Oil-control anti-inflammatory cosmetic and preparation method thereof

Abstract

The invention belongs to the technical field of cosmetics, and particularly relates to an oil-control anti-inflammatory cosmetic and a preparation method thereof. The cosmetic comprises an active component and a matrix component, the active ingredients are prepared from the following raw materials: tea tree oil, zinc gluconate, capryloyl glycine, dipeptide diaminobutyryl benzyl amide diacetate, sodium carboxymethyl glucan, vitamin E and salicylic acid; the matrix component is prepared from the following raw materials: polyvinyl alcohol copolymerized phosphatidylcholine, carboxylated cholesterol, an emulsifier, sodium hyaluronate, coconut oil, glycerol, citric acid, polyvinylpyrrolidone, phenoxyethanol and deionized water. By combining the zinc gluconate, the low-concentration salicylic acid, the capryloyl glycine, the tea tree oil, the dipeptide diaminobutyrylbenzylamide diacetate and the sodium carboxymethyl dextran and utilizing a water-in-oil emulsion system, the skin state is comprehensively adjusted, and the problems of excessive grease secretion and inflammation are solved.

Description

Technical Field

[0001] The invention belongs to the technical field of cosmetics, and particularly relates to an oil-controlling and anti-inflammatory cosmetic and a preparation method thereof. Background Art

[0002] Cosmetics refer to chemicals or natural substances used to clean, maintain, beautify the skin or change the appearance. They are widely used in daily life to meet people's pursuit of beauty and health. With the advancement of science and technology and the development of society, people's demand for cosmetics is also changing, from simple cleaning and moisturizing to products with specific functions, such as anti-aging, whitening, oil control and anti-inflammatory. In addition, as a rapidly developing field, the cosmetics industry not only focuses on the appearance design of the product, but more importantly, its internal ingredients and technology. In recent years, consumers have paid more and more attention to product safety and effectiveness, which has prompted cosmetics manufacturers to pay more attention to research and development and use advanced science and technology to develop new products. For example, active ingredients such as plant extracts, peptides, and antioxidants are added to skin care products to achieve better skin care effects. However, with the accelerated pace of life and the intensification of environmental pollution, many people's skin problems are becoming increasingly prominent, among which excessive sebum secretion is one of the common phenomena. Excessive oil not only causes enlarged pores, but may also cause acne and other problems; therefore, products that can effectively control oil secretion have received widespread attention; at the same time, due to factors such as poor eating habits and excessive stress, the number of people with sensitive skin has gradually increased, and the skin of this group of people is more easily irritated and produces symptoms such as redness, swelling, and itching, and there is a strong demand for anti-inflammatory and repairing cosmetics. At present, there are many defects in cosmetics on the market. For example, in order to achieve the effect of rapid oil control, some products may contain high concentrations of alcohol, salicylic acid and other ingredients, which may cause irritation or dryness to sensitive skin, resulting in damage to the skin barrier; many oil control products are mainly aimed at reducing oil secretion, but they are not comprehensive enough in terms of anti-inflammation. Therefore, based on the above problems, it is extremely necessary to develop a safe, reliable, and non-irritating oil-control and anti-inflammatory cosmetic. Summary of the invention

[0003] In view of the defects of the prior art, the object of the present invention is to provide an oil-controlling anti-inflammatory cosmetic and a preparation method thereof.

[0004] The technical effect of the present invention is achieved by the following technical scheme: an oil-controlling anti-inflammatory cosmetic, which comprises an active ingredient and a matrix component; the active ingredient comprises the following raw materials in parts by weight: 0.5-1 part of tea tree oil, 0.5-0.8 part of zinc gluconate, 1-2 parts of capryloyl glycine, 0.1-0.2 part of dipeptide diaminobutyryl benzylamide diacetate, 0.5-1 part of carboxymethyl dextran sodium, 0.2-0.5 part of vitamin E and 0.5-0.7 parts of salicylic acid; the matrix component comprises the following raw materials in parts by weight: 1-2 parts of polyvinyl alcohol co-polyphosphatidylcholine, 0.5-1 parts of carboxylated cholesterol, 4-5 parts of emulsifier, 0.2-0.5 parts of sodium hyaluronate, 4-5 parts of coconut oil, 2-3 parts of glycerol, 0.1-0.2 parts of citric acid, 0.3-0.5 parts of polyvinyl pyrrolidone, 0.5-0.6 parts of phenoxyethanol and 70-80 parts of deionized water.

[0005] Preferably, the specific preparation steps of the polyvinyl alcohol co-polymerized phosphatidylcholine are as follows: A1: Add polyvinyl alcohol to deionized water, heat to 80-90°C, and stir until completely dissolved to obtain a polyvinyl alcohol solution; add phosphatidylcholine to anhydrous ethanol, stir and dissolve evenly to obtain a phosphatidylcholine solution; A2: Mix the polyvinyl alcohol solution and phosphatidylcholine solution prepared in step A1, add glutaraldehyde dropwise and stir, and slowly add sulfuric acid at the same time, control the reaction temperature to 40-60°C, continue stirring for 5-6 hours, and then add NaHCO 3 The solution was neutralized to terminate the reaction, and the solution was washed with deionized water for three times, and then vacuum dried at 60°C to a constant weight to obtain polyvinyl alcohol-co-phosphatidylcholine; Preferably, in step A1, the ratio of the amount of polyvinyl alcohol to deionized water is 1-2 g:20 mL; the ratio of the amount of phosphatidylcholine to ethanol solution is 1-2 g:20 mL; Preferably, in step A2, the volume ratio of the polyvinyl alcohol solution to the phosphatidylcholine solution is 10:1-2; the amount of glutaraldehyde is 0.2-0.5% of the sum of the volumes of the polyvinyl alcohol solution and the phosphatidylcholine solution; and the amount of sulfuric acid is 0.03-0.05% of the volume of the polyvinyl alcohol solution.

[0006] Preferably, the specific preparation steps of the carboxylated cholesterol are as follows: B1: Add cholesterol to dichloromethane, heat to 40-50°C, and stir until completely dissolved to obtain a cholesterol solution; slowly add maleic anhydride and p-toluenesulfonic acid, increase the temperature to 60-70°C, stir to react for 2-4 hours, and then cool to room temperature to obtain a mixed solution; B2: Add sodium hydroxide solution to the mixed solution prepared in step B1 to neutralize the pH to neutral, separate the organic phase from the aqueous phase with a separatory funnel, take the organic phase, remove the solvent by rotary evaporation, set the parameters of temperature to 45°C, pressure to 20-50 mbar, time to 1-2 h, wash with anhydrous ethanol, and vacuum dry at 40°C for 12-24 h to obtain carboxylated cholesterol; Preferably, in step B1, the ratio of the amount of cholesterol to dichloromethane is 1 g:20-30 mL; the mass ratio of the amount of maleic anhydride, p-toluenesulfonic acid and cholesterol is 0.6-0.8:0.005-0.01:1.

[0007] Preferably, the emulsifier is any one of caprylic / decanoic acid triglyceride, PEG-7 and Tween-80.

[0008] Preferably, another aspect of the present invention is to provide a method for preparing an oil-controlling anti-inflammatory cosmetic, and the specific preparation steps are as follows: S1: Coconut oil, tea tree oil, capryloyl glycine and vitamin E are mixed, heated to 35-40° C. in an inert atmosphere, one fifth of the weight of an emulsifier is added, and stirred at 2000 rpm for 20-30 min to obtain an oil phase; S2: dissolving polyvinyl alcohol co-polyphosphatidylcholine in deionized water at 80-90°C, cooling to 40-45°C, adding carboxylated cholesterol, stirring to dissolve evenly, then sequentially adding salicylic acid, sodium carboxymethyl dextran, zinc gluconate solution, sodium hyaluronate, dipeptide diaminobutyryl benzylamide diacetate, polyvinyl pyrrolidone and glycerol, stirring until completely dissolved evenly, then adding citric acid to adjust the pH to obtain an aqueous phase; S3: adding the remaining weight portion of the emulsifier to the aqueous phase prepared in step S2, stirring and mixing evenly, slowly dropping the oil phase prepared in step S1, pre-stirring at 1000-1500 rpm for 8-12 min, increasing the speed to 3000-4000 rpm and stirring for 10-15 min, then homogenizing at a pressure of 20-25 MPa for 3-5 times, continuously stirring at a speed of 100-300 rpm and slowly cooling to room temperature to obtain an emulsion; S4: adding phenoxyethanol to the emulsion prepared in step S3, and continuously stirring at a rotation speed of 500 to 600 rpm for 30 to 60 minutes to obtain a cosmetic.

[0009] Preferably, in step S2, the zinc gluconate solution is prepared by adding zinc gluconate to 10 parts by weight of sodium citrate-citric acid buffer; Preferably, in step S3, when the oil phase and the water phase are mixed, the oil phase is kept at a temperature of 45-50°C, and the water phase is kept at a temperature of 40-45°C; and during the homogenization treatment, the temperature is maintained at 40°C each time.

[0010] The beneficial effects of the present invention are as follows: The present invention comprehensively regulates the skin condition, improves the problem of excessive oil secretion and inflammation by combining the oil control and anti-inflammatory effect of zinc gluconate, the mild exfoliation effect of low-concentration salicylic acid, the antibacterial effect of capryloyl glycine and tea tree oil, the anti-inflammatory repair effect of dipeptide diaminobutyryl benzylamide diacetate and the moisturizing effect of carboxymethyl dextran sodium, and zinc gluconate inhibits sebaceous gland oil secretion and reduces inflammatory response to regulate the oil-water balance of the skin, and salicylic acid removes dead skin cells on the surface of the skin through exfoliation, helps to enhance the permeability of zinc gluconate, and directly exerts the oil control and anti-inflammatory effects. The exfoliation effect of salicylic acid is combined with the soothing effect of capryloyl glycine to reduce skin irritation, and enhance the permeability of other active ingredients, ensure their slow release, and provide continuous oil control and anti-inflammatory effects. Salicylic acid penetrates and removes the stratum corneum, and tea tree oil is continuously released through nano-scale oil droplets to prolong the antibacterial action time. The two coordinately regulate the balance of oil and microorganisms in stages. Dipeptide diaminobutyryl benzylamide diacetate relieves the irritation that salicylic acid may cause and promotes skin self-repair by inhibiting inflammatory factors and promoting skin barrier recovery; sodium carboxymethyl dextran forms a hydrophilic film on the skin surface, reduces water evaporation, indirectly maintains skin hydration, balances water and oil, and reduces the irritation of other ingredients to the skin. Through multiple synergistic effects, the skin's condition is comprehensively regulated, and the skin's anti-inflammatory, oil-control, antibacterial, moisturizing and other multiple functions are improved to ensure that the effect is long-lasting and gentle.

[0011] The water-in-oil emulsion system of the present invention disperses the oil phase components into tiny droplets through a homogenization process, and promotes the dispersion and release of hydrophobic components (tea tree oil, capryloyl glycine) in combination with the stabilizing effect of the emulsifier, enhances its permeability in the skin surface layer, and provides a lasting effect through sustained release, reducing irritation to the skin; the aqueous phase part provides a lasting moisturizing effect, helping to maintain skin comfort. Polyvinyl alcohol co-polyphosphatidylcholine (PVA-co-PC) and carboxylated cholesterol are used as composite emulsifiers to form a stable emulsified system by reducing interfacial tension, and wrap the oil phase droplets, delay the release of hydrophobic components (tea tree oil, capryloyl glycine), and improve their stability and skin retention time; the composite structure of micelles helps to enhance the permeability of the components, while achieving slow release, ensuring the stability of the components and reducing irritation to the skin, and the water-in-oil emulsion and citric acid regulation can effectively ensure that salicylic acid exists in the form of free acid and directly acts on the stratum corneum; in addition, carboxylated cholesterol combines with the stratum corneum of the skin through hydrophobic interaction to form a protective film, enhancing the adhesion of the emulsion. This synergistic effect not only improves the overall stability, moisturizing and permeability of the emulsion, but also provides a protective barrier for the active ingredients, slowing down their risk of oxidation and degradation, and ensuring their long-lasting and stable effects on the skin. Specifically, polyvinyl alcohol co-polyphosphatidylcholine stabilizes the emulsion structure, reduces the contact between zinc gluconate in the aqueous phase and the oil phase components, reduces its risk of degradation, and enhances its ability to penetrate the stratum corneum, ensuring better oil control and anti-inflammatory effects. In addition, ingredients such as salicylic acid, zinc gluconate, and capryloyl glycine added to the emulsion can penetrate the skin more effectively, exert their anti-inflammatory, antibacterial and oil control effects, and enhance the skin's comfort and self-repair ability. In an acidic environment, the emulsion system provides additional protection for these active ingredients to prevent them from oxidation and degradation, ensuring the stability and long-term effectiveness of the emulsion. BRIEF DESCRIPTION OF THE DRAWINGS

[0012] In order to more clearly illustrate the technical solutions in the present invention or the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings in the following description are only for the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0013] Figure 1 The biocompatibility test results of the oil-control cosmetics prepared in Examples 1 to 3 and Comparative Examples 1 to 4 of the present invention; Figure 2 This is a graph showing the antibacterial performance test results of the oil-control cosmetics prepared in Examples 1 to 3 of the present invention; Figure 3 1 is a graph showing the anti-inflammatory performance test results of the oil-control cosmetics prepared in Example 2 of the present invention and Comparative Examples 1 to 4; Figure 41 is a graph showing the antioxidant performance test results of the oil-control cosmetics prepared in Example 2 of the present invention and Comparative Examples 1 to 4; Figure 5 1 is a graph showing the stability test results of the oil-controlling anti-inflammatory cosmetics prepared in Example 2 of the present invention and Comparative Examples 1 and 4; Figure 6 1 is a graph showing the oil control performance test results of the oil control anti-inflammatory cosmetics prepared in Example 2 of the present invention and Comparative Example 4; Figure 7 This is the FTIR infrared spectrum of the polyvinyl alcohol co-polyphosphatidylcholine prepared in Example 2 of the present invention. DETAILED DESCRIPTION

[0014] The technical solution of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them; based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention. It should be noted that, unless otherwise specified, the raw materials involved in the present invention are purchased through conventional commercial channels.

[0015] Embodiment 1: An oil-controlling anti-inflammatory cosmetic, comprising an active ingredient and a matrix component; the active ingredient comprises the following raw materials in parts by weight: 0.5 parts of tea tree oil, 0.5 parts of zinc gluconate, 1 parts of capryloyl glycine, 0.1 parts of dipeptide diaminobutyryl benzylamide diacetate, 0.5 parts of sodium carboxymethyl dextran, 0.2 parts of vitamin E and 0.5 parts of salicylic acid; the matrix component comprises the following raw materials in parts by weight: 1 parts of polyvinyl alcohol co-polyphosphatidylcholine, 0.5 parts of carboxylated cholesterol, 4 parts of emulsifier, 0.2 parts of sodium hyaluronate, 4 parts of coconut oil, 2 parts of glycerin, 0.1 parts of citric acid, 0.3 parts of polyvinyl pyrrolidone, 0.5 parts of phenoxyethanol and 70 parts of deionized water.

[0016] The specific preparation steps of polyvinyl alcohol co-polymerized phosphatidylcholine are as follows: A1: Add 10g of polyvinyl alcohol to 200mL of deionized water, heat to 80°C, and stir until completely dissolved to obtain a polyvinyl alcohol solution; add 2g of phosphatidylcholine to 40mL of anhydrous ethanol, stir and dissolve evenly to obtain a phosphatidylcholine solution; A2: Mix 200 mL of polyvinyl alcohol solution prepared in step A1 and 20 mL of phosphatidylcholine solution, add 0.44 mL of glutaraldehyde dropwise and stir, add 0.06 mL of sulfuric acid at the same time, control the reaction temperature to 40 °C, continue stirring for 5 h, and add NaHCO 3 The solution was neutralized to terminate the reaction, and the solution was washed with deionized water for three times, and then vacuum dried at 60°C to a constant weight to obtain polyvinyl alcohol-co-phosphatidylcholine; The specific preparation steps of carboxylated cholesterol are as follows: B1: Add 10 g of cholesterol to 200 mL of dichloromethane, heat to 40°C, and stir until completely dissolved to obtain a cholesterol solution; then slowly add 6 g of maleic anhydride and 0.05 g of p-toluenesulfonic acid to the 200 mL cholesterol solution, increase the temperature to 60°C, stir and react for 4 hours, and then cool to room temperature to obtain a mixed solution; B2: Add sodium hydroxide solution to the mixed solution prepared in step B1 to neutralize the pH to neutral, separate the organic phase from the aqueous phase with a separatory funnel, take the organic phase, remove the solvent by rotary evaporation, set the parameters of temperature to 45°C, pressure to 50 mbar, time to 1 hour, wash with anhydrous ethanol, and vacuum dry at 40°C for 12 hours to obtain carboxylated cholesterol; The specific preparation steps of oil-controlling anti-inflammatory cosmetics are as follows: S1: Mix coconut oil, tea tree oil, capryloyl glycine and vitamin E, heat to 35°C in an inert atmosphere, add one fifth of caprylic / decanoic acid triglyceride, stir at 2000 rpm for 20-30 min, and stir until completely dissolved; S2: dissolving polyvinyl alcohol co-polyphosphatidylcholine in 80°C deionized water, cooling to 40°C, adding carboxylated cholesterol, stirring to dissolve evenly, then sequentially adding salicylic acid, sodium carboxymethyl dextran, zinc gluconate solution, sodium hyaluronate, dipeptide diaminobutyryl benzylamide diacetate, polyvinyl pyrrolidone and glycerol, stirring until completely dissolved evenly, then adding citric acid to adjust the pH to obtain an aqueous phase; S3: adding the remaining weight portion of caprylic acid triglyceride to the aqueous phase prepared in step S2, stirring and mixing evenly, slowly dropping the oil phase prepared in step S1, maintaining the temperature of the oil phase at 45°C, maintaining the temperature of the aqueous phase at 40°C, pre-stirring at 1000 rpm for 12 min, increasing the speed to 3000 rpm and stirring for 15 min, then homogenizing at a pressure of 20 MPa for 3 times, maintaining the temperature at 40°C, continuously stirring at a speed of 100 rpm and slowly cooling to room temperature to obtain an emulsion; S4: Add phenoxyethanol to the emulsion prepared in step S3, and continue stirring at a rotation speed of 500 rpm for 30 minutes to obtain an oil-controlling anti-inflammatory cosmetic.

[0017] Embodiment 2: An oil-controlling anti-inflammatory cosmetic, comprising an active ingredient and a matrix component; the active ingredient comprises the following raw materials in parts by weight: 0.8 parts of tea tree oil, 0.7 parts of zinc gluconate, 1.8 parts of capryloyl glycine, 0.15 parts of dipeptide diaminobutyryl benzylamide diacetate, 0.7 parts of sodium carboxymethyl dextran, 0.3 parts of vitamin E and 0.6 parts of salicylic acid; the matrix component comprises the following raw materials in parts by weight: 1.8 parts of polyvinyl alcohol co-polyphosphatidylcholine, 0.8 parts of carboxylated cholesterol, 4.5 parts of emulsifier, 0.4 parts of sodium hyaluronate, 4.5 parts of coconut oil, 2.5 parts of glycerin, 0.15 parts of citric acid, 0.45 parts of polyvinyl pyrrolidone, 0.55 parts of phenoxyethanol and 78 parts of deionized water.

[0018] The specific preparation steps of polyvinyl alcohol co-polymerized phosphatidylcholine are as follows: A1: Add 20g of polyvinyl alcohol to 200mL of deionized water, heat to 85°C, and stir until completely dissolved to obtain a polyvinyl alcohol solution; add 4g of phosphatidylcholine to 40mL of anhydrous ethanol, stir and dissolve evenly to obtain a phosphatidylcholine solution; A2: Mix 200 mL of polyvinyl alcohol solution prepared in step A1 and 30 mL of phosphatidylcholine solution, add 1 mL of glutaraldehyde dropwise and stir, add 0.08 mL of sulfuric acid at the same time, control the reaction temperature to 50 °C, continue stirring for 6 h, and add NaHCO 3 The solution was neutralized to terminate the reaction, and the solution was washed with deionized water for three times, and then vacuum dried at 60°C to a constant weight to obtain polyvinyl alcohol-co-phosphatidylcholine; The specific preparation steps of carboxylated cholesterol are as follows: B1: Add 10 g of cholesterol to 280 mL of dichloromethane, heat to 45°C, and stir until completely dissolved to obtain a cholesterol solution; then slowly add 7.5 g of maleic anhydride and 0.08 g of p-toluenesulfonic acid to the 280 mL cholesterol solution, increase the temperature to 65°C, stir to react for 3 hours, and then cool to room temperature to obtain a mixed solution; B2: Add sodium hydroxide solution to the mixed solution prepared in step B1 to neutralize the pH to neutral, separate the organic phase from the aqueous phase with a separatory funnel, take the organic phase, remove the solvent by rotary evaporation, set the parameters of temperature to 45°C, pressure to 30 mbar, time to 1.5 h, wash with anhydrous ethanol, and vacuum dry at 40°C for 18 h to obtain carboxylated cholesterol; The specific preparation steps of oil-controlling anti-inflammatory cosmetics are as follows: S1: Coconut oil, tea tree oil, capryloyl glycine and vitamin E are mixed, heated to 38° C. in an inert atmosphere, PEG-7 is added in one fifth by weight, and stirred at 2000 rpm for 20 to 30 min to obtain an oil phase; S2: dissolving polyvinyl alcohol co-polyphosphatidylcholine in 85°C deionized water, cooling to 43°C, adding carboxylated cholesterol, stirring to dissolve evenly, then sequentially adding salicylic acid, sodium carboxymethyl dextran, zinc gluconate solution, sodium hyaluronate, dipeptide diaminobutyryl benzylamide diacetate, polyvinyl pyrrolidone and glycerol, stirring until completely dissolved evenly, then adding citric acid to adjust the pH to obtain an aqueous phase; S3: Add the remaining weight portion of PEG-7 to the aqueous phase prepared in step S2, stir at 2000 rpm for 20-30 min, slowly dropwise add the oil phase prepared in step S1, keep the temperature of the oil phase at 48°C, keep the temperature of the aqueous phase at 43°C, pre-stir at 1200 rpm for 10 min, increase the speed to 3500 rpm and stir for 12 min, homogenize at 25 MPa for 5 times, keep the temperature at 40°C, continue stirring at 150 rpm and slowly cool to room temperature to obtain an emulsion; S4: Phenoxyethanol was added to the emulsion prepared in step S3, and the mixture was stirred at a rotation speed of 550 rpm for 50 min to obtain an oil-controlling anti-inflammatory cosmetic.

[0019] Example 3: An oil-controlling and anti-inflammatory cosmetic, comprising an active ingredient and a matrix component; the active ingredient comprises the following raw materials in parts by weight: 1 part of tea tree oil, 0.8 parts of zinc gluconate, 2 parts of capryloyl glycine, 0.2 parts of dipeptide diaminobutyryl benzylamide diacetate, 1 part of sodium carboxymethyl dextran, 0.5 parts of vitamin E and 0.7 parts of salicylic acid; the matrix component comprises the following raw materials in parts by weight: 2 parts of polyvinyl alcohol co-polyphosphatidylcholine, 1 part of carboxylated cholesterol, 5 parts of emulsifier, 0.5 parts of sodium hyaluronate, 5 parts of coconut oil, 3 parts of glycerin, 0.2 parts of citric acid, 0.5 parts of polyvinyl pyrrolidone, 0.6 parts of phenoxyethanol and 80 parts of deionized water.

[0020] The specific preparation steps of polyvinyl alcohol co-polymerized phosphatidylcholine are as follows: A1: Add 18 g of polyvinyl alcohol to 200 mL of deionized water, heat to 90°C, and stir until completely dissolved to obtain a polyvinyl alcohol solution; add 3 g of phosphatidylcholine to 40 mL of anhydrous ethanol, stir and dissolve evenly to obtain a phosphatidylcholine solution; A2: Mix 200 mL of polyvinyl alcohol solution prepared in step A1 and 40 mL of phosphatidylcholine solution, add 1.2 mL of glutaraldehyde dropwise and stir, add 0.1 mL of sulfuric acid at the same time, control the reaction temperature to 60 °C, continue stirring for 5.5 h, and add NaHCO 3 The solution was neutralized to terminate the reaction, and the solution was washed with deionized water for three times, and then vacuum dried at 60°C to a constant weight to obtain polyvinyl alcohol-co-phosphatidylcholine; The specific preparation steps of carboxylated cholesterol are as follows: B1: Add 10 g of cholesterol to 300 mL of dichloromethane, heat to 50°C, and stir until completely dissolved to obtain a cholesterol solution; then slowly add 8 g of maleic anhydride and 0.1 g of p-toluenesulfonic acid to the 300 mL cholesterol solution, increase the temperature to 70°C, stir and react for 2 hours, and then cool to room temperature to obtain a mixed solution; B2: Add sodium hydroxide solution to the mixed solution prepared in step B1 to neutralize the pH to neutral, separate the organic phase from the aqueous phase with a separatory funnel, take the organic phase, remove the solvent by rotary evaporation, set the parameters of temperature to 45°C, pressure to 20 mbar, time to 1 hour, wash with anhydrous ethanol, and vacuum dry at 40°C for 24 hours to obtain carboxylated cholesterol; The specific preparation steps of oil-controlling anti-inflammatory cosmetics are as follows: S1: Coconut oil, tea tree oil, capryloyl glycine and vitamin E are mixed, heated to 40° C. in an inert atmosphere, one fifth of Tween-80 is added, and stirred at 2000 rpm for 20 to 30 minutes to obtain an oil phase; S2: dissolving polyvinyl alcohol co-polyphosphatidylcholine in 90°C deionized water, cooling to 45°C, adding carboxylated cholesterol, stirring to dissolve evenly, then sequentially adding salicylic acid, sodium carboxymethyl dextran, zinc gluconate solution, sodium hyaluronate, dipeptide diaminobutyryl benzylamide diacetate, polyvinyl pyrrolidone and glycerol, stirring until completely dissolved evenly, then adding citric acid to adjust the pH to obtain an aqueous phase; S3: Add Tween-80 to the aqueous phase prepared in step S2, stir at 2000 rpm for 20-30 min, then slowly drop the oil phase prepared in step S1, keep the temperature of the oil phase at 50°C, keep the temperature of the aqueous phase at 45°C, pre-stir at 1500 rpm for 8 min, increase the speed to 4000 rpm and stir for 10 min, then homogenize at 23 MPa for 4 times, keep the temperature at 40°C, continue stirring at 300 rpm and slowly cool to room temperature to obtain an emulsion; S4: Phenoxyethanol is added to the emulsion prepared in step S3, and stirring is continued at a rotation speed of 600 rpm for 60 minutes to obtain an oil-controlling anti-inflammatory cosmetic.

[0021] Comparative Example 1: The operation of Comparative Example 1 is substantially the same as that of Example 2, except that polyvinyl alcohol-co-phosphatidylcholine is not added in Comparative Example 1.

[0022] Comparative Example 2: The operation of Comparative Example 2 is substantially the same as that of Example 2, except that dipeptide diaminobutyrylbenzylamide diacetate is not added in Comparative Example 2.

[0023] Comparative Example 3: The operation of Comparative Example 3 is substantially the same as that of Example 2, except that zinc gluconate is not added in Comparative Example 3.

[0024] Comparative Example 4: The operation of Comparative Example 4 is substantially the same as that of Example 2, except that, in the preparation of the cosmetic in Comparative Example 4, all ingredients are directly mixed, and no emulsifier is used.

[0025] Performance Test: Biocompatibility test: The oil-control cosmetic samples prepared in Examples 1 to 3 and Comparative Examples 1 to 4 (the cosmetic samples were mixed with DMEM culture medium at a volume ratio of 1:10, extracted at 37°C for 24 hours, and then the supernatant was centrifuged for use) were placed at the bottom of the culture plate, and 8 wells per group of samples were evenly distributed in a 96-well plate. 50 μL of DMEM culture medium was added to each well, and then the fibroblasts were diluted to 1×10 4 After that, 50 μL was inoculated into the wells with the sample added, and the temperature was set to 37°C and the concentration of CO was 5%. 2 , after culturing for 24 h and 72 h, 5 μL of 5 mg / mL MTT solution was added, and after continuing to cultivate for 4 h, the culture medium in the well was aspirated, and then 50 μL of dimethyl sulfoxide was added to the well, and the absorbance (OD value) was measured at 490 nm using a microplate reader, and the activity percentage was calculated [biocompatibility (%) = (OD value of the embodiment - OD value of the negative control group) / (OD value of the positive control group - OD value of the negative control group) × 100%], positive control group: treated with 10 wt% dimethyl sulfoxide solution; negative control group: untreated cells were used as control; cell survival rate results are shown in Figure 1 shown.

[0026] Depend on Figure 1 The results show that the cosmetics prepared by the present invention have excellent biocompatibility, will not have a negative impact on the activity of cells, and can be used effectively and safely; from the results of Comparative Example 1 and Example 2, it can be seen that PVA-co-PC is a key emulsifier and sustained-release carrier, and its absence will lead to a decrease in the stability of the emulsion, rapid release of the oil phase, and possible direct damage to cells due to excessive local concentration; due to the lack of micelle encapsulation, irritating ingredients such as salicylic acid and capryloylglycine directly contact cells, resulting in a significant impact on cell activity; from the results of Comparative Example 4 and Example 2, it can be seen that direct mixing may lead to excessive concentrations of certain ingredients, especially in local areas, which may be toxic to cells, and inadequately dissolved ingredients may precipitate or aggregate in the cell culture medium, and unemulsified salicylic acid forms a strong acidic microenvironment locally, inducing cell acidosis, thereby significantly decreasing cell survival rate.

[0027] Antibacterial test: fresh bacterial suspensions of Staphylococcus aureus, Escherichia coli and Candida albicans were prepared at a concentration of 1×10 8CFU / mL, 1 mL of bacterial solution was added to every 100 mL of culture medium, 3 plates were prepared for each bacterial species, a positive control group (Examples 1 to 3, the filter paper was directly immersed in the cosmetic solution and then dried naturally) and a negative control group (normal saline) were set up, and cultured at 37°C for 24 hours, among which Candida albicans was cultured at 27°C for 48 hours, and the size of the inhibition zone was measured and recorded. The results are as follows Figure 2 shown.

[0028] Depend on Figure 2 The results show that the cosmetics prepared by the present invention have excellent antibacterial properties, effectively inhibit bacteria, and can be used safely.

[0029] Anti-inflammatory performance test: RAW264.7 (mouse macrophages) were inoculated in a sterile culture medium containing DMEM + 10% fetal bovine serum at 37°C and CO 2 The concentration was 5%. After 48 h of incubation, the mixture was diluted to a concentration of 1 × 10 5 The cell solution of cells / mL was divided into 18 groups (1 mL per group), and the cosmetic samples prepared in Example 2 and Comparative Examples 1 to 4 were taken, and each sample was divided into 3 portions, each portion was 1 mL (0.1 mL cosmetic sample + 0.9 mL PBS buffer), and these samples were added to 15 groups of cell solutions in sequence, and the remaining 3 groups were the control groups, which were not treated in any way. After mixing, the culture was continued for 24 hours, and the cell culture supernatant was collected; 100 μL of sample from each group was added to the ELISA plate pre-coated with TNF-α antibody, and allowed to stand at room temperature for 2 hours, and washed 5 times with PBS buffer. Then, 100 μL of a secondary antibody labeled with horseradish peroxidase (HRP) diluted 1000 times was added, and the cells were allowed to stand at room temperature for 1 h. After washing three times with PBS buffer, 100 μL of a 0.1 mg / mL TMB solution was added, and the cells were allowed to stand for 15 min. 100 μL of 1 mol / L hydrochloric acid was added, and the absorbance was read at 450 nm using an enzyme reader. The anti-inflammatory activity was calculated [anti-inflammatory activity (%) = (average TNF-α concentration in the control group - average TNF-α concentration in the example) / average TNF-α concentration in the control group × 100%]. The results are shown in FIG. Figure 3 shown.

[0030] Depend on Figure 3As a result, the cosmetics prepared by the present invention can effectively reduce inflammation and inhibit the secretion of TNF-α, and have excellent anti-inflammatory properties; from the results of Comparative Example 1 and Example 2, it can be seen that the lack of polyvinyl alcohol co-polyphosphatidylcholine as an emulsifier and micelle carrier may lead to a decrease in the utilization of active ingredients, causing the active ingredients to be affected by degradation, thereby resulting in a significant decrease in the anti-inflammatory effect; from the results of Comparative Example 2 and Example 2, it can be seen that dipeptide diaminobutyryl benzylamide diacetate has an anti-inflammatory and repairing effect, can help inhibit the secretion of inflammatory factors, and is particularly important for skin barrier repair, but cannot exert its synergistic effect with other anti-inflammatory ingredients, and its lack may result in a decrease in anti-inflammatory performance; from the results of Comparative Example 3 and Example 2, it can be seen that zinc gluconate has a significant anti-inflammatory effect, and the lack of the synergistic effect of zinc gluconate may result in a significant decrease in the anti-inflammatory effect; from the results of Comparative Example 4 and Example 2, it can be seen that directly mixing all the ingredients without using an emulsifier significantly affects the stability and permeability of the active ingredients, thereby resulting in a significant decrease in the anti-inflammatory effect.

[0031] DPPH scavenging rate test: Take 2mL of DPPH solution and 2mL of the sample solution to be tested (0.1mL of the oil-control anti-inflammatory cosmetic samples of Example 2 and Comparative Examples 1 to 4 were respectively dissolved in 5mL of anhydrous ethanol), mix well, and place in the dark for 30min. With the anhydrous ethanol solution as a reference, the absorbance value at 517nm was measured. The DPPH solution is a 0.1mM solution prepared with anhydrous ethanol as the solvent. The DPPH free radical scavenging rate was calculated (scavenging rate (%) = [1-(absorbance of the mixture of sample and DPPH-absorbance of the sample solution without DPPH / absorbance of the solution containing only DPPH] × 100%). The results are as follows: Figure 4 shown.

[0032] Depend on Figure 4 As can be seen from the results, the cosmetics prepared by the present invention have excellent DPPH free radical scavenging efficiency and excellent antioxidant performance; from the results of Comparative Example 1 and Example 2, it can be seen that due to the lack of micelle encapsulation, the fat-soluble components vitamin E and tea tree oil cannot be effectively dispersed, and the antioxidant components are quickly released but the local concentration is uneven, which leads to a significant decrease in the free radical scavenging efficiency; from the results of Comparative Example 3 and Example 2, it can be seen that the lack of zinc gluconate affects the free radical scavenging ability, which leads to a weakened antioxidant effect; from the results of Comparative Example 4 and Example 2, it can be seen that direct mixing may make it difficult to evenly disperse the active ingredients, and the various active ingredients cannot effectively play their role, resulting in a significant decrease in the free radical scavenging efficiency.

[0033] Stability test: The oil-controlling anti-inflammatory cosmetic samples prepared in Example 2 of the present invention and Comparative Examples 1 and 4 were sealed in commercial packaging and placed at a temperature of 40 ± 2°C and a relative humidity of 75 ± 5% for 6 months. Samples were taken once in the first, second, third and sixth months of the test period to test the pH value. The results are as follows: Figure 5 shown.

[0034] Depend on Figure 5 The results show that the pH of the cosmetics prepared by the present invention changes stably over a long period of time without obvious fluctuations, has excellent stability, and can be effectively preserved for a long time; from the results of Comparative Example 1 and Example 2, it can be seen that due to the lack of stabilizing effect of polyvinyl alcohol co-phosphatidyl cholesterol on the emulsion, this may lead to large fluctuations in pH; from the results of Comparative Example 4 and Example 2, it can be seen that direct mixing may cause the active ingredients to be unable to be effectively preserved, the stability of the preparation is significantly affected, the active ingredients are degraded, and the pH fluctuates significantly.

[0035] Oil control test: 30 volunteers with oily skin aged between 20 and 35 were selected. The subjects were randomly divided into an experimental group and a control group, with 10 people in each group, divided into experimental group 1, 2 and a control group. Before the test, Sebumeter was used to measure the initial sebum secretion of all subjects. The experimental groups 1 and 2 used the oil-control anti-inflammatory cosmetics prepared in Example 2 and Comparative Example 4 once a day after washing their faces with clean water. The test lasted for four weeks, and measurements were taken once a week at the same time point (10 am). The sebum secretion was recorded and the oil control rate was calculated [oil control rate (%) = (1-average sebum secretion before using the product / average sebum secretion after using the product) × 100%]. The results are as follows Figure 6 As shown, at the same time, the cosmetics of Example 2 and Comparative Example 4 were scored, and the results were averaged (the full score is 5 points, and the lower the score, the more severe the discomfort), and the results are shown in Table 1.

[0036] Table 1. Rating of cosmetics usage experience

[0037] Depend on Figure 6 As can be seen from the results in Table 1, the oil-controlling anti-inflammatory cosmetics prepared by the present invention have excellent oil-control performance, have an excellent use experience, will not cause obvious discomfort to the skin and have no allergic phenomenon during use, can be effectively used for a long time and inhibit skin oil secretion, and avoid the loss of skin balance caused by excessive oil control; from the results of Comparative Example 4 and Example 2, it can be seen that the lack of a stable delivery mechanism and the protective effect of micelles, the permeability and stability of the active ingredients in the skin are poor, and the oil control effect is significantly affected.

[0038] Spectrum test: The spectrum of the polyvinyl alcohol co-polyphosphatidylcholine prepared in Example 2 was measured using an FTIR spectrometer. The results are as follows: Figure 7 shown.

[0039] Depend on Figure 7 The results show that the spectrum shows obvious ester group (C=O) stretching vibration peaks and phosphate group (P=O) vibration peaks, as well as the COC stretching vibration peak of polyvinyl alcohol. Polyvinyl alcohol co-polyphosphatidylcholine was successfully and effectively prepared.

[0040] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. An oil-controlling anti-inflammatory cosmetic, characterized in that: The composition comprises active ingredients and matrix ingredients; the active ingredients comprise the following raw materials in parts by weight: 0.5-1 parts of tea tree oil, 0.5-0.8 parts of zinc gluconate, 1-2 parts of capryloyl glycine, 0.1-0.2 parts of dipeptide diaminobutyryl benzylamide diacetate, 0.5-1 parts of carboxymethyl dextran sodium, 0.2-0.5 parts of vitamin E and 0.5-0.7 parts of salicylic acid; the matrix ingredients comprise the following raw materials in parts by weight: 1-2 parts of polyvinyl alcohol co-polyphosphatidylcholine, 0.5-1 parts of carboxylated cholesterol, 4-5 parts of emulsifier, 0.2-0.5 parts of sodium hyaluronate, 4-5 parts of coconut oil, 2-3 parts of glycerin, 0.1-0.2 parts of citric acid, 0.3-0.5 parts of polyvinyl pyrrolidine, 0.5-0.6 parts of phenoxyethanol and 70-80 parts of deionized water.

2. The oil-controlling anti-inflammatory cosmetic according to claim 1, characterized in that: The specific preparation steps of the polyvinyl alcohol co-polymerized phosphatidylcholine are as follows: A1: Add polyvinyl alcohol to deionized water, heat, and stir until completely dissolved to obtain a polyvinyl alcohol solution; add phosphatidylcholine to anhydrous ethanol, stir and dissolve evenly to obtain a phosphatidylcholine solution; A2: Mix the polyvinyl alcohol solution and phosphatidylcholine solution prepared in step A1, add glutaraldehyde dropwise and stir, add sulfuric acid at the same time, control the reaction temperature, continue stirring, add NaHCO3 solution to neutralize and terminate the reaction, repeatedly wash with deionized water, and then vacuum dry to constant weight to obtain polyvinyl alcohol co-polyphosphatidylcholine.

3. The oil-controlling anti-inflammatory cosmetic according to claim 2, characterized in that: In step A1, the ratio of the amount of polyvinyl alcohol to deionized water is 1-2 g:20 mL; the ratio of the amount of phosphatidylcholine to anhydrous ethanol is 1-2 g:20 mL.

4. The oil-controlling anti-inflammatory cosmetic according to claim 3, characterized in that: In step A2, the volume ratio of the polyvinyl alcohol solution to the phosphatidylcholine solution is 10:1-2; the amount of glutaraldehyde is 0.2-0.5% of the sum of the volumes of the polyvinyl alcohol solution and the phosphatidylcholine solution; and the amount of sulfuric acid is 0.03-0.05% of the volume of the polyvinyl alcohol solution.

5. The oil-controlling anti-inflammatory cosmetic according to claim 4, characterized in that: The specific preparation steps of the carboxylated cholesterol are as follows: B1: Add cholesterol to dichloromethane, heat, and stir until completely dissolved to obtain a cholesterol solution; then slowly add maleic anhydride and p-toluenesulfonic acid to the cholesterol solution, increase the temperature, stir to react, and cool to room temperature to obtain a mixed solution; B2: Add sodium hydroxide solution to the mixed solution prepared in step B1 to neutralize the pH to neutral, separate the organic phase from the aqueous phase using a separatory funnel, take the organic phase, remove the solvent by rotary evaporation, wash with anhydrous ethanol, and vacuum dry to obtain carboxylated cholesterol.

6. The oil-controlling anti-inflammatory cosmetic according to claim 5, characterized in that: In step B1, the ratio of the cholesterol to dichloromethane is 1 g:20-30 mL; the ratio of the maleic anhydride, p-toluenesulfonic acid and cholesterol is 0.6-0.8:0.005-0.01:

1.

7. The oil-controlling and anti-inflammatory cosmetic according to claim 6, characterized in that: The emulsifier is any one of caprylic / capric triglyceride, PEG-7 and Tween-80.

8. A method for preparing the oil-controlling anti-inflammatory cosmetic according to any one of claims 1 to 7, characterized in that: The specific preparation steps are as follows: S1: Coconut oil, tea tree oil, capryloyl glycine and vitamin E are mixed, heated under a nitrogen atmosphere, and one fifth of the weight of an emulsifier is added, and stirred to obtain an oil phase; S2: dissolving polyvinyl alcohol co-polyphosphatidylcholine in hot deionized water, adding carboxylated cholesterol after cooling, stirring to dissolve evenly, then sequentially adding salicylic acid, sodium carboxymethyl dextran, zinc gluconate solution, sodium hyaluronate, dipeptide diaminobutyryl benzylamide diacetate, polyvinyl pyrrolidone and glycerol, stirring until completely dissolved evenly, then adding citric acid to adjust the pH to obtain an aqueous phase; S3: adding the remaining weight portion of the emulsifier to the water phase prepared in step S2, stirring and mixing evenly, slowly dropping the oil phase prepared in step S1, pre-stirring, then increasing the speed of stirring, homogenizing, and then continuing stirring and slowly cooling to room temperature to obtain an emulsion; S4: adding phenoxyethanol to the emulsion prepared in step S3, and continuously stirring to obtain a cosmetic.

9. The method for preparing the oil-controlling anti-inflammatory cosmetic according to claim 8, characterized in that: In step S3, when the oil phase and the water phase are mixed, the oil phase is kept at a temperature of 45-50°C, and the water phase is kept at a temperature of 40-45°C; during the homogenization treatment, the temperature is maintained at 40°C each time.

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