Bicontinuous-phase cleansing oil and preparation method thereof
By using a bicontinuous phase cleansing oil preparation method, a stable three-dimensional network structure is formed by surfactants and anti-inflammatory and moisturizing ingredients are added. This solves the problems of poor cleansing effect and skin sensitivity of traditional cleansing oils, achieving highly efficient cleansing, no residue and moisturizing effect.
Patent Information
- Application Number
- CN202511459391.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-10-13
- Publication Date
- 2025-11-28
AI Technical Summary
Existing cleansing oils have limited effectiveness in removing waterproof makeup, tend to leave an oil film, and may contain irritating ingredients that can cause skin sensitivity or allergies.
The cleansing oil is prepared using a bicontinuous phase method. Surfactants such as PEG-7 glyceryl cocoate and PEG-20 glyceryl triisostearate form a three-dimensional network structure in which oil channels and water channels interpenetrate. Combined with ingredients such as cetyl ethylhexanoate and isododecane, the oil and water phases are stably mixed. Gentiana macrophylla extract and Cordyceps sinensis mycelium powder are added to provide anti-inflammatory and moisturizing effects.
It effectively removes stubborn makeup without leaving a greasy residue, has low skin irritation, and provides good moisturizing effects, making it suitable for sensitive skin.
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Abstract
Description
Technical Field
[0001] This application relates to the technical field of daily cosmetics, and in particular to a bicontinuous phase makeup remover oil and its preparation method. The makeup remover oil has a bicontinuous structure of aqueous and oil phases, which can effectively remove makeup, while also having the functions of gentleness, moisturizing and repairing the skin barrier. Background Technology
[0002] In recent years, bicontinuous phase structures have attracted attention in the cosmetics field. A bicontinuous phase refers to the simultaneous and continuous existence of an aqueous phase and an oil phase, forming an interconnected network structure. This structure can leverage the advantages of both aqueous and oil phases, exhibiting excellent cleansing power and gentleness. However, existing research on bicontinuous phase makeup removers is limited, and existing technologies suffer from problems such as poor stability and complex preparation processes.
[0003] Traditional cleansing oils are primarily oil-based, achieving their makeup-removing function through emulsification. However, these products have the following problems: (1) They have limited effectiveness in removing waterproof makeup, requiring repeated wiping; (2) They tend to leave an oil film after use, requiring secondary cleansing and increasing the burden on the skin; (3) Some products contain irritating ingredients, which can easily lead to skin sensitivity or allergies. Summary of the Invention
[0004] In order to improve the problems of poor makeup removal effect, easy residue and easy skin allergy caused by traditional makeup remover oil, this application provides a bicontinuous phase makeup remover oil and its preparation method.
[0005] This application provides a dual continuous-phase cleansing oil, employing the following technical solution: A bicontinuous phase cleansing oil, comprising, by weight percentage, component A and component B, wherein component A comprises: 1-10% PEG-7 glyceryl cocoate, 10-20% PEG-20 glyceryl triisostearate, 10-30% cetyl ethylhexanoate, 10-30% cocoyl octanoate / caprylate, and 10-20% isododecane; Component B: 1-15% methyl propylene glycol, 1-10% glycerin, 0.5-2% Gentiana macrophylla extract, 1-10% butylene glycol, 0.5-2% 1,2-hexanediol, 0.5-3% 1,2-pentanediol, 0.5-2% Cordyceps sinensis mycelium powder, water balance.
[0006] By employing the above technical solution, in component A, PEG-7 glyceryl cocoate can combine oily components with water to form a stable emulsion, promoting ingredient absorption. It also effectively cleanses dirt and makeup residue from the skin surface and has excellent moisturizing effects, increasing skin hydration. PEG-20 glyceryl triisostearate has excellent emulsifying properties, quickly dissolving makeup and dirt, making makeup removal easier and more thorough, while also providing moisturizing effects. When component A (oil phase) and component B (aqueous phase) are mixed, these two surfactants work synergistically to form a continuous and stable three-dimensional network structure where oil and water channels interpenetrate, i.e., a bicontinuous phase.
[0007] Cetyl ethylhexanoate possesses excellent breathability, spreadability, dispersibility, and moisturizing properties, allowing for rapid absorption into the skin without leaving a greasy residue. It also helps other active ingredients penetrate the skin more effectively. Cocoyl caprylate / caprylate has excellent spreadability and superior moisturizing effects, excellent skin compatibility, is non-irritating, has low viscosity, and improves the product's feel. Isododecane has good volatility and solubility, evaporating quickly to prevent a greasy residue after use, while also helping to dissolve makeup and dirt. The combination of these three components results in a smooth, oily texture that is easy to apply, dissolving and penetrating makeup. However, after a few seconds, the isododecane evaporates, leaving the skin feeling exceptionally dry. Oil phase components: PEG-7 glyceryl cocoate, PEG-20 glyceryl triisostearate, cetyl ethylhexanoate, coconut caprylate / caprylate, isododecane, etc., serve as the oil phase, possessing excellent makeup and sebum-dissolving abilities. These components form a continuous oil phase network through intermolecular interactions. Emulsification: PEG-7 glyceryl cocoate and PEG-20 glyceryl triisostearate, as nonionic surfactants, can reduce the interfacial tension between the oil phase and the aqueous phase, promote the uniform mixing of the oil phase and the aqueous phase, and form a bicontinuous phase structure.
[0008] In component B, methylpropanediol has low volatility and viscosity, which helps dissolve other ingredients and also provides some moisturizing effects. Glycerin has strong hygroscopic properties, absorbing moisture from the air and keeping the skin soft and elastic. Gentiana macrophylla extract has anti-inflammatory and antioxidant effects, which may help relieve skin inflammation and protect the skin from oxidative damage. Butylene glycol has moisturizing effects, helping to keep the skin hydrated, improve skin quality, and dissolve other ingredients. 1,2-Hexanediol and 1,2-Pentanediol have a mild sweet scent, antibacterial properties, and act as moisturizers and penetration enhancers. Cordyceps sinensis mycelium powder can promote the activity of immune cells, help enhance the body's immunity, and also has antioxidant effects, helping to slow down the cellular aging process and protect the skin. Aqueous phase components: Methylpropanediol, glycerin, butylene glycol, 1,2-hexanediol, 1,2-pentanediol, and other polyols form the aqueous phase, providing good moisturizing and gentle properties. These components form a continuous aqueous network through hydrogen bonding.
[0009] Gentian root extract has anti-inflammatory and soothing effects, relieving skin irritation that may occur during makeup removal, making it suitable for sensitive skin. Cordyceps mycelium powder is rich in polysaccharides, amino acids, and other active ingredients, possessing antioxidant properties and repairing the skin barrier, thus enhancing the skin's resistance. Moisturizing ingredients: Glycerin, butylene glycol, 1,2-hexanediol, 1,2-pentanediol, and other polyols have excellent moisturizing properties, providing long-lasting hydration after makeup removal and preventing dryness.
[0010] Components A and B are mixed. In component A, PEG-20 glyceryl triisostearate and PEG-7 glyceryl cocoate, these surfactant molecules, are uniformly dissolved in the oil. When component B (aqueous phase) is added, the oil and aqueous phases are dispersed into tiny regions. The surfactant molecules arrange themselves in an orderly manner at the oil-water interface, assembling into a three-dimensional network structure where oil and water channels intertwine, interweave, and are continuously interconnected. Upon use, this provides instant emulsification, easy rinsing, a refreshing feel, and delivers the effective ingredients for comprehensive cleansing.
[0011] Stability of the bicontinuous phase structure: By precisely controlling the ratio of the oil phase to the water phase, as well as the amount of surfactant, the bicontinuous phase structure remains stable during storage and use, preventing stratification or deterioration. Antioxidant and preservative properties: 1,2-Hexanediol and 1,2-Pentanediol not only have moisturizing effects but also preservative and antioxidant functions, which can extend the product's shelf life.
[0012] Dissolving Makeup: The oil phase effectively dissolves oil-soluble makeup (such as foundation, mascara, lipstick, etc.), while the water phase dissolves water-soluble makeup (such as eyeliner, water-soluble dirt, etc.). The dual continuous phase structure allows the oil and water phases to work simultaneously, achieving a comprehensive makeup removal effect.
[0013] Emulsifying Cleansing: When the cleansing oil comes into contact with the skin and is massaged, makeup and dirt are dissolved in the oil phase. Subsequently, after adding a small amount of water, the surfactants (PEG-7 glyceryl cocoate and PEG-20 glyceryl triisostearate) come into play, encapsulating the oil phase to form tiny droplets, separating the oil and water phases, making it easy to rinse off with water.
[0014] Lightweight Texture: The use of light oils such as isododecane and cetyl ethylhexanoate makes the cleansing oil lightweight, easy to apply and massage, and non-greasy on the skin. Rapid Emulsification: The excellent emulsifying properties of PEG-7 glyceryl cocoate and PEG-20 glyceryl triisostearate allow the cleansing oil to emulsify quickly upon contact with water, making it easy to rinse and reducing residue.
[0015] The bicontinuous-phase cleansing oil of this application, through its unique bicontinuous-phase structure, combines highly effective cleansing, soothing, and moisturizing ingredients to achieve multiple benefits including efficient makeup removal, gentle cleansing, and long-lasting hydration. Its preparation method is simple, suitable for industrial production, and has broad market application prospects.
[0016] Preferably, the mass ratio of PEG-7 glyceryl cocoate to PEG-20 glyceryl triisostearate is 1:8-13.
[0017] By employing the above technical solution and further limiting the mass ratio of PEG-7 glyceryl cocoate and PEG-20 glyceryl triisostearate within a certain range, the resulting oil phase exhibits excellent makeup removal performance. PEG-20 glyceryl triisostearate (lipophilic end) is highly compatible with oils and makeup, effectively dissolving them. EG-7 glyceryl cocoate (hydrophilic end) ensures that dissolved makeup and dirt can be carried away by water. The combination of the two provides both the strong dissolving power of oil-based systems and the easy cleansing properties of water-based systems, resulting in a light, smooth, and non-sticky skin feel. After rinsing, the skin feels clean, breathable, and without any oily residue.
[0018] Preferably, the mass ratio of Gentiana macrophylla extract, Cordyceps sinensis mycelium powder, and methyl propylene glycol is 1:1:10-20.
[0019] By employing the above technical solution and further limiting the mass ratio of Gentiana macrophylla extract, Cordyceps sinensis mycelium powder, and methyl propylene glycol, the resulting aqueous phase exhibits comprehensive effects. Gentiana macrophylla extract possesses anti-inflammatory and antioxidant properties, alleviating skin redness and mild burning sensations caused by massage friction or makeup residue during makeup removal. Cordyceps sinensis mycelium powder forms a thin moisturizing film on the skin surface, reducing rapid moisture loss after cleansing and replenishing natural moisturizing factors. Methyl propylene glycol rapidly dissolves the effective monomers of both active ingredients, forming a homogeneous and stable solution, preventing the active substances from agglomerating and failing to exert their effects; it also promotes the penetration of active ingredients, allowing the anti-inflammatory components of Gentiana macrophylla extract and the polysaccharides of Cordyceps sinensis mycelium powder to function more effectively.
[0020] Preferably, the pretreatment of Gentiana macrophylla extract includes the following: (1) Disperse Gentiana macrophylla extract, aloe polysaccharide, modified nanoporous silica and sodium hyaluronate in deionized water and stir evenly to obtain core material; (2) Disperse sodium alginate, gum arabic, soybean lecithin, glycerin and PEG600 in deionized water and stir evenly at 70-75℃ to obtain wall material; (3) Mix the core material and wall material, homogenize, and spray dry to obtain Gentiana macrophylla extract microcapsules.
[0021] By adopting the above technical solution, Gentiana macrophylla extract provides anti-inflammatory and soothing effects. Aloe polysaccharides and sodium hyaluronate increase the viscosity of the aqueous phase, preventing the aggregation of Gentiana macrophylla extract and modified nanoporous silica. Modified nanoporous silica has a huge specific surface area, which adsorbs active molecules such as Gentiana macrophylla extract. In subsequent use, it plays a certain role in the slow release of active substances, prolonging the effect of active ingredients.
[0022] Sodium alginate combined with gum arabic enhances the film-forming properties and emulsion stability of the system. Soy lecithin reduces the oil-water interfacial tension, helping to form finer and more stable emulsion droplets during homogenization. Its phospholipid structure is similar to that of skin cell membranes, promoting transdermal absorption of active ingredients. Glycerin and PEG600 increase the flexibility of the membrane wall, preventing it from becoming too brittle and prone to cracking after spray drying.
[0023] The core material and wall material are mixed and homogenized. The aqueous phase containing the active ingredient is dispersed into extremely small droplets, which are then uniformly suspended in the wall material solution. Spray drying yields a free-flowing powder.
[0024] During makeup removal, moisture on the skin's surface slowly penetrates into the microcapsule wall material, causing the cross-linked structure of the wall material to swell slightly. At this time, the active ingredients (Gentiana macrophylla extract and aloe polysaccharide) can be slowly released to the skin surface through the pores of the wall material. This avoids local irritation caused by a one-time release and allows the active ingredients to continuously exert a soothing and moisturizing effect throughout the makeup removal process, relieving skin discomfort caused by makeup removal friction.
[0025] Preferably, the mass ratio of Gentiana macrophylla extract, modified nanoporous silica, and sodium hyaluronate is 1:0.62-0.75:0.26-0.41.
[0026] By employing the above technical solution and further limiting the mass ratio of Gentiana macrophylla extract, modified nanoporous silica, and sodium hyaluronate, the resulting Gentiana macrophylla extract microcapsules exhibit superior stability and makeup-removing effect. The modified nanoporous silica contains numerous nanoscale pores, providing ample adhesion space for Gentiana macrophylla extract molecules and significantly increasing the active ingredient loading of the final microcapsules. The active ingredients of Gentiana macrophylla extract (such as gentiopicroside) are adsorbed by silica and interact with sodium hyaluronate to jointly form the core material of the microcapsules. Sodium hyaluronate increases the viscosity of the aqueous phase, helping to suspend and stabilize the extract particles adsorbed by silica, preventing precipitation and resulting in a more uniform mixing system.
[0027] Gentian root extract is responsible for temporarily opening the skin barrier and stimulating local inflammation. Modified nanoporous silica is responsible for instantly absorbing makeup and releasing a high concentration of bitter glycosides. Sodium hyaluronate is responsible for locking water in the skin and carrying the bitter glycosides deeper. When these three are combined, makeup removal is more thorough, soothing is faster, and moisturizing is longer-lasting.
[0028] Preferably, the homogenization pressure is 20-30 MPa and the time is 30-35 min.
[0029] By adopting the above technical solution and setting homogeneous conditions, the obtained powder particles have better uniformity, water content, morphology and retention of active ingredients, which helps to improve the subsequent makeup removal effect.
[0030] Preferably, the method for preparing the modified nanoporous silica includes the following steps: The nanoporous silica was dispersed in hydrochloric acid solution, soaked for 10-15 min, washed with water, calcined at 300-350℃ for 30-35 min, then dispersed in silane coupling agent aqueous solution, hexadecyltrimethylammonium bromide was added, filtered, washed with water, dried, and then impregnated in alginate solution and dried to obtain modified nanoporous silica. Preparation of alginate solution: Disperse alginate in deionized water, add treated polyvinyl alcohol fiber, sodium dodecylbenzene sulfonate, and ascorbic acid, stir for 1-2 hours to obtain alginate solution; Polyvinyl alcohol fibers are cut to a length of 0.1-0.15 mm to obtain treated polyvinyl alcohol fibers.
[0031] By employing the above technical solution, hydrochloric acid dissolves impurities that may exist in the pores and surface of silica, and protonates the silanol groups on the surface, making them more reactive. Calcination removes moisture and organic contaminants from the pores, opens the pores, and significantly increases the density of surface silanol groups, which facilitates subsequent reactions.
[0032] One end of the silane coupling agent molecule can covalently bond with the silanol groups on the silica surface, while the long organic chain at the other end extends outward. This film changes the silica surface from hydrophilic to hydrophobic. Hexadecyltrimethylammonium bromide is used to modify the hydrophobic silica surface, enhancing its hydrophobic properties.
[0033] PVA fibers were shortened to 0.1-0.15 mm and processed at high speed using a pulper to fibrillate them, resulting in PVA microfibers with smaller diameters and larger specific surface areas. This significantly improved their entanglement with alginate molecules, acting as a reinforcing phase to significantly enhance the mechanical strength and toughness of the coating and prevent cracking. Sodium dodecylbenzenesulfonate facilitated the dispersion of PVA microfibers and the wetting and encapsulation of the hydrophobic silica surface by the alginate solution. Ascorbic acid provided antioxidant properties, protecting the active ingredients in the system. Modified nanoporous silica exhibited a higher loading capacity for Gentiana macrophylla extract, better dispersion stability in the oil phase of the makeup remover, and more effective protection for the Gentiana macrophylla extract.
[0034] Preferably, the method for preparing the polyvinyl alcohol fiber includes the following steps: Polyvinyl alcohol is dispersed in deionized water and stirred at 80-85℃ for 30-35 minutes. The resulting polyvinyl alcohol solution is degassed under vacuum, and inulin, sodium carboxymethyl cellulose, and preservative are added. The solution is then sonicated for 1-2 hours to obtain a spinning solution. The spinning solution is then spun, hot-stretched, and cooled to room temperature to obtain polyvinyl alcohol fibers.
[0035] By employing the above technical solution, vacuum degassing removes air bubbles entangled in the solution during stirring, which can cause fiber breakage or defects during spinning. Inulin forms a microstructure within the fiber, increasing its hygroscopicity or providing space for subsequent drug loading. Sodium carboxymethyl cellulose adjusts the rheological properties of the spinning solution, making it easier to spin. The resulting spinning solution is spun, stretched, and then polyvinyl alcohol (PVA) fibers are obtained. The resulting PVA fibers exhibit good flexibility, which contributes to the stability of subsequent microcapsules.
[0036] During the makeup removal process, the network formed by polyvinyl alcohol fibers helps to break down stubborn makeup more quickly by physically encapsulating it and working synergistically with surfactants.
[0037] Secondly, this application also provides a method for preparing a bicontinuous phase cleansing oil, comprising the following steps: mixing PEG-7 glyceryl cocoate, PEG-20 glyceryl triisostearate, cetyl ethylhexanoate, cocoyl octanoate / decanoate, and isododecane, stirring evenly at a stirring speed of 10-20 r / min, then adding methyl propylene glycol, glycerin, Gentiana macrophylla extract, butylene glycol, 1,2-hexanediol, 1,2-pentanediol, Cordyceps sinensis mycelium powder, and water, stirring evenly, and filtering with a 100-200 mesh filter cloth to obtain the bicontinuous phase cleansing oil.
[0038] By adopting the above technical solution and preparation method, the operation is simple and helps to improve the stability and makeup removal performance of the prepared bicontinuous phase makeup remover oil. The resulting bicontinuous phase makeup remover oil has good practicality.
[0039] In summary, this application has the following beneficial effects: 1. This application can effectively remove stubborn makeup such as waterproof mascara and lipstick. It has passed skin irritation tests and no adverse reactions such as redness, swelling or itching have occurred. After use, the skin's moisture content increases by 25%-35%.
[0040] 2. The bicontinuous-phase cleansing oil in this application is based on the principle of bicontinuous-phase microemulsions. Through specific ingredient combinations and preparation processes, a unique microstructure is formed. A bicontinuous-phase microemulsion is a system that simultaneously possesses a continuous structure of oil and water phases. The oil and water phases intertwine at the microscale, forming a three-dimensional network structure. This structure enables the cleansing oil to dissolve both water-soluble and oil-soluble makeup and dirt, achieving a highly effective cleansing effect.
[0041] 3. In this application, when component B (aqueous phase) is added, the oil phase and aqueous phase are dispersed into tiny regions, and surfactant molecules are arranged and assembled in an orderly manner at the oil and water interface to form a three-dimensional network structure in which oil channels and water channels are intertwined, interwoven and continuously connected. Detailed Implementation
[0042] The present application will be further described in detail below with reference to the embodiments.
[0043] The raw materials used in the examples and comparative examples are all commercially available.
[0044] Preparation example of pretreatment of Gentiana macrophylla extract Preparation Example 1-1 Pretreatment of Gentiana macrophylla extract includes the following: (1) Disperse 10kg of Gentiana macrophylla extract, 2kg of aloe polysaccharide, modified nanoporous silica and sodium hyaluronate in 55L of deionized water and stir evenly to obtain the core material; (2) Disperse 20kg sodium alginate, 15kg gum arabic, 4kg soybean lecithin, 6kg glycerin and 2kg PEG600 in 60L deionized water and stir evenly at 72℃ to obtain wall material; (3) Mix 5 kg of core material and 25 kg of wall material, homogenize, and spray dry to obtain Gentiana macrophylla extract microcapsules.
[0045] The mass ratio of Gentiana macrophylla extract, modified nanoporous silica, and sodium hyaluronate was 1:0.62:0.26.
[0046] The homogenization pressure was 25 MPa, and the time was 32 min.
[0047] The conditions for spray drying are: inlet air temperature 155℃, outlet air temperature 80℃, feed flow rate 20mL / min, and spray air flow rate 660L / h.
[0048] The preparation method of modified nanoporous silica includes the following steps: 8 kg of nanoporous silica was dispersed in 15 L of 3% hydrochloric acid solution, soaked for 13 min, washed with water, calcined at 320 °C for 33 min, then dispersed in 20 L of 2% silane coupling agent KH550 aqueous solution, 1 kg of hexadecyltrimethylammonium bromide was added, filtered, washed with water, dried, and then impregnated in alginate solution and dried to obtain modified nanoporous silica. Preparation of alginate solution: 2 kg of alginate was dispersed in 10 L of deionized water, and 0.6 kg of treated polyvinyl alcohol fiber, 0.1 kg of sodium dodecylbenzenesulfonate and 0.3 kg of ascorbic acid were added. The mixture was stirred for 1.5 h to obtain alginate solution. Polyvinyl alcohol fibers were cut to a length of 0.1 mm and processed by a refining machine at 3000 rpm for 3 times to obtain treated polyvinyl alcohol fibers.
[0049] The preparation method of polyvinyl alcohol fiber includes the following steps: 1.5 kg of polyvinyl alcohol was dispersed in 5 L of deionized water and stirred at 82 °C for 33 min to obtain a polyvinyl alcohol solution. The solution was then degassed under vacuum (-0.09 MPa, 60 °C for 15 min), and 0.9 kg of inulin, 0.2 kg of sodium carboxymethyl cellulose, and 0.05 kg of preservative (phenoxyethanol) were added. The solution was sonicated for 1.5 h to obtain a spinning solution. The spinning solution was spun at 25 °C with a flow rate of 3 mL / h. The coagulation bath was methanol / water = 70 / 30 (v / v) at 10 °C. The solution was then hot-stretched at 120 °C to a length 1.2 times the initial fiber length. The solution was cooled to room temperature to obtain polyvinyl alcohol fibers.
[0050] Preparation Examples 1-2 The difference from Preparation Example 1-1 is that no modified nanoporous silica is added.
[0051] Preparation Examples 1-3 The difference from Preparation Example 1-1 is that sodium hyaluronate is not added.
[0052] Preparation Examples 1-4 The difference from Preparation Example 1-1 is that the mass ratio of Gentiana macrophylla extract, modified nanoporous silica, and sodium hyaluronate is 1:0.75:0.41.
[0053] Preparation Examples 1-5 The difference from Preparation Example 1-1 is that the mass ratio of Gentiana macrophylla extract, modified nanoporous silica, and sodium hyaluronate is 1:0.1:0.8.
[0054] Preparation Examples 1-6 The difference from Preparation Example 1-1 is that no alginate solution is added in the preparation method of modified nanoporous silica.
[0055] Preparation Examples 1-7 The difference from Preparation Example 1-1 is that polyvinyl alcohol fibers are not added in the preparation method of modified nanoporous silica.
[0056] Preparation Examples 1-8 The difference from Preparation Example 1-1 is that in the preparation method of polyvinyl alcohol fiber, inulin is not added.
[0057] Preparation Examples 1-9 The difference from Preparation Example 1-1 is that sodium carboxymethyl cellulose is not added in the preparation method of polyvinyl alcohol fiber. Example
[0058] Example 1 A bicontinuous phase cleansing oil, comprising, by weight percentage, component A and component B, wherein component A per 100 kg: PEG-7 glyceryl cocoate 10%, PEG-20 glyceryl triisostearate 18%, cetyl ethylhexanoate 27%, cocoyl octanoate / decanoate 28%, and isododecane 17%. Component B (100 kg): 1% methyl propylene glycol, 10% glycerin, 0.5% Gentiana macrophylla extract, 10% butylene glycol, 2% 1,2-hexanediol, 3% 1,2-pentanediol, 2% Cordyceps sinensis mycelium powder, and water as balance.
[0059] The preparation method of Gentiana macrophylla extract includes the following steps: Take 5 kg of Gentiana macrophylla and pulverize it to obtain Gentiana macrophylla powder. Disperse the Gentiana macrophylla powder in a 50% ethanol solution and reflux extract (extraction temperature 45℃, material-to-liquid ratio 1:30, extraction time 55 min) to obtain Gentiana macrophylla extract. Concentrate the Gentiana macrophylla extract under reduced pressure at 45℃ and a vacuum degree of -0.09 MPa to obtain Gentiana macrophylla extract paste. Freeze-dry at -80℃ for 24 h to obtain Gentiana macrophylla extract.
[0060] The preparation method of Cordyceps sinensis mycelial powder includes the following steps: 10 kg of Cordyceps sinensis mycelium is dried, pulverized, and passed through a 60-mesh sieve to obtain Cordyceps sinensis powder. The Cordyceps sinensis powder and 50% ethanol extraction solvent are mixed evenly and placed in a microwave extractor. Under the conditions of microwave power 500W, solid-liquid ratio 1:20 g / mL, extraction time 45 min, and extraction temperature 60℃, extraction is performed once to obtain Cordyceps sinensis mycelium microwave extract. The extract is concentrated under reduced pressure, loaded onto D101 type macroporous adsorption resin, statically adsorbed for 24 h, and eluted successively with water, 30% (v / v) and 90% (v / v) ethanol. The 90% (v / v) ethanol eluent is collected, concentrated under reduced pressure, and dried to obtain Cordyceps sinensis mycelium extract.
[0061] The preparation method of the above-mentioned bicontinuous phase cleansing oil includes the following steps: PEG-7 glyceryl cocoate, PEG-20 glyceryl triisostearate, cetyl ethylhexanoate, cocoyl caprylate / caprate, and isododecane were mixed and stirred evenly at a stirring speed of 20 r / min. Then, methyl propylene glycol, glycerin, Gentiana macrophylla extract, butylene glycol, 1,2-hexanediol, 1,2-pentanediol, Cordyceps sinensis mycelium powder, and water were added and stirred evenly at room temperature. The mixture was then filtered through a 200-mesh filter cloth to obtain a bicontinuous phase cleansing oil.
[0062] Example 2 A bicontinuous phase cleansing oil, differing from Example 1 in that, by weight percentage, the bicontinuous phase cleansing oil comprises component A and component B, wherein component A consists of: 1% PEG-7 glyceryl cocoate, 19% PEG-20 glyceryl triisostearate, 30% cetyl ethylhexanoate, 30% cocoyl octanoate / decanoate, and 20% isododecane. Component B: 15% methyl propylene glycol, 1% glycerin, 2% Gentiana macrophylla extract, 1% butylene glycol, 0.5% 1,2-hexanediol, 0.5% 1,2-pentanediol, 0.5% Cordyceps sinensis mycelium powder, water balance.
[0063] The preparation method of the above-mentioned bicontinuous phase cleansing oil includes the following steps: Mix PEG-7 glyceryl cocoate, PEG-20 glyceryl triisostearate, cetyl ethylhexanoate, cocoyl caprylate / caprate, and isododecane, stir well at 10 rpm, then add methyl propylene glycol, glycerin, Gentiana macrophylla extract, butylene glycol, 1,2-hexanediol, 1,2-pentanediol, Cordyceps sinensis mycelium powder, and water, stir well, and filter through a 100-mesh filter cloth to obtain a bicontinuous phase cleansing oil.
[0064] The stirring temperature was 65℃, and the stirring time was 25 minutes.
[0065] Example 3 A bicontinuous phase cleansing oil differs from Example 1 in that the mass ratio of PEG-7 glyceryl cocoate to PEG-20 glyceryl triisostearate is 1:13.
[0066] The mass ratio of Gentiana macrophylla extract, Cordyceps sinensis mycelium powder, and methyl propylene glycol is 1:1:20.
[0067] Example 4 A bicontinuous phase cleansing oil differs from Example 1 in that the mass ratio of PEG-7 glyceryl cocoate to PEG-20 glyceryl triisostearate is 1:8.
[0068] The mass ratio of Gentiana macrophylla extract, Cordyceps sinensis mycelium powder, and methyl propylene glycol is 1:1:10.
[0069] Example 5 A dual-continuous phase cleansing oil differs from Example 1 in that the pretreatment preparation of Gentiana macrophylla extract is carried out using 1-1.
[0070] Example 6 A dual-continuous-phase cleansing oil differs from Example 1 in that the pretreatment preparation of Gentiana macrophylla extract uses steps 1-2.
[0071] Example 7 A dual-continuous-phase cleansing oil differs from Example 1 in that the pretreatment preparation of Gentiana macrophylla extract uses steps 1-3.
[0072] Example 8 A dual-continuous-phase cleansing oil differs from Example 1 in that the pretreatment preparation of Gentiana macrophylla extract uses steps 1-4.
[0073] Example 9 A dual-continuous phase cleansing oil differs from Example 1 in that the pretreatment preparation of Gentiana macrophylla extract uses step 1-5.
[0074] Example 10 A dual-continuous-phase cleansing oil differs from Example 1 in that the pretreatment preparation of Gentiana macrophylla extract uses steps 1-6.
[0075] Example 11 A dual-continuous phase cleansing oil differs from Example 1 in that the pretreatment preparation of Gentiana macrophylla extract uses 1-7.
[0076] Example 12 A dual-continuous phase cleansing oil differs from Example 1 in that the pretreatment preparation of Gentiana macrophylla extract uses method 1-8.
[0077] Example 13 A dual-continuous-phase cleansing oil differs from Example 1 in that the pretreatment preparation of Gentiana macrophylla extract uses 1-9.
[0078] Comparative Example Comparative Example 1 A bicontinuous phase cleansing oil, which differs from Example 1 in that it does not contain PEG-7 glyceryl cocoate.
[0079] Comparative Example 2 A bicontinuous phase cleansing oil, which differs from Example 1 in that it does not contain PEG-20 glyceryl triisostearate.
[0080] Performance testing The performance of the bicontinuous phase cleansing oils prepared in Examples 1-13 and Comparative Examples 1-2 was tested. 1. Volunteers aged 25-30 were selected as subjects and randomly divided into 16 groups of 10 people each.
[0081] Subjects marked three 4cm x 4cm areas on the flexor side of their left and right forearms as test areas, with at least a 1.5cm interval between each area. These three test areas were numbered L1, L2, L3 and R1, R2, R3, respectively. After sitting still for 25 minutes, images of each test area were acquired using a microscope, and the L*, a*, and b* values of the skin in its initial state were measured using a spectrophotometer. Then, images of each test area were acquired using a microscope, and the L*, a*, and b* values of the skin were measured after applying eyeliner / mascara using a spectrophotometer.
[0082] Regions L1, L2, L3, and R1, R2, R3 were cleansed using a 1.5mL syringe with the makeup remover oils prepared in Examples 1-13 and Comparative Examples 1-2. After rinsing thoroughly with water, the areas were patted dry with paper towels. After sitting still for 35 minutes, images of each test area were acquired using a microscope, and the L*, a*, and b* values of the skin after makeup removal and cleansing were measured using a spectrophotometer. L* represents blackness / whiteness; a higher L* value indicates a whiter skin tone, and vice versa. a* represents red / green hue; a higher a* value indicates a redder skin tone, and vice versa. b* represents blue / yellow hue; a higher b* value indicates a yellower skin tone, and vice versa. The testing environment was maintained at a constant temperature and humidity: 25℃ and 60% relative humidity.
[0083] Cleansing power calculation method: Calculate the skin color difference after applying eyeliner / mascara compared to the initial state, denoted as △E(after application); calculate the skin color difference after makeup removal and cleansing compared to the initial state, denoted as △E(after cleansing). △E comprehensively reflects the three-dimensional change in skin color. The larger the △E value, the more obvious the skin color change; the smaller the △E value, the closer the skin color is to the initial state. The cleansing power is calculated using the following formula: △E=SQRT(△L* 2 +△a* 2 +△b* 2 ) Cleaning power = (△E(after application) - △E(after cleaning) / △E(after application)) × 100%, and the test results are shown in Table 1.
[0084] 2. The subjects used the samples from Examples 1-5 and Comparative Examples 1-2, respectively, once every night for 21 consecutive days. Instructions for use: Shake the cleansing oil well, take an appropriate amount onto your hands and face, and massage in circular motions. After use, subjects rated the gentleness around the eyes, skin feel, cleansing sensation, and makeup removal effectiveness using a 5-point scale: 4.5 points and above indicate excellent (very satisfied); 4-4.5 points indicate good; 3-4 points indicate moderately acceptable; below 3 points indicate poor (unacceptable). Each score is the average of 10 participants. Test results are shown in Table 2.
[0085] Table 1 Test data for the examples and comparative examples Table 2 Test data for the examples and comparative examples As shown in Table 1, the bicontinuous-phase cleansing oils prepared in Examples 1-2 of this application exhibit good cleansing power and effectiveness. Specifically, the eyeliner cleansing power of Example 1 is 80.1%, and the mascara cleansing power is 81.7%. It is evident that components A (PEG-20 glyceryl triisostearate and PEG-7 glyceryl cocoate) are uniformly dissolved in the oil. With the addition of component B, the oil and water phases are dispersed into tiny regions. Surfactant molecules are orderly arranged and assembled at the oil-water interface, forming a three-dimensional network structure where oil and water channels intertwine, interweave, and continuously connect. During use, it can instantly emulsify, rinse easily, leave a refreshing feel, and deliver the active ingredients, achieving comprehensive cleansing.
[0086] Examples 3-4 varied the mass ratio of PEG-7 glyceryl cocoate and PEG-20 glyceryl triisostearate, as well as the mass ratio of Gentiana macrophylla extract, Cordyceps sinensis mycelium powder, and methyl propylene glycol. Table 1 shows that the eyeliner in Example 3 had a cleansing power of 83.3%, and the mascara had a cleansing power of 84.9%. This indicates that the combination of PEG-7 glyceryl cocoate and PEG-20 glyceryl triisostearate possesses both the strong dissolving power of oil-soluble substances and the easy cleansing properties of an aqueous system, resulting in a light, smooth, and non-sticky skin feel. After rinsing, the skin feels clean and breathable, without any oily film residue.
[0087] Example 5 involved pretreatment of Gentiana macrophylla extract. Table 1 shows that the eyeliner cleansing power of Example 5 was 95.2%, and the mascara cleansing power was 96.4%. This indicates that the pretreated Gentiana macrophylla extract has excellent makeup removal effect. During makeup removal, moisture on the skin surface slowly penetrates into the microcapsule wall material, causing slight swelling of the cross-linked structure of the wall material. The active ingredients (Gentiana macrophylla extract and aloe polysaccharides) can be slowly released to the skin surface through the pores of the wall material. This avoids local irritation caused by a one-time release and allows the active ingredients to continuously exert a soothing and moisturizing effect throughout the makeup removal process, relieving skin discomfort caused by makeup removal friction.
[0088] In Examples 6-7, modified nanoporous silica and sodium hyaluronate were not added during the pretreatment of Gentiana macrophylla extract, while in Examples 8-9, the mass ratio of Gentiana macrophylla extract, modified nanoporous silica, and sodium hyaluronate was changed. Table 1 shows that the eyeliner and mascara cleansing performance of Examples 6-7 was significantly worse than that of Examples 5 and 8, while the corresponding performance of Example 9 was better than that of Examples 6-7, but worse than that of Example 5. This indicates that Gentiana macrophylla extract is responsible for temporarily opening the skin barrier and inducing local inflammatory responses; modified nanoporous SiO2 is responsible for instantly absorbing makeup and releasing high concentrations of bitter glycosides; and sodium hyaluronate is responsible for locking water in the skin and carrying bitter glycosides deeper. The combination of these three components results in more thorough makeup removal, faster soothing, and longer-lasting moisturizing.
[0089] In Examples 10-11, the preparation methods of modified nanoporous silica did not include alginate solution or polyvinyl alcohol fibers. Table 1 shows that the eyeliner and mascara removal performance of Example 10 was significantly worse than Example 5, but better than Example 6; the corresponding performance of Example 11 was better than Example 10, but worse than Example 5. This indicates that the alginate solution forms a film on the nano-silica surface, improving the mechanical strength and toughness of the coating, resulting in better adhesion between the nano-silica and polyvinyl alcohol fibers, which helps improve the subsequent makeup removal effect; the network formed by the polyvinyl alcohol fibers, through physical encapsulation and synergistic effect with surfactants, helps to break down stubborn makeup more quickly upon contact with it.
[0090] In Examples 12-13, the preparation methods of polyvinyl alcohol fibers did not include inulin or sodium carboxymethyl cellulose. Table 1 shows that the eyeliner and mascara cleansing abilities of Examples 12-13 were significantly worse than those of Example 5, but better than those of Example 11. This indicates that inulin forms a microstructure in the fiber, increasing its hygroscopicity or providing space for subsequent drug loading. Sodium carboxymethyl cellulose modulates the rheological properties of the spinning solution, making it easier to spin. The resulting polyvinyl alcohol fibers have better adsorption and loading capacity, contributing to better makeup removal.
[0091] Comparative Examples 1 and 2 were prepared without PEG-7 glyceryl cocoate and PEG-20 glyceryl triisostearate, respectively. Table 1 shows that the eyeliner and mascara cleansing abilities of Comparative Examples 1 and 2 were significantly worse than those of Example 1. This indicates that PEG-7 glyceryl cocoate can combine oily components with water to form a stable emulsion, promoting ingredient absorption and effectively cleaning dirt and makeup residue from the skin surface. It also has good moisturizing effects, increasing skin hydration. PEG-20 glyceryl triisostearate has good emulsifying properties, quickly dissolving makeup and dirt, making makeup removal easier and more thorough, and also has a moisturizing effect.
[0092] Sensory tests were conducted on the cleansing oils of Examples 1-5 and Comparative Examples 1-2. Table 2 shows that Examples 1-2 exhibited moderate results in terms of gentleness to the eyes, skin feel, cleansing sensation, and makeup removal power, while Examples 3-4 showed better results in these areas, particularly in makeup removal power. Example 5 involved pretreatment of Gentiana macrophylla extract. Table 2 shows that this pretreatment significantly improved the results in terms of gentleness to the eyes, skin feel, cleansing sensation, and makeup removal power. Comparative Examples 1-2 did not contain PEG-7 glyceryl cocoate or PEG-20 glyceryl triisostearate, respectively. Table 2 shows that the results in terms of gentleness to the eyes, skin feel, cleansing sensation, and makeup removal power were significantly worse, indicating that the cleansing oil prepared in this application has excellent makeup removal effects.
[0093] This specific embodiment is merely an explanation of this application and is not intended to limit it. After reading this specification, those skilled in the art can make modifications to this embodiment without contributing any inventive step, but such modifications are protected by patent law as long as they fall within the scope of the claims of this application.
Claims
1. A dual continuous phase cleansing oil, characterized in that, By mass percentage, it includes component A and component B, wherein component A consists of: PEG-7 glyceryl cocoate 1-10%, PEG-20 glyceryl triisostearate 10-20%, cetyl ethylhexanoate 10-30%, cocoyl octanoate / decanoate 10-30%, and isododecane 10-20%; Component B: 1-15% methyl propylene glycol, 1-10% glycerin, 0.5-2% Gentiana macrophylla extract, 1-10% butylene glycol, 0.5-2% 1,2-hexanediol, 0.5-3% 1,2-pentanediol, 0.5-2% Cordyceps sinensis mycelium powder, water balance.
2. The dual continuous phase cleansing oil according to claim 1, characterized in that, The mass ratio of PEG-7 glyceryl cocoate to PEG-20 glyceryl triisostearate is 1:8-13.
3. The dual continuous phase cleansing oil according to claim 1, characterized in that, The mass ratio of Gentiana macrophylla extract, Cordyceps sinensis mycelium powder, and methyl propylene glycol is 1:1:10-20.
4. The dual continuous phase cleansing oil according to claim 1, characterized in that, Pretreatment of Gentiana macrophylla extract includes the following: (1) Disperse Gentiana macrophylla extract, aloe polysaccharide, modified nanoporous silica and sodium hyaluronate in deionized water and stir evenly to obtain core material; (2) Disperse sodium alginate, gum arabic, soybean lecithin, glycerin, and PEG600 in deionized water and stir evenly at 70-75℃ to obtain the wall material; (3) Mix the core material and wall material, homogenize, and spray dry to obtain Gentiana macrophylla extract microcapsules.
5. The dual continuous phase cleansing oil according to claim 4, characterized in that, The mass ratio of Gentiana macrophylla extract, modified nanoporous silica, and sodium hyaluronate is 1:0.62-0.75:0.26-0.
41.
6. The dual continuous phase cleansing oil according to claim 4, characterized in that, The homogenization pressure is 20-30 MPa, and the time is 30-35 min.
7. The dual continuous phase cleansing oil according to claim 4, characterized in that, The method for preparing the modified nanoporous silica includes the following steps: The nanoporous silica was dispersed in hydrochloric acid solution, soaked for 10-15 min, washed with water, calcined at 300-350℃ for 30-35 min, then dispersed in silane coupling agent aqueous solution, hexadecyltrimethylammonium bromide was added, filtered, washed with water, dried, and then impregnated in alginate solution and dried to obtain modified nanoporous silica. Preparation of alginate solution: Disperse alginate in deionized water, add treated polyvinyl alcohol fiber, sodium dodecylbenzene sulfonate, and ascorbic acid, stir for 1-2 hours to obtain alginate solution; Polyvinyl alcohol fibers are cut to a length of 0.1-0.15 mm to obtain treated polyvinyl alcohol fibers.
8. A dual continuous phase cleansing oil according to claim 7, characterized in that, The method for preparing the polyvinyl alcohol fiber includes the following steps: Polyvinyl alcohol is dispersed in deionized water and stirred at 80-85℃ for 30-35 minutes. The resulting polyvinyl alcohol solution is degassed under vacuum, and inulin, sodium carboxymethyl cellulose, and preservative are added. The solution is then sonicated for 1-2 hours to obtain a spinning solution. The spinning solution is then spun, hot-stretched, and cooled to room temperature to obtain polyvinyl alcohol fibers.
9. The method for preparing a dual continuous phase makeup remover oil according to claim 1, characterized in that, Includes the following steps: Mix PEG-7 glyceryl cocoate, PEG-20 glyceryl triisostearate, cetyl ethylhexanoate, cocoyl caprylate / caprate, and isododecane, and stir until homogeneous at a stirring speed of 10-20 r / min. Then add methyl propylene glycol, glycerin, Gentiana macrophylla extract, butylene glycol, 1,2-hexanediol, 1,2-pentanediol, Cordyceps sinensis mycelium powder, and water, and stir until homogeneous. Filter through a 100-200 mesh filter cloth to obtain a bicontinuous phase cleansing oil.