Oil-powder double-dosage-form skin care essence oil as well as preparation method and application thereof
Through the preparation method of oil-powder dual-dose skin care essence oil, porous powder is used to physically adsorb water-soluble and alcohol-soluble active ingredients, which solves the problem of solubility stability of active ingredients in essence oil and achieves efficient and safe skin care effects.
Patent Information
- Application Number
- CN202510931659.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-07-07
- Publication Date
- 2025-09-09
AI Technical Summary
The water-soluble and alcohol-soluble active ingredients in existing essence oils are difficult to dissolve, which limits their application. Traditional methods have stability issues and may cause skin irritation. Existing porous powders are only used in essence oils to highlight the appearance without solving the problem of active ingredient adsorption.
A dual-dose skin care essence oil of oil and powder is used, and the water-soluble and alcohol-soluble active ingredients are physically adsorbed by the porous powder, combined with a dispersing aid to improve stability. The preparation method includes porous powder pretreatment, active ingredient dissolution, vacuum freeze drying and uniform mixing, and the oil and powder are mixed in proportion.
The high stability and high retention rate of water-soluble and alcohol-soluble active ingredients are achieved. The essence oil has a clear and transparent appearance and has antioxidant, whitening, firming and anti-wrinkle effects. It is safe, mild and non-irritating, and has good high and low temperature and light stability.
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Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of cosmetics, and in particular relates to an oil-powder dual-dose skin care essence oil, a preparation method thereof, and uses thereof. Background Art
[0002] The growing demand for essential oils in the skincare market, particularly with the rise of the oil-based skincare concept, has driven the rapid development of the oil-based skincare market. Essential oils typically use plant oils or synthetic esters as a base phase, infused with various active ingredients. They offer multiple skincare benefits, including hydration, barrier repair, skin brightening, anti-aging, and antioxidant properties, catering to consumers with diverse skin types, including dry, oily, and combination skin.
[0003] The stability and solubility of active ingredients in essential oils have always been technical difficulties. Since essential oils are mainly oil-phase systems, except for a small amount of oil-soluble active ingredients (such as coenzyme Q10, myristyl nicotinate, etc.) that can be directly dissolved, many water-soluble active ingredients (such as vitamin C, peptides, etc.) and alcohol-soluble active ingredients (ferulic acid, resveratrol, etc.) are difficult to dissolve directly in the oil phase, which seriously limits the application of these effective ingredients in essential oils. Currently, the industry primarily employs the following technical solutions to address this issue: First, emulsifiers or solubilizers (such as polyglyceryl-3 laurate, polyglyceryl-3 polyricinoleate, and PEG-8 isostearate) are used to improve the dispersibility of active ingredients. However, this method relies on surfactants to maintain system stability, and long-term use can cause skin irritation and barrier damage. Second, liposome encapsulation or microencapsulation techniques are employed. However, these carriers are prone to rupture in the oil phase, leading to premature release of the active ingredients. Furthermore, the active ingredients are easily degraded and inactivated under high temperatures or light, affecting the product's effectiveness. Furthermore, the preparation process is complex and costly. Third, innovative dosage forms, such as water-oil-separated essence oils, allow the addition of relevant water-soluble active ingredients to the aqueous phase. However, the temporary mixing of water-oil-separated shaken essence oils can easily lead to uneven dispersion and low active ingredient utilization. Therefore, there is an urgent need to develop a technology to address the technical challenges of incorporating both water-soluble and alcohol-soluble active ingredients into essence oils.
[0004] Porous powder refers to a micron or nanometer-scale functional powder material with a high specific surface area and a rich pore structure. Its unique physical structure gives it multiple functions such as adsorption and oil control, soft focus modification, and active delivery in skin care products, and it is widely used in skin care products. Porous powder provides a new idea for the application of non-oil-soluble active ingredients in essential oils and shows good application prospects. However, in the prior art, there is no method of using porous powder to adsorb water-soluble and alcohol-soluble active substances and apply them to essential oils. Only in the Chinese patent CN114224757A (application number CN202111602982.8) is the powder mixed with the essential oil, but it can only make the product have a high-gloss appearance, and the appearance is not clear and transparent, and the adsorption of active ingredients by porous powder is not developed, and the technical problem of applying non-oil-soluble active ingredients to essential oils is not solved. Summary of the Invention
[0005] In response to the above-mentioned problems existing in the prior art, the purpose of the present invention is to design and provide a technical solution for a dual-formulation oil-powder skin care essence oil, its preparation method and use. The powder contains water-soluble and alcohol-soluble active ingredients, breaking through the limitations of traditional pure oil formulas in using active ingredients; the active ingredients in the powder part are physically adsorbed in the powder pores, with higher stability and retention rate; the obtained essence oil has antioxidant, whitening, firming and anti-wrinkle, and repair effects.
[0006] The oil-powder dual-formulation skin care essence oil is characterized by being composed of an oil agent: a powder agent at a mass ratio of 40 to 100:1; The powder comprises: 30-60 parts of porous powder, 30-60 parts of dispersing aid, and 0.01-10 parts of active ingredient; The porous powder is one of silicon dioxide, polymethyl methacrylate, corn starch, modified corn starch, and cassava starch, and the porous powder has a specific surface area of ≥300 m² / g and a pore diameter of 2 to 50 nm; The dispersing aid is an amphiphilic solvent selected from one of ethoxydiglycol, diethoxyethyl succinate, diisopropyl sebacate, propylene glycol dicaprylate / dicaprate, butylene glycol dicaprylate / dicaprate, and bis-diethoxydiglycol cyclohexane 1,4-dicarboxylate; The active ingredient is a water-soluble active ingredient or an alcohol-soluble active ingredient; The water-soluble active ingredient is at least one of vitamin C, sodium hyaluronate, asiaticoside, madecassoside, tea polyphenols, ergothioneine, rhamnose, tripeptide-1 copper, acetyl tetrapeptide-11, acetyl tetrapeptide-9, acetyl tetrapeptide-2, palmitoyl tripeptide-1, palmitoyl tripeptide-5, and acetyl hexapeptide-8; and the alcohol-soluble active ingredient is at least one of ferulic acid, resveratrol, phloretin, tetrahydrocurcumin, tetrahydromagnanol, and glabridin.
[0007] The oil agent comprises: 1 to 90 parts of vegetable oil, 1 to 90 parts of synthetic oil, 0.01 to 8 parts of material protective agent, and 0.01 to 1 part of flavoring and coloring agent.
[0008] The oil-powder dual-formulation skin care essence oil is characterized in that the mass ratio of oil:powder is 60-90:1, and the preferred mass ratio of oil:powder is 70-80:1.
[0009] The oil-powder dual-dose skin care essence oil is characterized by: a powder part comprising 40-50 parts of porous powder, 40-50 parts of a dispersing aid, and 1-6 parts of an active ingredient; and an oil part comprising 20-85 parts of vegetable oil, 20-85 parts of a synthetic oil, 0.1-5 parts of a material protective agent, and 0.1-0.5 parts of a flavoring and coloring agent; preferably, 40-60 parts of vegetable oil, 40-60 parts of a synthetic oil, 0.1-2 parts of a material protective agent, and 0.1-0.2 parts of a flavoring and coloring agent.
[0010] The oil-powder dual-dose skin care essence oil is characterized in that the plant oil is at least one of meadowfoam seed oil, jojoba seed oil, sesame seed oil, filbert seed oil, camellia seed oil, perilla seed oil, corn germ oil, sweet almond oil, dog rose fruit oil, camelina seed oil, macadamia seed oil, sea buckthorn fruit oil, ganoderma lucidum spore oil, borage seed oil, avocado oil, camellia seed oil, and wheat germ oil.
[0011] The oil-powder dual-dose skin care essence oil is characterized in that the synthetic oil is at least one of caprylic / capric triglyceride, squalane, coconut oil caprylate / caprate, C9-12 alkane, dicaprylyl carbonate, isopropyl myristate, and ethylhexyl palmitate.
[0012] The oil-powder dual-dose skin care essence oil is characterized in that the material protective agent is at least one of ascorbyl tetraisopalmitate, dimethylmethoxychromanol, vitamin E, tocopheryl acetate, and rosemary extract; and the fragrance and colorant is at least one of lavender oil, cedar wood oil, bergamot fruit oil, and β-carotene.
[0013] The method for preparing the oil-powder dual-dose skin care essence oil is characterized by comprising the following steps: 1) Weigh 30-60 parts of porous powder, 30-60 parts of dispersing aid, and 0.01-10 parts of active ingredient and set aside; soak the porous powder in deionized water at room temperature for 12-24 hours and vacuum dry; 2) dissolving the active ingredient in water or a polyol solvent at a mass ratio of 1:4 to 500, then uniformly mixing the porous structure powder pretreated in step 1) with the active ingredient solution, and freeze-drying in a vacuum; 3) Slowly adding the mixture obtained in step 2) to the dispersing aid, stirring until homogenized, and standing at room temperature to obtain a powder; 4) Weigh 0-99 parts of vegetable oil, 0-99 parts of synthetic oil, 0.01-8 parts of material protective agent, and 0.01-1 part of flavoring and coloring agent, and stir evenly to obtain an oil solution; 5) Before use, the oil and powder prepared in the above steps are uniformly mixed at a mass ratio of 40 to 100:1 to obtain the essential oil.
[0014] The method for preparing the oil-powder dual-formulation skin care essence oil is characterized in that in step 1), the vacuum drying temperature is 100-130° C. and the drying time is 4-12 hours; preferably, the temperature is 110-120° C. and the drying time is 8-10 hours.
[0015] The method for preparing an oil-powder dual-formulation skin care essence oil is characterized in that in step 2), the mass ratio of active ingredient to water or polyol solvent is 1:100-200, the porous structure powder and the active ingredient are stirred at 200-500 rpm for 20-60 minutes, and then vacuum freeze-dried under the conditions of vacuum degree ≤5 Pa and -40°C; the stirring speed is preferably 300-400 rpm, and the stirring time is 30-40 minutes; In step 3), the mixture is added to the dispersing aid and stirred at 200-500 rpm for 5-10 minutes, homogenized at 5000-10000 rpm for 10-20 minutes, and then allowed to stand at room temperature for 4-6 hours. During the standing process, the container is gently shaken every 30 minutes to obtain a powder.
[0016] The oil-powder dual-formulation skin care essence oil is used in the preparation of antioxidant, whitening, firming, anti-wrinkle and repair cosmetics.
[0017] The porous powder used in this invention possesses a high specific surface area and a rich nanoscale pore structure (specific surface area ≥300 m² / g, pore diameter 2-50 nm). This high specific surface area means that each tiny powder particle has numerous adsorption sites, enabling more effective adsorption of large quantities of non-oil-soluble active ingredients. The nanoscale pore size ensures that these active ingredients can smoothly enter and be adsorbed within the porous powder's pores, achieving uniform adsorption and avoiding localized accumulation of active ingredients or ineffective fixation to the powder, thereby improving the stability and delivery efficiency of the active ingredients. The amphiphilic nature of the dispersing aid effectively links the active ingredients within the porous powder with the oil, providing excellent dispersion stability of the porous powder in the essential oil, preventing powder agglomeration in the oil and enhancing the stability of the porous powder in the essential oil. This facilitates rapid and uniform mixing of the powder and oil compartments before use, enabling the realization of an oil-powder dual-dose formulation, thus overcoming the limitations of traditional pure oil formulations for the use of non-oil-soluble active ingredients.
[0018] The aforementioned dual-formulation oil-to-powder skincare essence oil contains both water-soluble and alcohol-soluble active ingredients in its powder form, resolving the issue of using water-soluble or alcohol-soluble active ingredients in all-oil cosmetic formulas and overcoming the limitations of traditional pure oil formulations in using active ingredients. The active ingredients in the powder form are physically adsorbed within the powder pores, effectively preventing damage to the active ingredients from air oxidation. This active ingredient exhibits greater stability and retention, resulting in improved skincare efficacy and efficient utilization. This essence oil is clear and transparent, exhibits excellent high-temperature and light stability, feels good on the skin, is safe, gentle, and non-irritating, and exhibits antioxidant, whitening, firming, anti-wrinkle, and repairing properties. DETAILED DESCRIPTION
[0019] The following describes the technical solutions of the present invention through corresponding embodiments. Obviously, the embodiments described are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.
[0020] Example 1 1) Silica was soaked in deionized water at room temperature for 12 hours, then vacuum-dried at 120°C for 6 hours. 0.01 g of ferulic acid was dissolved in 40 g of ethanol. 50 g of the pretreated porous powder was mixed with the active ingredient solution, stirred at 200 rpm for 40 minutes, and then freeze-dried at -40°C for 24 hours under vacuum conditions of ≤5 Pa. 2) Slowly add the resulting mixture to 49 g of ethoxydiglycol, stir at 200 rpm for 10 min, homogenize at 5000 rpm for 20 min, then let stand at room temperature for 4 h, gently shaking the container every 30 min to obtain a powder: 3) Weigh 19.8 g of meadowfoam seed oil, 60 g of caprylic / capric triglyceride, 20 g of C9-12 alkane, 0.1 g of tocopherol, and 0.1 g of β-carotene, and mix well to obtain an oil; 4) The oil and powder prepared in the above steps are mixed uniformly at a mass ratio of 100:1 before use to obtain an oil-powder dual-formulation skin care essence oil.
[0021] Example 2 1) Silica was soaked in deionized water at room temperature for 16 hours, then vacuum-dried at 110°C for 8 hours. 5 g of ferulic acid was dissolved in 40 g of water. 44 g of the pretreated porous powder was weighed and mixed with the active ingredient solution. After stirring at 300 rpm for 30 minutes, the mixture was freeze-dried at -40°C under vacuum conditions of ≤5 Pa for 36 hours. 2) Slowly add the resulting mixture to 55 g of ethoxydiglycol, stir at 500 rpm for 5 minutes, homogenize at 6000 rpm for 15 minutes, and then let stand at room temperature for 5 hours, gently shaking the container every 30 minutes to obtain a powder; 3) Weigh 49.9 g of meadowfoam seed oil, 30 g of caprylic / capric triglyceride, 20 g of C9-12 alkane, 0.1 g of ascorbyl tetraisopalmitate, and 0.2 g of β-carotene, and stir well to obtain an oil; 4) The oil and powder prepared in the above steps are mixed uniformly at a mass ratio of 90:1 before use to obtain an oil-powder dual-formulation skin care essence oil.
[0022] Example 3 1) Soak silica in deionized water at room temperature for 18 hours, then vacuum dry at 130°C for 4 hours. Dissolve 10 g of ferulic acid in 40 g of ethanol. Weigh 40 g of the pretreated porous powder and mix it with the active ingredient solution. Stir at 200 rpm for 60 minutes, then freeze-dry at -40°C for 48 hours in a vacuum of ≤5 Pa. 2) Slowly add the resulting mixture to 50 g of ethoxydiglycol, stir at 300 rpm for 8 minutes, homogenize at 8000 rpm for 15 minutes, and then let stand at room temperature for 5 hours, gently shaking the container every 30 minutes to obtain a powder; 3) Weigh 79.4 g of meadowfoam seed oil, 10 g of caprylic / capric triglyceride, 10 g of C9-12 alkane, 0.5 g of ascorbyl tetraisopalmitate, and 0.1 g of bergamot fruit oil and mix well to obtain an oil; 4) The oil and powder prepared in the above steps are mixed uniformly at a mass ratio of 80:1 before use to obtain an oil-powder dual-formulation skin care essence oil.
[0023] Example 4 1) Soak silica in deionized water at room temperature for 24 hours, then vacuum dry at 100°C for 10 hours. Dissolve 0.1 g of palmitoyl tripeptide-1 in 40 g of deionized water. Weigh 50 g of the pretreated porous structure powder and mix it with the active ingredient solution. Stir at 500 rpm for 20 minutes, and then freeze-dry at -40°C for 24 hours in a vacuum of ≤5 Pa. 2) Slowly add the resulting mixture to 49.9 g of ethoxydiglycol, stir at 400 rpm for 5 min, homogenize at 10,000 rpm for 10 min, and then let stand at room temperature for 6 h. Gently shake the container every 30 min to obtain a powder; 3) Weigh 50 g of meadowfoam seed oil, 30 g of caprylic / capric triglyceride, 19.6 g of C9-12 alkane, 0.2 g of tocopheryl acetate, and 0.2 g of β-carotene, and stir well to obtain an oil; 4) The oil and powder prepared in the above steps are mixed uniformly at a mass ratio of 70:1 before use to obtain an oil-powder dual-formulation skin care essence oil.
[0024] Example 5 1) Silica was soaked in deionized water at room temperature for 24 hours, then vacuum-dried at 130°C for 8 hours. 10 g of ferulic acid was dissolved in 40 g of ethanol. 60 g of the pretreated porous powder was mixed with the active ingredient solution, stirred at 200 rpm for 50 minutes, and then freeze-dried at -40°C for 36 hours in a vacuum of ≤5 Pa. 2) Slowly add the resulting mixture to 30 g of ethoxydiglycol, stir at 200 rpm for 10 min, homogenize at 5000 rpm for 20 min, and then let stand at room temperature for 6 h. Gently shake the container every 30 min to obtain a powder. 3) Weigh 28.9 g of meadowfoam seed oil, 30 g of caprylic / capric triglyceride, 40 g of C9-12 alkane, 1 g of tocopheryl acetate, and 0.1 g of β-carotene, and stir well to obtain an oil; 4) The oil and powder prepared in the above steps are mixed uniformly at a mass ratio of 60:1 before use to obtain an oil-powder dual-formulation skin care essence oil.
[0025] Example 6 1) Silica was soaked in deionized water at room temperature for 12 hours, then vacuum-dried at 110°C for 8 hours. 10 g of ferulic acid was dissolved in 40 g of ethanol. 40 g of the pretreated porous powder was weighed and mixed with the active ingredient solution. After stirring at 400 rpm for 40 minutes, the mixture was freeze-dried at -40°C under vacuum conditions of ≤5 Pa for 48 hours. 2) Slowly add the resulting mixture to 50 g of ethoxydiglycol, stir at 300 rpm for 8 minutes, homogenize at 8000 rpm for 20 minutes, and then let stand at room temperature for 8 hours, gently shaking the container every 30 minutes to obtain a powder; 3) Weigh 49.35 g of meadowfoam seed oil, 30 g of caprylic / capric triglyceride, 20 g of C9-12 alkane, 0.5 g of tocopheryl acetate, and 0.15 g of lavender oil and mix well to obtain an oil; 4) The oil and powder prepared in the above steps are mixed uniformly at a mass ratio of 40:1 before use to obtain an oil-powder dual-formulation skin care essence oil.
[0026] Comparative Example 1 1) Weigh 39.75 g of meadowfoam seed oil, 40 g of caprylic / capric triglyceride, 20 g of C9-12 alkane, 0.1 g of tocopheryl acetate, and 0.15 g of lavender oil and mix well to obtain an oil; 2) Add 0.1g of ferulic acid directly to 100g of oil without using porous powder for adsorption and mix well.
[0027] Comparative Example 2 1) Silica was soaked in deionized water at room temperature for 12 hours, then dried at 120°C for 8 hours. 1 g of ferulic acid was dissolved in 10 g of ethanol. 50 g of the pretreated porous powder was weighed and mixed with the active ingredient solution. The mixture was stirred for 40 minutes and then freeze-dried at -40°C under vacuum at ≤5 Pa for 48 hours to obtain a powder. 2) Weigh 39.8 g of meadowfoam seed oil, 40 g of caprylic / capric triglyceride, 20 g of C9-12 alkane, 0.1 g of tocopherol, and 0.1 g of β-carotene, and stir well to obtain an oil; 3) The oil and powder prepared in the above steps are mixed uniformly at a mass ratio of 100:1 before use to obtain an oil-powder dual-formulation skin care essence oil.
[0028] Comparative Example 3 1) Silica (conventional silica powder, non-porous) was soaked in deionized water at room temperature for 12 hours, then vacuum-dried at 120°C for 6 hours. 0.01 g of ferulic acid was dissolved in 40 g of ethanol. 50 g of the pretreated porous powder was mixed with the active ingredient solution, stirred at 200 rpm for 40 minutes, and then freeze-dried at -40°C for 24 hours in a vacuum of ≤5 Pa. 2) Slowly add the resulting mixture to 49 g of ethoxydiglycol, stir at 200 rpm for 10 min, homogenize at 5000 rpm for 20 min, then let stand at room temperature for 4 h, gently shaking the container every 30 min to obtain a powder: 3) Weigh 39.8 g of meadowfoam seed oil, 40 g of caprylic / capric triglyceride, 20 g of C9-12 alkane, 0.1 g of tocopherol, and 0.1 g of bergamot fruit oil and mix well to obtain an oil; 4) The oil and powder prepared in the above steps are mixed uniformly at a mass ratio of 100:1 before use to obtain an oil-powder dual-formulation skin care essence oil.
[0029] Comparative Example 4 1) Silica was soaked in deionized water at room temperature for 12 hours, then vacuum-dried at 120°C for 6 hours. 0.01 g of ferulic acid was dissolved in 40 g of ethanol. 50 g of the pretreated porous powder was mixed with the active ingredient solution, stirred at 200 rpm for 40 minutes, and then freeze-dried at -40°C for 24 hours under vacuum conditions of ≤5 Pa. 2) Slowly add the resulting mixture to 49 g of caprylic / capric triglyceride, stir at 200 rpm for 10 min, homogenize at 5000 rpm for 20 min, then let stand at room temperature for 4 h, gently shaking the container every 30 min to obtain a powder: 3) Weigh 39.8 g of meadowfoam seed oil, 40 g of caprylic / capric triglyceride, 20 g of C9-12 alkane, 0.1 g of tocopherol, and 0.1 g of β-carotene, and stir well to obtain an oil; 4) The oil and powder prepared in the above steps are mixed uniformly at a mass ratio of 100:1 before use to obtain an oil-powder dual-formulation skin care essence oil.
[0030] The beneficial effects of the present invention are further demonstrated below through corresponding test results and experimental data.
[0031] Experiment 1: Encapsulation efficiency and stability test The above examples and comparative examples were placed under different environmental conditions for different periods of time: one month at -10°C, and three months at 5°C, 25°C, 40°C, and 48°C under light conditions. Stability tests were performed and the sample stability was observed after 4 and 12 weeks. Table 1 shows the initial appearance and stability test results for the comparative examples and examples. The encapsulation efficiency of the porous powder for the active ingredient was tested. An appropriate amount of porous powder adsorbing the active ingredient was added to a solvent (ethanol and water for alcohol-soluble and water-soluble active ingredients, respectively) and mixed uniformly. The active ingredient in the porous powder was extracted by ultrasonication for 20 minutes. The powder was then placed in an ultrafiltration centrifuge tube and centrifuged at 10,000 rpm for 30 minutes until no liquid remained in the ultrafiltration centrifuge tube. The porous powder in the inner centrifuge tube was collected and an appropriate amount of solvent was added. The active ingredient content was determined by HPLC. Each sample was tested three times and the average value was taken. The encapsulation efficiency was calculated using the following formula: Encapsulation efficiency (%) = (encapsulated active ingredient content / total active ingredient content) × 100%. HPLC was also used to determine the content (Ct) of the powder samples of each example at 48°C for three months. Each sample was tested three times and the average value was taken. The initial active ingredient content was referred to as the encapsulated active ingredient content (C0). The active ingredient retention rate was calculated as: Retention rate (%) = (Ct / C0) × 100%. The test results are shown in Table 2.
[0032] Table 1 Stability test results
[0033] Note: √ indicates clear and transparent appearance; / indicates no observation As shown in Table 1, Examples 1-6 all initially had a clear and transparent appearance. Stability tests under various environmental conditions also revealed a clear and transparent appearance, without any abnormalities such as precipitation. This demonstrates that the use of porous powders to adsorb non-oil-soluble active ingredients to prepare a dual-composition skincare essence oil not only solves the application issues of the active ingredient but also provides the essence oil with a clear and transparent appearance and excellent high-temperature and light stability. In Comparative Example 1, the active ingredient failed to dissolve in the essence oil without porous powder adsorption. In Comparative Example 3, conventional silica powder without a porous structure was used, and the powder failed to evenly disperse in the essence oil, resulting in a clear and transparent appearance. This demonstrates that the porous structure of the porous powder allows for high oil absorption, enabling even dispersion in the essence oil and a clear and transparent appearance. Comparative Examples 2 and 4 initially present a clear and transparent appearance, but the porous powder is not pretreated with a dispersing aid, or caprylic capric triglyceride is used as a dispersing aid to treat the porous powder. The powder has agglomeration in the long-term stability in the essence oil. Therefore, ethoxydiglycol and the like are selected as dispersing aids. Due to their amphiphilic properties, they can better link the active ingredients and oils in the porous powders, have good dispersion stability for the porous powders in the essence oil, avoid powder agglomeration in the oil, enhance the stability of the porous powders in the essence oil, and facilitate rapid and uniform mixing of the powder and oil before use, thereby enhancing the convenience of using the oil-powder dual-dose skin care essence oil.
[0034] Table 2 Initial encapsulation efficiency and active ingredient retention rate after three months of stability test
[0035] As shown in Table 2, Examples 1-6 and Comparative Examples 2 and 4 used porous powders to adsorb active ingredients, and the active ingredient encapsulation efficiency was not less than 96%. This indicates that the active ingredients in the powder portion were physically adsorbed within the powder pores, with a good encapsulation efficiency, which effectively prevented the active ingredients from being damaged by air oxidation and ensured the stability of the active ingredients. Under the environmental conditions of 48°C for three months, the active ingredient retention rate was not less than 94%, indicating that the use of porous powders to adsorb non-oil-soluble active ingredients can ensure the stability of the active ingredients. Under the dual effects of powder pore fixation and dispersing aids, the active ingredients still have a high retention rate under long-term environmental conditions. However, Comparative Example 3 used conventional silica powder, and the measured active ingredient encapsulation efficiency was only 10.82%, and the long-term stable retention rate was only 4.71%. This indicates that conventional powders without a porous structure cannot efficiently adsorb active ingredients, or they simply accumulate on the powder surface and cannot be evenly dispersed in the essence oil. Therefore, porous powders are used to adsorb active ingredients. The high specific surface area and rich nano-scale pore structure of porous powders can effectively adsorb non-oil-soluble active ingredients, avoiding the problem of local accumulation of active ingredients or inability to be effectively adsorbed on the powder, and solving the problem of applying non-oil-soluble active ingredients in pure oil systems.
[0036] Test 2: Irritation test Thirty-two volunteers aged 18-60 were selected and subjected to an irritation test based on the human skin patch test in the "Safety Technical Specifications for Cosmetics 2015 Edition." The samples from Examples 1-6 were placed in a patch tester. The patch tester containing the sample was then applied to the subject's back using non-irritating tape. The patch was gently pressed with the palm of the hand to evenly adhere to the skin. After 24 hours, the patch tester was removed. The test substance residue on the test area was gently wiped with a moistened cotton ball. After 0.5 hours, the skin reaction was observed after the indentation disappeared. The skin reaction was observed again 24 hours and 48 hours after the patch was removed. The reaction results were recorded according to the grading standard. If fewer than five people experienced a Grade 1 adverse skin reaction and there were no Grade 2-4 adverse skin reactions, the product was considered to have no adverse reaction to humans. The test results are shown in Table 3.
[0037] Table 3 Results of irritation test
[0038] As can be seen from Table 3, the patch test results showed that only a few grade 1 adverse reactions occurred in Examples 2 and 4, but the number of people who used the patch test was less than 5 and there was no grade 2 to 4 skin adverse reaction. It can be determined that the essential oils of Examples 1-6 all showed no adverse reactions to the human body, indicating that the oil-powder dual-dose skin care essential oil provided by the present invention has high safety and is mild and non-irritating.
[0039] Experiment 3: Human efficacy test Antioxidant efficacy test: 20 subjects who met the ITA screening criteria were selected. According to T / ZHCA 025-2023 "Cosmetic Antioxidant Human Test Method", Example 2 was selected as the experimental group. The negative control was a light-exposed group without product application. Three areas that met the inclusion criteria were selected from the volunteers' test sites for instrument measurement, evaluation, and photography. The area of the area should be no less than 30cm 2, Pre-MED irradiation was performed in one of the areas, and the experimental group sample was smeared on one random area, and the other area was used as a negative control. The sample area of the experimental group was smeared with the sample of Example 2 once a day for 4 consecutive days. On the first day of sample smearing, the MED of each subject's test site was determined, and the PreMED area was selected as the irradiation area on the subject's back skin. Six points were irradiated with different doses of ultraviolet rays, and the results were observed after 22-23.5 hours. The lowest irradiation dose or the shortest irradiation time at which erythema appeared on the skin was taken as the MED of the subject. On the 4th day of sample smearing, the sample was smeared first, and then irradiated 30 minutes later. A total of 3 wells were irradiated in each area, and the irradiation intensity of each well was 1*MED, 2*MED, and 3*MED, respectively. 22-23.5 hours after the irradiation, the same evaluation and test as before the sample was used were performed again, including the use of erythema visual score, erythema visual score 0.0 to 7.0 rating standard, 0.5 point system, the smaller the erythema visual score, the less severe the skin erythema and the stronger the antioxidant capacity; skin colorimeter to measure the skin a * Value, skin a * Smaller values indicate less redness and stronger antioxidant capacity. The skin hemoglobin analyzer measures EI values; lower values indicate lower hemoglobin levels in the skin, lowering the redness of the skin from oxidative damage caused by ultraviolet radiation, and stronger antioxidant capacity. Data were analyzed using SPSS software, with a significance level of P < 0.05. Specific experimental results are shown in Table 4.
[0040] Table 4 Antioxidant efficacy test results
[0041] As shown in Table 4, when the irradiation intensity is 1*MED, 2*MED, and 3*MED, the a * The values, EI values, and erythema visual scores were all lower than those of the negative control group, indicating that compared with the negative control group, the severity of skin erythema in the experimental group was lower, the skin was relatively less red, and the skin hemoglobin content was lower. * The smaller the difference, the smaller the increase in skin redness, the smaller the EI difference, the less the increase in hemoglobin content, the smaller the difference in erythema visual score, and the less severe the skin erythema generated after irradiation. According to the difference data, compared with the negative control, the test evaluation results of irradiation 22-23.5h and before application are as follows: for 1*MED, the a* value, EI value, and erythema visual score difference of the experimental group's use area are significantly improved; for 2*MED, the a* value, EI value, and erythema visual score difference of the experimental group's use area are significantly improved; for 3*MED, the a* value, EI value, and erythema visual score difference of the experimental group's use area are significantly improved. Therefore, it can be seen that the sample in the experimental group has an antioxidant effect, and the oil-powder dual-dose skin care essence oil prepared by using porous powder to adsorb ferulic acid provided by the present invention has an antioxidant effect.
[0042] Test 4: Whitening efficacy test 40 healthy female volunteers were selected and randomly divided into an experimental group and a control group. Example 2 was selected as the experimental group. The experimental group used the essence oil of Example 2 after cleansing their face in the morning and evening for 28 consecutive days. The control group used the essence oil composed of the same proportion as Example 2 without adding the porous powder of ferulic acid (the usage remained consistent, about 2g / time), and no other skin care products were used during the period. The experiment required the volunteers to mainly engage in indoor activities during the test period and avoid long-term unprotected exposure to the sun. The face of the volunteer was selected as the test site, and the test was carried out before use, after use for 14 days, and after use for 28 days after the volunteer cleansed his face. The melanin skin detector mexamter was used to test the skin melanin MI value of the volunteer. The lower the measured value, the less melanin content in the skin. The data were analyzed using SPSS software, with a significance level of P < 0.05. The test results are shown in Table 5.
[0043] Table 5 Whitening efficacy test
[0044] As shown in Table 5, after 14 days of continuous use of the essence oil, the melanin content in the skin of the volunteers in the experimental group decreased by 16.69%. After 28 days, the melanin content in the skin decreased by 21.88%, showing a significant whitening effect compared with the control group. This shows that the samples in the experimental group have a whitening effect. The oil-powder dual-formulation skin care essence oil prepared by using a porous powder to absorb brown ferulic acid has a whitening effect.
[0045] Experiment 5: Firming, anti-wrinkle and repair efficacy test 40 healthy female volunteers with wrinkles at the corners of the eyes were selected and randomly divided into an experimental group and a control group. Example 4 was selected as the experimental group. The essential oil of Example 4 was used after cleansing the face in the morning and evening for 28 consecutive days. The control group used an essential oil composed of the same proportion as Example 4 without adding the porous powder of palmitoyl tripeptide-1 (the usage amount remained the same, about 2g / time), and no other skin care products were used during the period. The faces and corners of the eyes of the volunteers were selected as test sites. The tests were conducted before use, after use for 14 days, and after use for 28 days after cleansing the face of the volunteers: the number of wrinkles and the average depth of total wrinkles were measured using the PROMIS LITE wrinkle measuring instrument, the skin elasticity R2 value and the skin firmness F4 value were measured using the Cutometer; the transepidermal water loss (TEWL) was measured using the Tewameter. The data were analyzed using SPSS software, with a significance level of P < 0.05. The test results are shown in Table 6.
[0046] Table 6 Test results of firming, anti-wrinkle and repairing effects
[0047] As shown in Table 6, after 28 days of continuous use of the essence oil, the number of wrinkles in the experimental group decreased by 21.80%, the average depth of total wrinkles also decreased by 20.45%, the skin elasticity R2 improved by 18.52%, the skin firmness improved by 22.36%, and the transepidermal water loss improved by 16.73%. Compared with the control group, it has significant firming, anti-wrinkle and repair effects. Therefore, it can be seen that the sample in the experimental group, using porous powder to adsorb palmitoyl tripeptide-1, to prepare a dual-dose oil-powder skin care essence oil, has firming, anti-wrinkle and repair effects.
[0048] Obviously, the above embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not limitations on the implementation methods of the present invention. For ordinary technicians in the relevant field, other different forms of changes or modifications can be made based on the above description. It is impossible to list all the implementation methods here. All obvious changes or modifications derived from the technical solution of the present invention are still within the scope of protection of the present invention.
Claims
1. An oil-powder dual-dose skin care essence oil, characterized in that It is composed of oil and powder in a mass ratio of 40 to 100:1; The powder comprises: 30-60 parts of porous powder, 30-60 parts of dispersing aid, and 0.01-10 parts of active ingredient; The porous powder is one of silicon dioxide, polymethyl methacrylate, corn starch, modified corn starch, and cassava starch, and the porous powder has a specific surface area of ≥300 m² / g and a pore diameter of 2 to 50 nm; The dispersing aid is an amphiphilic solvent selected from one of ethoxydiglycol, diethoxyethyl succinate, diisopropyl sebacate, propylene glycol dicaprylate / dicaprate, butylene glycol dicaprylate / dicaprate, and bis-diethoxydiglycol cyclohexane 1,4-dicarboxylate; The active ingredient is a water-soluble active ingredient or an alcohol-soluble active ingredient; The water-soluble active ingredient is at least one of vitamin C, sodium hyaluronate, asiaticoside, madecassoside, tea polyphenols, ergothioneine, rhamnose, tripeptide-1 copper, acetyl tetrapeptide-11, acetyl tetrapeptide-9, acetyl tetrapeptide-2, palmitoyl tripeptide-1, palmitoyl tripeptide-5, and acetyl hexapeptide-8; and the alcohol-soluble active ingredient is at least one of ferulic acid, resveratrol, phloretin, tetrahydrocurcumin, tetrahydromagnanol, and glabridin.
2. The oil comprises: 1-90 parts of vegetable oil, 1-90 parts of synthetic oil, 0.01-8 parts of material protective agent, 0.01-1 part of flavoring and coloring agent, The oil-powder dual-formulation skin care essence oil according to claim 1, characterized in that the mass ratio of oil:powder is 60-90:1, preferably the mass ratio of oil:powder is 70-80:
1.
3. The oil-powder dual-dose skin care essence oil according to claim 1, characterized in that: Powder part: 40-50 parts of porous powder, 40-50 parts of dispersing aid, 1-6 parts of active ingredient; Oil part: 20-85 parts of vegetable oil, 20-85 parts of synthetic oil, 0.1-5 parts of material protective agent, 0.1-0.5 parts of flavoring and coloring agent; preferably 40-60 parts of vegetable oil, 40-60 parts of synthetic oil, 0.1-2 parts of material protective agent, 0.1-0.2 parts of flavoring and coloring agent.
4. The oil-powder dual-dose skin care essence oil according to claim 1, characterized in that The vegetable oil is at least one of meadowfoam seed oil, jojoba seed oil, sesame seed oil, filbert seed oil, camellia seed oil, perilla seed oil, corn germ oil, sweet almond oil, dog rose fruit oil, camelina seed oil, macadamia seed oil, sea buckthorn fruit oil, ganoderma lucidum spore oil, borage seed oil, avocado oil, camellia seed oil, and wheat germ oil.
5. The oil-powder dual-dose skin care essence oil according to claim 1, characterized in that The synthetic oil is at least one of caprylic / capric triglyceride, squalane, coconut oil alcohol-caprylate / caprate, C9-12 alkane, dioctyl carbonate, isopropyl myristate, and ethylhexyl palmitate.
6. The oil-powder dual-dose skin care essence oil according to claim 1, characterized in that The material protective agent is at least one of ascorbyl tetraisopalmitate, dimethylmethoxychromanol, vitamin E, tocopheryl acetate, and rosemary extract; and the flavoring and coloring agent is at least one of lavender oil, cedarwood oil, bergamot fruit oil, and beta-carotene.
7. The method for preparing an oil-powder dual-dose skin care essential oil according to claim 1, characterized in that The following steps are involved: 1) Weigh 30-60 parts of porous powder, 30-60 parts of dispersing aid, and 0.01-10 parts of active ingredient and set aside; soak the porous powder in deionized water at room temperature for 12-24 hours and vacuum dry; 2) dissolving the active ingredient in water or a polyol solvent at a mass ratio of 1:4 to 500, then uniformly mixing the porous structure powder pretreated in step 1) with the active ingredient solution, and freeze-drying in a vacuum; 3) Slowly adding the mixture obtained in step 2) to the dispersing aid, stirring until homogenized, and standing at room temperature to obtain a powder; 4) Weigh 0-99 parts of vegetable oil, 0-99 parts of synthetic oil, 0.01-8 parts of material protective agent, and 0.01-1 part of flavoring and coloring agent, and stir evenly to obtain an oil solution; 5) Before use, the oil and powder prepared in the above steps are uniformly mixed at a mass ratio of 40 to 100:1 to obtain the essential oil.
8. The method for preparing an oil-powder dual-dose skin care essential oil according to claim 7, characterized in that In step 1), the vacuum drying temperature is 100-130° C., and the drying time is 4-12 hours; preferably, the temperature is 110-120° C., and the drying time is 8-10 hours.
9. The method for preparing an oil-powder dual-dose skin care essential oil according to claim 7, characterized in that In step 2), the active ingredient and water or polyol solvent are stirred at a mass ratio of 1:100-200, the porous structure powder and the active ingredient are stirred at 200-500 rpm for 20-60 minutes, and then freeze-dried under vacuum conditions of ≤5 Pa and -40°C; the stirring speed is preferably 300-400 rpm, and the stirring time is 30-40 minutes; In step 3), the mixture is added to the dispersing aid and stirred at 200-500 rpm for 5-10 minutes, homogenized at 5000-10000 rpm for 10-20 minutes, and then allowed to stand at room temperature for 4-6 hours. During the standing process, the container is gently shaken every 30 minutes to obtain a powder.
10. Use of the oil-powder dual-formulation skin care essence oil according to claim 1 in the preparation of antioxidant, whitening, firming, anti-wrinkle and repairing cosmetics.
Citation Information
Patent Citations
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