellodendron bark extract B; the Phellodendron bark extract B is extracted by alkali extraction; the weight ratio of the Phellodendron bark extract A to the Phellodendron bark extract B is 1.65:0.78;
[0104] The preparation steps of the Phellodendron bark extract B are as follows: (1) drying the dried Phellodendron medicinal material and then putting it into a grinder to grind it, and the obtained powder is sieved through a 60-mesh sieve to obtain material A; (2) dissolving material A in a sodium hydroxide aqueous solution with a mass fraction of 1% according to a material-liquid ratio of 20:1 (V / W) to obtain material B; (3) ultrasonically treating material B at 40°C at an ultrasonic power of 300W for 15 minutes to obtain material C; (4) stirring material C at 80°C for 4 hours to obtain material D; (5) centrifuging material D at 4000r / min for 15 minutes, and retaining the supernatant to obtain material E; (6) concentrating material E to one-third of its own volume to obtain material F; (7) adding material F to material F 3 volumes of 95% ethanol were mixed evenly, allowed to settle at 4°C for 24 hours, and centrifuged at 3000 r / min for 8 minutes to obtain the solid material G; (8) Material G was dried to constant weight to obtain Phellodendron amurense bark extract B;
[0105] The plant essential oil is a combination of tea tree essential oil, patchouli essential oil, lemon essential oil, and melaleuca essential oil in a ratio of 10:3:2:10;
[0106] The moisturizing agent is propylene glycol (CAS number is 57-55-6);
[0107] The thickener includes a combination of ammonium acryloyldimethyltaurate / VP copolymer and acrylic acid (ester) / C10-30 alkyl acrylate cross-linked polymer, and the weight ratio thereof is 1:1.5; the thickener also includes polyethylene glycol-240 / HDI copolymer bis-decyltetradecyl alcohol polyether-20; the weight of the polyethylene glycol-240 / HDI copolymer bis-decyltetradecyl alcohol polyether-20 is 5% of the weight of the moisturizer;
[0108] The pH regulator is tromethamine (CAS No. 77-86-1);
[0109] The cooling agent is a combination of borneol and menthol, with a weight ratio of 1:0.1;
[0110] The oil-water mixed solvent is PEG-40 hydrogenated castor oil,
[0111] The preparation method of the squalene gel is as follows: (1) adding a thickener to 40 wt% deionized water, soaking for 25 minutes, heating to 60°C and stirring evenly to obtain material A; (2) adding a pH regulator and 1 wt% deionized water, stirring evenly to obtain material B; (3) melting a cooling agent and adding it to 5 wt% deionized water, stirring evenly, and then adding an oil-water mixed solvent to obtain material C; (4) adding 15 wt% deionized water and a lactic acid bacteria fermentation product to material C to obtain material D; (5) adding material A and the remaining deionized water to a main pot, stirring evenly at 70°C, cooling to 45°C, adding the remaining raw materials, material B, and material D, stirring evenly, and vacuum homogenizing to obtain squalene gel.
[0112] Phellodendron amurense was purchased from Shunwangcheng Chinese Medicine Market; honeysuckle flower extract was purchased from Shanghai Xier Biotechnology Co., Ltd., with the brand name of honeysuckle flower extract; creeping stemonae extract was purchased from Ganzhou Baizhentang Biological Co., Ltd., with the brand name of stemonae extract; cnidium monnieri extract was purchased from Shanghai Xier Biotechnology Co., Ltd., with the brand name of cnidium monnieri extract; sophora flavescens extract was purchased from Shanghai Xier Biotechnology Co., Ltd., with the brand name of sophora flavescens extract; pulsatilla striata extract was purchased from Shaanxi Tianzhirun Biotechnology Co., Ltd., with the brand name of pulsatilla striata extract; salvia miltiorrhiza extract was purchased from Shanghai Xier Biotechnology Co., Ltd., with the brand name of salvia miltiorrhiza extract; camellia seed extract was purchased from Ganzhou Baizhentang Biological Co., Ltd. , brand name is tea seed extract; coix seed extract was purchased from Shanghai Ou Rong Biotechnology Development Center, brand name is coix seed oil; tea tree essential oil was purchased from Wuhan Huaxiang Kejie Biotechnology Co., Ltd.; patchouli essential oil was purchased from Jinan Yunuo Chemical Co., Ltd.; lemon essential oil was purchased from Wuhan Huaxiang Kejie Biotechnology Co., Ltd.; melaleuca essential oil was purchased from Jiangxi Global Natural Flavor Co., Ltd.; squalene was purchased from Guangzhou Limeida Import and Export Trading Co., Ltd.; ammonium acryloyldimethyltaurate / VP copolymer was purchased from Shanghai Zhirou Chemical Co., Ltd., brand name is AVC; acrylic acid (ester) / C10-30 alkyl acrylate cross-linked polymer was purchased from Shanghai Zhaoheng Industrial Co., Ltd., brand name is Carbopol Ultrez 20; polyethylene glycol-240 / HDI copolymer bis-decyltetradecyl alcohol polyether-20 was purchased from Shanghai Zhaoheng Industrial Co., Ltd. with the brand name Adeka NOL GT-730; the borneol was purchased from Shanghai Xier Biotechnology Co., Ltd.; the menthol was purchased from Shanghai Xier Biotechnology Co., Ltd.; PEG-40 hydrogenated castor oil was purchased from Shanghai Xierui Industrial Development Co., Ltd. with the brand name CO 40; lactic acid bacteria fermentation products were purchased from Hangzhou Ma'an New Materials Co., Ltd. with the brand name BioMAPS.
[0113] Example 2
[0114] A squalene gel, the raw materials of which include, by weight percentage, 8.73% of a skin conditioner, 1.54% of squalene, 1.23% of a lactic acid bacteria fermentation product, 1% of a thickener, 0.6% of a pH regulator, 0.15% of a cooling agent, 1% of an oil-water mixed solvent, and deionized water supplemented to 100%.
[0115] The skin conditioning agent comprises plant active ingredients, plant essential oils and moisturizers, and the weight ratio thereof is 3.07:0.66:5; the plant active ingredients are a combination of Stemona japonica extract, Honeysuckle flower extract, Phellodendron chinense bark extract, Cnidium monnieri extract, Sophora flavescens extract, Pulsatilla scabra extract, Salvia miltiorrhiza extract, Camellia seed extract and Coix lachryma-jobi extract, and the weight ratio thereof is 2:3:2:3:5:2:5:3:4; the plant essential oils are a combination of Tea Tree essential oil, Patchouli essential oil, Lemon essential oil and Melaleuca alternifolia essential oil, and the weight ratio thereof is 10:3:2:10;
[0116] The moisturizing agent is the same as in Example 1; the thickener is the same as in Example 1; the pH adjusting agent is the same as in Example 1; the cooling agent is the same as in Example 1; the oil-water mixed solvent is the same as in Example 1;
[0117] The preparation method of the squalene gel is the same as that of Example 1.
[0118] Phellodendron bark extract was purchased from Shanghai Xier Biotechnology Co., Ltd. under the brand name Phellodendron extract; Lonicera japonica extract was purchased from Shanghai Xier Biotechnology Co., Ltd. under the brand name Lonicera japonica extract; Stemona radiata extract was purchased from Ganzhou Baizhentang Biological Co., Ltd. under the brand name Stemona radiata extract; Cnidium monnieri extract was purchased from Shanghai Xier Biotechnology Co., Ltd. under the brand name Cnidium monnieri extract; Sophora flavescens extract was purchased from Shanghai Xier Biotechnology Co., Ltd. under the brand name Sophora flavescens extract; Pulsatilla striata extract was purchased from Shaanxi Tianzhirun Biotechnology Co., Ltd. under the brand name Pulsatilla striata extract; Salvia miltiorrhiza extract was purchased from Shanghai Xier Biotechnology Co., Ltd. under the brand name Salvia miltiorrhiza extract; Camellia seed extract was purchased from Ganzhou Baizhentang Biological Co., Ltd. under the brand name Tea seed extract; Coix seed extract was purchased from Shanghai Ou Rong Biotechnology Development Center under the brand name Coix seed oil; Squalene was purchased from Guangzhou Limeida Import and Export Trading Co., Ltd.; lactic acid bacteria fermentation products were purchased from Hangzhou Ma'an New Materials Co., Ltd. under the brand name BioMAPS.
[0119] Example 3
[0120] A squalene gel, the raw materials of which include, by weight percentage, 8.73% of a skin conditioner, 1.54% of squalene, 1.23% of a lactic acid bacteria fermentation product, 1% of a thickener, 0.6% of a pH regulator, 0.15% of a cooling agent, 1% of an oil-water mixed solvent, and deionized water supplemented to 100%.
[0121] The skin conditioning agent includes plant active ingredients, plant essential oils, and moisturizers in a weight ratio of 3.07:0.66:5;
[0122] The plant active ingredients are a combination of Stemona japonica extract, Honeysuckle flower extract, Phellodendron chinense bark extract, Cnidium monnieri extract, Sophora flavescens extract, Pulsatilla scabra extract, Salvia miltiorrhiza extract, Camellia japonica seed extract, and Coix lachryma-jobi seed extract, and the weight ratio thereof is 2:3:2:3:5:2:5:3:4;
[0123] The Phellodendron bark extract is Phellodendron bark extract B; the Phellodendron bark extract B is the same as in Example 1; the plant essential oil is the same as in Example 1; the moisturizer is the same as in Example 1; the thickener is the same as in Example 1; the pH adjuster is the same as in Example 1; the cooling agent is the same as in Example 1; the oil-water mixed solvent is the same as in Example 1;
[0124] The preparation method of the squalene gel is the same as that of Example 1.
[0125] Phellodendron chinense was purchased from Shunwangcheng Chinese Medicine Market; honeysuckle flower extract was purchased from Shanghai Xier Biotechnology Co., Ltd. under the brand name of honeysuckle extract; Stemona bud extract was purchased from Ganzhou Baizhentang Biological Co., Ltd. under the brand name of Stemona bud extract; Cnidium monnieri extract was purchased from Shanghai Xier Biotechnology Co., Ltd. under the brand name of Cnidium monnieri extract; Sophora flavescens extract was purchased from Shanghai Xier Biotechnology Co., Ltd. under the brand name of Sophora flavescens extract; Pulsatilla striata extract was purchased from Shaanxi Tianzhirun Biotechnology Co., Ltd. under the brand name of Pulsatilla striata extract; Salvia miltiorrhiza extract was purchased from Shanghai Xier Biotechnology Co., Ltd. under the brand name of Salvia miltiorrhiza extract; Camellia seed extract was purchased from Ganzhou Baizhentang Biological Co., Ltd. under the brand name of tea seed extract; Coix seed extract was purchased from Shanghai Ou Rong Biotechnology Development Center under the brand name of coix seed oil; squalene was purchased from Guangzhou Limeida Import and Export Trading Co., Ltd.; lactic acid bacteria fermentation products were purchased from Hangzhou Ma'an New Materials Co., Ltd. under the brand name of BioMAPS.
[0126] Example 4
[0127] A squalene gel, the raw materials comprising, by weight percentage, 8.73% of a skin conditioner, 1.54% of squalene, 1.23% of a lactic acid bacteria fermentation product, 1% of a thickener, 0.6% of a pH regulator, 0.15% of a cooling agent, 1% of an oil-water mixed solvent, and deionized water supplemented to 100%;
[0128] The skin conditioning agent is the same as in Example 1; the moisturizing agent is the same as in Example 1; the pH adjusting agent is the same as in Example 1; the cooling agent is the same as in Example 1; the oil-water mixed solvent is the same as in Example 1;
[0129] The thickener includes a combination of ammonium acryloyldimethyltaurate / VP copolymer and acrylic acid (ester) / C10-30 alkyl acrylate cross-linked polymer, with a weight ratio of 1:1.5;
[0130] The preparation method of the squalene gel is the same as that of Example 1.
[0131] Squalene was purchased from Guangzhou Limeida Import and Export Trading Co., Ltd.; ammonium acryloyldimethyltaurate / VP copolymer was purchased from Shanghai Zhirou Chemical Co., Ltd. with the brand name AVC; acrylic acid (esters) / C10-30 alkyl acrylate cross-linked polymer was purchased from Shanghai Zhaoheng Industrial Co., Ltd. with the brand name Carbopol Ultrez 20; lactic acid bacteria fermentation products were purchased from Hangzhou Ma'an New Materials Co., Ltd. with the brand name BioMAPS.
[0132] Example 5
[0133] A squalene gel, the raw materials comprising, by weight percentage, 8.73% of a skin conditioner, 1.54% of squalene, 1.23% of a lactic acid bacteria fermentation product, 1% of a thickener, 0.6% of a pH regulator, 0.15% of a cooling agent, 1% of an oil-water mixed solvent, and deionized water supplemented to 100%;
[0134] The skin conditioning agent is the same as in Example 1; the moisturizing agent is the same as in Example 1; the pH is the same as in Example 1; the cooling agent is the same as in Example 1; the oil-water mixed solvent is the same as in Example 1;
[0135] The thickener is ammonium acryloyldimethyltaurate / VP copolymer; the thickener also includes polyethylene glycol-240 / HDI copolymer bis-decyltetradecyl alcohol polyether-20; the weight of the polyethylene glycol-240 / HDI copolymer bis-decyltetradecyl alcohol polyether-20 is 5% by weight of the moisturizer;
[0136] The squalene gel is the same as that in Example 1.
[0137] Squalene was purchased from Guangzhou Limeida Import and Export Trading Co., Ltd.; ammonium acryloyldimethyltaurate / VP copolymer was purchased from Shanghai Zhirou Chemical Co., Ltd. with the brand name AVC; polyethylene glycol-240 / HDI copolymer di-decyltetradecyl alcohol polyether-20 was purchased from Shanghai Zhaoheng Industrial Co., Ltd. with the brand name Adeka NOL GT-730; lactic acid bacteria fermentation products were purchased from Hangzhou Ma'an New Materials Co., Ltd. with the brand name BioMAPS.
[0138] Performance Testing
[0139] 1. Take 6 g of the gel in each example and spread it on a 12 square centimeter (3 cm×4 cm) smooth rectangular glass plate, then touch it with your hand to see if it feels smooth.
[0140] 2. Take 6 g of the gel in the example and evenly spread it on the same glass slide (the area of the glass slide is 25 square centimeters). The spread area is 8 square centimeters. After shaking the glass slide 5 times with the same force, record the area A1 of the gel on the glass slide.
[0141] The test results are shown in Table 1:
[0142] Table 1
[0143] Fineness <![CDATA[A1(cm 2 )]]> Example 1 exquisite 9.2 Example 2 Rough 10 Example 3 Rough 10.4 Example 4 More delicate 18.6 Example 5 exquisite 16.4
[0144] The foregoing examples are merely illustrative and are used to explain some features of the method of the present invention. The appended claims are intended to claim the widest possible range that can be conceived, and the embodiments presented herein are only illustrations of selected implementations according to the combination of all possible embodiments. Therefore, it is the applicant's intention that the appended claims are not limited by the selection of examples that illustrate the features of the present invention. Some numerical ranges used in the claims also include sub-ranges within them, and changes in these ranges should also be interpreted as being covered by the appended claims where possible.
Claims
1. A squalene gel, characterized in that: The raw materials include, by weight percentage: 8.73% skin conditioner, 1.54% squalene, 1.23% lactic acid bacteria fermentation product, 1% thickener, 0.6% pH adjuster, 0.15% cooling agent, 1% oil-water mixed solvent, and deionized water supplemented to 100%; The skin conditioning agent comprises plant active ingredients, plant essential oils and moisturizers, and the weight ratio thereof is 3.07:0.66:5; the plant active ingredients are a combination of Stemona japonica extract, Honeysuckle flower extract, Phellodendron chinense bark extract, Cnidium monnieri extract, Sophora flavescens extract, Pulsatilla scabra extract, Salvia miltiorrhiza extract, Camellia seed extract and Coix lachryma-jobi seed extract, and the weight ratio thereof is 2:3:2:3:5:2:5:3:4; The Phellodendron bark extract includes Phellodendron bark extract A; the Phellodendron bark extract A is obtained by alcohol extraction; The preparation steps of the Phellodendron bark extract A are as follows: (1) drying the Phellodendron bark medicinal material and then putting it into a grinder to grind it, and the obtained powder is sieved through a 60-mesh sieve to obtain substance A; (2) dissolving substance A in 95% ethanol by volume according to a solid-liquid ratio of 15:1 (V / W) to obtain substance B; (3) subjecting substance B to ultrasonic treatment at 150W ultrasonic power for 12 minutes at room temperature to obtain substance C; (4) subjecting substance C to reflux reaction at 70°C for 1.5 hours and then filtering to obtain filtrate D; (5) concentrating filtrate D to one-third of its volume to obtain concentrated solution E; (6) adding 95% ethanol by volume in an amount of 3 times the volume of concentrated solution E to the concentrated solution E to mix evenly, allowing the solution to settle at 4°C for 24 hours, and centrifuging at 3000 r / min for 8 minutes to retain the solid, which is substance F; (7) drying substance F to constant weight to obtain Phellodendron bark extract A; The Phellodendron bark extract also includes Phellodendron bark extract B; the Phellodendron bark extract B is extracted by alkali extraction; the weight ratio of the Phellodendron bark extract A to the Phellodendron bark extract B is 1.65:0.78; The preparation steps of the Phellodendron bark extract B are as follows: (1) drying the dried Phellodendron medicinal material and then putting it into a grinder to grind it, and the obtained powder is sieved through a 60-mesh sieve to obtain material A; (2) dissolving material A in a sodium hydroxide aqueous solution with a mass fraction of 1% according to a material-liquid ratio of 20:1 (V / W) to obtain material B; (3) ultrasonically treating material B at 40°C at an ultrasonic power of 300W for 15 minutes to obtain material C; (4) stirring material C at 80°C for 4 hours to obtain material D; (5) centrifuging material D at 4000r / min for 15 minutes, and retaining the supernatant to obtain material E; (6) concentrating material E to one-third of its own volume to obtain material F; (7) adding material F to material F 3 volumes of 95% ethanol were mixed evenly, allowed to settle at 4°C for 24 hours, and centrifuged at 3000 r / min for 8 minutes to obtain the solid material G; (8) Material G was dried to constant weight to obtain Phellodendron amurense bark extract B; The plant essential oil is a combination of tea tree essential oil, patchouli essential oil, lemon essential oil, and melaleuca essential oil in a ratio of 10:3:2:10; The moisturizing agent is propylene glycol; The thickener includes a combination of ammonium acryloyldimethyltaurate / VP copolymer and acrylic acid (ester) / C10-30 alkyl acrylate cross-linked polymer, and the weight ratio thereof is 1:1.5; the thickener also includes polyethylene glycol-240 / HDI copolymer bis-decyltetradecyl alcohol polyether-20; the weight of the polyethylene glycol-240 / HDI copolymer bis-decyltetradecyl alcohol polyether-20 is 5% of the weight of the moisturizer; The pH regulator is tromethamine; The cooling agent is a combination of borneol and menthol, with a weight ratio of 1:0.1; The oil-water mixed solvent is PEG-40 hydrogenated castor oil; The preparation method of squalene gel comprises the following preparation steps: (1) adding the thickener into 40 wt% deionized water, soaking for 25 min, heating at 60° C. and stirring to obtain material A; (2) mixing a pH regulator and 1 wt% deionized water, and uniformly stirring to obtain material B; (3) melting the cooling agent and adding it into 5 wt% deionized water, stirring evenly, and then adding an oil-water mixed solvent to obtain material C; (4) adding 15 wt % deionized water and lactic acid bacteria fermentation product to material C to obtain material D; (5) Add material A and the remaining deionized water to the main pot, stir evenly at 70°C, then cool to 45°C, add the remaining raw materials, material B, and material D, stir evenly, and vacuum homogenize to obtain squalene gel.
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