An oil-control and anti-inflammatory cosmetic and its preparation method

Abstract

The present invention belongs to the technical field of cosmetics, and particularly relates to an oil-control and anti-inflammatory cosmetic and a preparation method thereof. The composition of the cosmetic includes active ingredients and matrix components; the active ingredients are composed of the following raw materials: tea tree oil, zinc gluconate, capryloyl glycine, dipeptide diamino butyryl benzylamide diacetate, carboxymethyl dextran sodium, vitamin E, and salicylic acid; the matrix components are composed of the following raw materials: polyvinyl alcohol copolymer phosphatidylcholine, carboxylated cholesterol, emulsifier, sodium hyaluronate, coconut oil, glycerol, citric acid, polyvinylpyrrolidone, phenoxyethanol, and deionized water. By combining zinc gluconate, low-concentration salicylic acid, capryloyl glycine, tea tree oil, dipeptide diamino butyryl benzylamide diacetate, and carboxymethyl dextran sodium, and using a water-in-oil emulsion system, the present invention comprehensively regulates the skin condition and improves the problems of excessive sebum secretion and inflammation.

Description

Technical Field

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

[0002] Cosmetics refer to chemical products or natural substances used for cleaning, maintaining, beautifying the skin or changing appearance. They are widely used in daily life to meet people's pursuit of beauty and health. With the progress of technology and the development of society, people's demand for cosmetics is constantly changing, from simple cleaning and moisturizing to products with specific functions, such as anti-aging, whitening, oil control and anti-inflammation. In addition, as a rapidly developing field, the cosmetics industry not only focuses on the appearance design of products, but more importantly, its internal components and technologies. In recent years, consumers have paid more and more attention to the safety and effectiveness of products, which has prompted cosmetics manufacturers to pay more attention to research and development and adopt advanced scientific technologies to develop new products. For example, adding active ingredients such as plant extracts, peptides, antioxidants, etc. to skin care products to achieve better skin care effects. However, with the acceleration of the pace of life and the aggravation of environmental pollution, many people's skin problems have become increasingly prominent, and excessive sebum secretion is one of the common phenomena. Excessive oil not only causes enlarged pores, but may also cause problems such as acne; therefore, products that can effectively control oil secretion have received wide attention; at the same time, due to factors such as poor eating habits and excessive stress, the population of sensitive skin is gradually expanding, and the skin of this group is more likely to be stimulated and produce symptoms such as redness, swelling and itching, and there is a strong demand for anti-inflammatory and repair cosmetics. At present, there are many defects in the cosmetics on the market. For example, in order to achieve the effect of rapid oil control, some products may contain high concentrations of ingredients such as alcohol and salicylic acid, which may cause irritation or dryness to sensitive skin and damage the skin barrier; many oil control products mainly focus on reducing oil secretion, but 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] Aiming at the defects of the prior art, the purpose of the present invention is to provide an oil-control and anti-inflammatory cosmetic and a preparation method thereof.

[0004] The technical effects of the present invention are achieved through the following technical solutions: An oil-control and anti-inflammatory cosmetic, the composition of which includes active ingredients and matrix ingredients; the composition of the active ingredients includes the following raw materials in parts by weight: 0.5 to 1 part of tea tree oil, 0.5 to 0.8 part of zinc gluconate, 1 to 2 parts of capryloyl glycine, 0.1 to 0.2 part of dipeptide diaminobutyryl benzylamide diacetate, 0.5 to 1 part of carboxymethyl glucan sodium, 0.2 to 0.5 part of vitamin E, and 0.5 to 0.7 part of salicylic acid; the composition of the matrix ingredients includes the following raw materials in parts by weight: 1 to 2 parts of polyvinyl alcohol copolymerized phosphatidylcholine, 0.5 to 1 part of carboxylated cholesterol, 4 to 5 parts of emulsifier, 0.2 to 0.5 part of sodium hyaluronate, 4 to 5 parts of coconut oil, 2 to 3 parts of glycerol, 0.1 to 0.2 part of citric acid, 0.3 to 0.5 part of polyvinylpyrrolidone, 0.5 to 0.6 part of phenoxyethanol, and 70 to 80 parts of deionized water.

[0005] Preferably, the specific preparation steps of the polyvinyl alcohol copolymerized phosphatidylcholine are as follows:

[0006] 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 absolute ethanol, stir and dissolve evenly to obtain a phosphatidylcholine solution;

[0007] A2: Mix the polyvinyl alcohol solution and the phosphatidylcholine solution prepared in step A1, dropwise add glutaraldehyde and stir, while slowly adding sulfuric acid, control the reaction temperature at 40 - 60 °C, continuously stir for 5 - 6 h, then add NaHCO3 solution to neutralize and terminate the reaction, wash with deionized water 3 times repeatedly, and then vacuum dry at 60 °C to constant weight to obtain polyvinyl alcohol copolymerized phosphatidylcholine;

[0008] Preferably, in step A1, the dosage ratio of polyvinyl alcohol to deionized water is 1 - 2 g:20 mL; the dosage ratio of phosphatidylcholine to ethanol solution is 1 - 2 g:20 mL;

[0009] Preferably, in step A2, the volume dosage ratio of the polyvinyl alcohol solution to the phosphatidylcholine solution is 10:1 - 2; the dosage of glutaraldehyde is 0.2 - 0.5% of the sum of the volumes of the polyvinyl alcohol solution and the phosphatidylcholine solution; the dosage of sulfuric acid is 0.03 - 0.05% of the volume of the polyvinyl alcohol solution.

[0010] Preferably, the specific preparation steps of the carboxylated cholesterol are as follows:

[0011] 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, raise the temperature to 60 - 70 °C, stir and react for 2 - 4 h, then cool to room temperature to obtain a mixed solution;

[0012] B2: Add sodium hydroxide solution to the mixed solution prepared in step B1 to neutralize the pH to neutral. Separate the organic phase and the aqueous phase with a separatory funnel. Take the organic phase, remove the solvent by rotary evaporation, set the parameters: temperature 45°C, pressure 20 - 50 mbar, time 1 - 2 h, wash with absolute ethanol, and dry in vacuum at 40°C for 12 - 24 h to obtain carboxylated cholesterol;

[0013] Preferably, in step B1, the dosage ratio of cholesterol to dichloromethane is 1 g:20 - 30 mL; the mass dosage ratio of maleic anhydride, p-toluenesulfonic acid to cholesterol is 0.6 - 0.8:0.005 - 0.01:1.

[0014] Preferably, the emulsifier is any one of glyceryl caprylate, PEG-7, and Tween-80.

[0015] Preferably, on the other hand, the present invention provides a method for preparing an oil-control and anti-inflammatory cosmetic, and the specific preparation steps are as follows:

[0016] S1: Mix coconut oil, tea tree oil, capryloyl glycine, and vitamin E, heat to 35 - 40°C in an inert atmosphere, add one-fifth weight part of the emulsifier, and stir at 2000 rpm for 20 - 30 min to obtain an oil phase;

[0017] S2: Dissolve polyvinyl alcohol copolymerized phosphatidylcholine in deionized water at 80 - 90°C, cool to 40 - 45°C, then add carboxylated cholesterol, stir to dissolve evenly, and then add salicylic acid, sodium carboxymethyl dextran, zinc gluconate solution, sodium hyaluronate, dipeptide diamino butyryl benzylamide diacetate, polyvinylpyrrolidone, and glycerol in sequence, stir until completely dissolved and evenly mixed, and then add citric acid to adjust the pH to obtain an aqueous phase;

[0018] S3: Add the remaining weight part of the emulsifier to the aqueous phase prepared in step S2, stir and mix evenly, then slowly dropwise add the oil phase prepared in step S1. After pre-stirring at 1000 - 1500 rpm for 8 - 12 min, increase the rotation speed to 3000 - 4000 rpm and stir for 10 - 15 min, and then homogenize at a pressure of 20 - 25 MPa for 3 - 5 times, and continuously stir at a rotation speed of 100 - 300 rpm and slowly cool to room temperature to obtain an emulsion;

[0019] S4: Add phenoxyethanol to the emulsion prepared in step S3, and continuously stir at a rotation speed of 500 - 600 rpm for 30 - 60 min to obtain a cosmetic.

[0020] Preferably, in step S2, the zinc gluconate solution is prepared by adding zinc gluconate to 10 times the weight part of sodium citrate-citric acid buffer solution;

[0021] Preferably, in step S3, when the oil phase and the water phase are mixed, the temperature of the oil phase is maintained at 45-50 °C, and the temperature of the water phase is maintained at 40-45 °C; for the homogenization treatment, the temperature is maintained at 40 °C each time.

[0022] The beneficial effects of the present invention are as follows:

[0023] By combining the oil-control and anti-inflammatory effects of zinc gluconate, the mild exfoliating effect of low-concentration salicylic acid, the antibacterial effects of capryloyl glycine and tea tree oil, as well as the anti-inflammatory and repair effects of dipeptide diaminobutyroyl benzylamide diacetate and the moisturizing efficacy of sodium carboxymethyl dextran, the present invention comprehensively regulates the skin condition, improves the problems of excessive sebum secretion and inflammation. Zinc gluconate regulates the oil-water balance of the skin by inhibiting sebum secretion of sebaceous glands and reducing inflammatory reactions. Salicylic acid removes dead skin cells on the skin surface through exfoliation, helps enhance the permeability of zinc gluconate, and directly exerts oil-control and anti-inflammatory effects. The exfoliating 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, ensuring their slow release and providing continuous oil-control and anti-inflammatory effects. Salicylic acid penetrates and removes the stratum corneum, and tea tree oil is continuously released through nano-sized oil droplets, prolonging the antibacterial action time. The two synergistically regulate the balance of oil and microorganisms in stages. Dipeptide diaminobutyroyl benzylamide diacetate relieves the possible irritation caused by salicylic acid by inhibiting inflammatory factors and promoting the restoration of the skin barrier, and promotes skin self-repair; 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 a variety of synergistic effects, the skin condition is comprehensively regulated, and the multiple effects of anti-inflammatory, oil-control, antibacterial, and moisturizing of the skin are improved, ensuring long-lasting and mild effects.

[0024] The oil-in-water emulsion system of the present invention disperses the oil-phase components into tiny droplets through a homogenization process. Combining with the stabilizing effect of the emulsifier, it promotes the dispersion and release of hydrophobic components (tea tree oil, capryloyl glycine), enhances their permeability on the skin surface, and provides a long-lasting effect through continuous release, reducing irritation to the skin; the aqueous phase provides a long-lasting moisturizing effect to help maintain skin comfort. Polyvinyl alcohol copolymerized phosphatidylcholine (PVA-co-PC) and carboxylated cholesterol are used as composite emulsifiers to form a stable emulsion system by reducing the interfacial tension and encapsulate the oil-phase droplets, delaying the release of hydrophobic components (tea tree oil, capryloyl glycine), improving their stability and skin residence time; the composite structure of the micelles helps enhance the permeability of the components and achieve slow release, ensuring the stability of the components and reducing irritation to the skin. The oil-in-water emulsion and citric acid adjustment can effectively ensure that salicylic acid exists in the free acid form and directly acts on the stratum corneum; in addition, carboxylated cholesterol binds to the skin stratum corneum through hydrophobic interactions to form a protective film, enhancing the adhesion of the emulsion. This synergistic effect not only improves the overall stability, moisturizing property, and permeability of the emulsion but also provides a protective barrier for the active ingredients, slowing down the risk of their oxidation and degradation, and ensuring a long-lasting and stable effect on the skin. Specifically, polyvinyl alcohol copolymerized phosphatidylcholine stabilizes the emulsion structure, reduces the contact between zinc gluconate in the aqueous phase and the oil-phase components, reduces its degradation risk, and at the same time 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 at the same time enhance the skin comfort and self-repair ability. In an acidic environment, the emulsion system provides additional protection for these active ingredients to prevent their oxidation and degradation, ensuring the stability and long-term effectiveness of the emulsion. Brief Description of the Drawings

[0025] In order to more clearly illustrate the technical solutions in the present invention or the prior art, the following will briefly introduce the drawings required for use in the description of the embodiments or the prior art. Obviously, the drawings in the following description are only those of the present invention. For those of ordinary skill in the art, without creative efforts, other drawings can also be obtained based on these drawings.

[0026] Figure 1 It is the biocompatibility test results of the oil-control cosmetics prepared in Examples 1-3 and Comparative Examples 1-4 of the present invention;

[0027] Figure 2 It is the test result diagram of the antibacterial performance of the oil-control cosmetics prepared in Examples 1-3 of the present invention;

[0028] Figure 3 It is the test result diagram of the anti-inflammatory performance of the oil-control cosmetics prepared in Example 2 and Comparative Examples 1-4 of the present invention;

[0029] Figure 4 It is a graph showing the test results of the antioxidant performance of the oil-control cosmetics prepared in Example 2 and Comparative Examples 1-4 of the present invention;

[0030] Figure 5 It is a graph showing the test results of the stability of the oil-control and anti-inflammatory cosmetics prepared in Example 2 and Comparative Examples 1 and 4 of the present invention;

[0031] Figure 6 It is a graph showing the test results of the oil-control performance of the oil-control and anti-inflammatory cosmetics prepared in Example 2 and Comparative Example 4 of the present invention;

[0032] Figure 7 It is the FTIR infrared spectrum of polyvinyl alcohol copolyphosphatidylcholine prepared in Example 2 of the present invention. Detailed implementation mode

[0033] Next, the technical solutions of the present invention will be clearly and completely described in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments; based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts belong to 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.

[0034] Example 1: An oil-control and anti-inflammatory cosmetic, the composition of which includes active ingredients and matrix components; the composition of the active ingredients includes the following raw materials in parts by weight: 0.5 part of tea tree oil, 0.5 part of zinc gluconate, 1 part of capryloyl glycine, 0.1 part of dipeptide diamino butyryl benzyl amide diacetate, 0.5 part of carboxymethyl glucan sodium, 0.2 part of vitamin E and 0.5 part of salicylic acid; the composition of the matrix components includes the following raw materials in parts by weight: 1 part of polyvinyl alcohol copolyphosphatidylcholine, 0.5 part of carboxylated cholesterol, 4 parts of emulsifier, 0.2 part of sodium hyaluronate, 4 parts of coconut oil, 2 parts of glycerol, 0.1 part of citric acid, 0.3 part of polyvinylpyrrolidone, 0.5 part of phenoxyethanol and 70 parts of deionized water.

[0035] The specific preparation steps of polyvinyl alcohol copolyphosphatidylcholine are as follows:

[0036] A1: Add 10 g of polyvinyl alcohol to 200 mL of deionized water, heat to 80 °C, and stir until completely dissolved to obtain a polyvinyl alcohol solution; add 2 g of phosphatidylcholine to 40 mL of absolute ethanol, stir and dissolve evenly to obtain a phosphatidylcholine solution;

[0037] A2: Mix the 200 mL of polyvinyl alcohol solution and 20 mL of phosphatidylcholine solution prepared in step A1, dropwise add 0.44 mL of glutaraldehyde and stir, while adding 0.06 mL of sulfuric acid, control the reaction temperature at 40 °C, continue stirring for 5 h, then add NaHCO3 solution to neutralize and terminate the reaction, wash with deionized water repeatedly for 3 times, and then dry in vacuum at 60 °C to constant weight to obtain polyvinyl alcohol copolymerized phosphatidylcholine;

[0038] The specific preparation steps of carboxylated cholesterol are as follows:

[0039] B1: Add 10 g of cholesterol to 200 mL of dichloromethane, heat to 40 °C, 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 200 mL of the cholesterol solution, raise the temperature to 60 °C, stir and react for 4 h, and then cool to room temperature to obtain a mixed solution;

[0040] B2: Add sodium hydroxide solution to the mixed solution prepared in step B1 to neutralize the pH to neutral, separate the organic phase and the aqueous phase with a separatory funnel, take the organic phase, remove the solvent by rotary evaporation, set the parameters of temperature at 45 °C, pressure at 50 mbar, time at 1 h, wash with absolute ethanol, and dry in vacuum at 40 °C for 12 h to obtain carboxylated cholesterol;

[0041] The specific preparation steps of the oil-control and anti-inflammatory cosmetic are as follows:

[0042] S1: Mix coconut oil, tea tree oil, capryloyl glycine and vitamin E, in an inert atmosphere, heat to 35 °C, add one-fifth weight part of triglyceride caprylate / caprate, stir at 2000 rpm for 20 - 30 min until completely dissolved;

[0043] S2: Dissolve polyvinyl alcohol copolymerized phosphatidylcholine in deionized water at 80 °C, cool to 40 °C, then add carboxylated cholesterol, stir to dissolve evenly, and then add salicylic acid, carboxymethyl dextran sodium, zinc gluconate solution, sodium hyaluronate, dipeptide diaminobutyryl benzylamide diacetate, polyvinylpyrrolidone and glycerol in sequence, stir until completely dissolved evenly, and then add citric acid to adjust the pH to obtain an aqueous phase;

[0044] S3: Add the remaining weight part of triglyceride caprylate / caprate to the aqueous phase prepared in step S2, stir and mix evenly, then slowly dropwise add the oil phase prepared in step S1, keep the temperature of the oil phase at 45 °C and the temperature of the aqueous phase at 40 °C, pre-stir at 1000 rpm for 12 min, then increase the rotation speed to 3000 rpm and stir for 15 min, and then homogenize at 20 MPa for 3 times, keep the temperature at 40 °C, and continue to stir at a rotation speed of 100 rpm and slowly cool to room temperature to obtain an emulsion;

[0045] S4: Add phenoxyethanol to the emulsion prepared in step S3, and continuously stir at a speed of 500 rpm for 30 min to obtain an oil-control and anti-inflammatory cosmetic.

[0046] Example 2: An oil-control and anti-inflammatory cosmetic, the composition of which includes active ingredients and matrix ingredients; the composition of the active ingredients includes the following raw materials by weight: 0.8 parts of tea tree oil, 0.7 parts of zinc gluconate, 1.8 parts of octanoyl glycine, 0.15 parts of dipeptide diaminobutyryl benzylamide diacetate, 0.7 parts of carboxymethyl glucan sodium, 0.3 parts of vitamin E, and 0.6 parts of salicylic acid; the composition of the matrix ingredients includes the following raw materials by weight: 1.8 parts of polyvinyl alcohol copolyphosphatidylcholine, 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 glycerol, 0.15 parts of citric acid, 0.45 parts of polyvinylpyrrolidone, 0.55 parts of phenoxyethanol, and 78 parts of deionized water.

[0047] The specific preparation steps of polyvinyl alcohol copolyphosphatidylcholine are as follows:

[0048] A1: Add 20 g of polyvinyl alcohol to 200 mL of deionized water, heat to 85 °C, and stir until completely dissolved to obtain a polyvinyl alcohol solution; add 4 g of phosphatidylcholine to 40 mL of absolute ethanol, stir and dissolve evenly to obtain a phosphatidylcholine solution.

[0049] A2: Mix 200 mL of the polyvinyl alcohol solution prepared in step A1 and 30 mL of the phosphatidylcholine solution, dropwise add 1 mL of glutaraldehyde and stir, while adding 0.08 mL of sulfuric acid, control the reaction temperature at 50 °C, continuously stir for 6 h, then add NaHCO3 solution to neutralize and terminate the reaction, wash with deionized water repeatedly for 3 times, and then vacuum dry at 60 °C to constant weight to obtain polyvinyl alcohol copolyphosphatidylcholine.

[0050] The specific preparation steps of carboxylated cholesterol are as follows:

[0051] 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 280 mL of the cholesterol solution, raise the temperature to 65 °C, stir and react for 3 h, and then cool to room temperature to obtain a mixed solution.

[0052] B2: Add sodium hydroxide solution to the mixed solution prepared in step B1 to neutralize the pH to neutral, separate the organic phase and the aqueous phase with a separatory funnel, take the organic phase, rotate and evaporate to remove the solvent, set the parameters: temperature 45 °C, pressure 30 mbar, time 1.5 h, wash with absolute ethanol, and vacuum dry at 40 °C for 18 h to obtain carboxylated cholesterol.

[0053] The specific preparation steps of the oil-control and anti-inflammatory cosmetic are as follows:

[0054] S1: Mix coconut oil, tea tree oil, capryloyl glycine, and vitamin E. In an inert atmosphere, heat to 38 °C, add one-fifth of the weight portion of PEG-7, and stir at 2000 rpm for 20 - 30 min to obtain the oil phase.

[0055] S2: Dissolve polyvinyl alcohol copolyphosphatidylcholine in deionized water at 85 °C. After cooling to 43 °C, add carboxylated cholesterol and stir to dissolve evenly. Then, successively add salicylic acid, carboxymethyl dextran sodium, zinc gluconate solution, sodium hyaluronate, dipeptide diamino butyryl benzylamide diacetate, polyvinylpyrrolidone, and glycerol, and stir until completely dissolved and homogeneous. Then, add citric acid to adjust the pH to obtain the aqueous phase.

[0056] S3: Add the remaining weight portion of PEG-7 to the aqueous phase prepared in step S2. After stirring 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 and the temperature of the aqueous phase at 43 °C. After pre-stirring at 1200 rpm for 10 min, increase the rotation speed to 3500 rpm and stir for 12 min. Homogenize at a pressure of 25 MPa for 5 times, keep the temperature at 40 °C, and continuously stir at a rotation speed of 150 rpm and slowly cool to room temperature to obtain the emulsion.

[0057] S4: Add phenoxyethanol to the emulsion prepared in step S3 and continuously stir at 550 rpm for 50 min to obtain the oil-control and anti-inflammatory cosmetic.

[0058] Example 3: An oil-control and anti-inflammatory cosmetic, whose composition includes active ingredients and matrix components; the composition of the active ingredients includes the following raw materials by weight portion: 1 part of tea tree oil, 0.8 part of zinc gluconate, 2 parts of capryloyl glycine, 0.2 part of dipeptide diamino butyryl benzylamide diacetate, 1 part of carboxymethyl dextran sodium, 0.5 part of vitamin E, and 0.7 part of salicylic acid; the composition of the matrix components includes the following raw materials by weight portion: 2 parts of polyvinyl alcohol copolyphosphatidylcholine, 1 part of carboxylated cholesterol, 5 parts of emulsifier, 0.5 part of sodium hyaluronate, 5 parts of coconut oil, 3 parts of glycerol, 0.2 part of citric acid, 0.5 part of polyvinylpyrrolidone, 0.6 part of phenoxyethanol, and 80 parts of deionized water.

[0059] The specific preparation steps of polyvinyl alcohol copolyphosphatidylcholine are as follows:

[0060] 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 absolute ethanol, stir to dissolve evenly to obtain a phosphatidylcholine solution.

[0061] A2: Mix the 200 mL of polyvinyl alcohol solution and 40 mL of phosphatidylcholine solution prepared in step A1, dropwise add 1.2 mL of glutaraldehyde and stir, while adding 0.1 mL of sulfuric acid, control the reaction temperature at 60 °C, continue stirring for 5.5 h, then add NaHCO3 solution to neutralize and terminate the reaction, wash with deionized water 3 times repeatedly, and then dry in vacuum at 60 °C to constant weight to obtain polyvinyl alcohol copolymerized phosphatidylcholine;

[0062] The specific preparation steps of carboxylated cholesterol are as follows:

[0063] B1: Add 10 g of cholesterol to 300 mL of dichloromethane, heat to 50 °C, 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 of cholesterol solution, raise the temperature to 70 °C, stir and react for 2 h, and then cool to room temperature to obtain a mixed solution;

[0064] B2: Add sodium hydroxide solution to the mixed solution prepared in step B1 to neutralize the pH to neutral, separate the organic phase and the aqueous phase with a separatory funnel, take the organic phase, rotate and evaporate to remove the solvent, set the parameters: temperature 45 °C, pressure 20 mbar, time 1 h, wash with absolute ethanol, and dry in vacuum at 40 °C for 24 h to obtain carboxylated cholesterol;

[0065] The specific preparation steps of the oil-control and anti-inflammatory cosmetic are as follows:

[0066] S1: Mix coconut oil, tea tree oil, capryloyl glycine and vitamin E, in an inert atmosphere, heat to 40 °C, add one-fifth weight portion of Tween-80, stir at 2000 rpm for 20 - 30 min to obtain an oil phase;

[0067] S2: Dissolve polyvinyl alcohol copolymerized phosphatidylcholine in deionized water at 90 °C, cool to 45 °C, then add carboxylated cholesterol, stir to dissolve evenly, and then add salicylic acid, carboxymethyl dextran sodium, zinc gluconate solution, sodium hyaluronate, dipeptide diamino butyryl benzylamide diacetate, polyvinylpyrrolidone and glycerol in sequence, stir until completely dissolved evenly, and then add citric acid to adjust the pH to obtain an aqueous phase;

[0068] S3: Add Tween-80 to the aqueous phase prepared in step S2, stir at 2000 rpm for 20 - 30 min, then slowly dropwise add the oil phase prepared in step S1, keep the temperature of the oil phase at 50 °C and the temperature of the aqueous phase at 45 °C, pre-stir at 1500 rpm for 8 min, then increase the rotation speed to 4000 rpm and stir for 10 min, and then homogenize at a pressure of 23 MPa for 4 times, keep the temperature at 40 °C, and continuously stir at a rotation speed of 300 rpm and slowly cool to room temperature to obtain an emulsion;

[0069] S4: Add phenoxyethanol to the emulsion prepared in step S3, and continuously stir at a speed of 600 rpm for 60 min to obtain an oil-control and anti-inflammatory cosmetic.

[0070] Comparative Example 1: The operation of Comparative Example 1 is basically the same as that of Example 2, except that polyvinyl alcohol copolyphosphatidylcholine is not added in Comparative Example 1.

[0071] Comparative Example 2: The operation of Comparative Example 2 is basically the same as that of Example 2, except that dipeptide diamino butyryl benzyl amide diacetate is not added in Comparative Example 2.

[0072] Comparative Example 3: The operation of Comparative Example 3 is basically the same as that of Example 2, except that zinc gluconate is not added in Comparative Example 3.

[0073] Comparative Example 4: The operation of Comparative Example 4 is basically the same as that of Example 2, except that in the preparation of the cosmetic in Comparative Example 4, all components are directly mixed and no emulsifier is used.

[0074] Performance test:

[0075] Biocompatibility test: Place the oil-control cosmetic samples prepared in Examples 1-3 and Comparative Examples 1-4 (mix the cosmetic samples with DMEM medium at a volume ratio of 1:10, centrifuge after extraction at 37 °C for 24 hours, and take the supernatant for use) at the bottom of the culture plate, evenly distribute 8 wells of each group of samples in a 96-well plate, add 50 μL of DMEM medium to each well, then dilute Fibroblasts fibroblasts to 1×10 4 cells / mL and inoculate 50 μL into the wells added with the samples above. Set the temperature at 37 °C and the CO2 concentration at 5%. Add 5 μL of 5 mg / mL MTT solution after culturing for 24 h and 72 h respectively. After continuing to culture for 4 h, aspirate the culture solution in the wells, then add 50 μL of dimethyl sulfoxide to the wells, measure the absorbance (OD value) at 490 nm using an enzyme-linked immunosorbent assay (ELISA) reader, and calculate the activity percentage [biocompatibility (%) = (OD value of the example - 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 a 10 wt% dimethyl sulfoxide solution; negative control group: untreated cells as a control; the results of cell viability are as Figure 1 shown.

[0076] From Figure 1It can be seen from the results 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 as a key emulsifier and sustained-release carrier, the absence of PVA-co-PC 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 too high local concentration; lacking micelle encapsulation, irritating components such as salicylic acid and octanoyl glycine directly contact cells, resulting in a significant impact on cell activity; from the results of Comparative Example 4 and Example 2, direct mixing may lead to too high concentration of some components, especially in local areas, which may be toxic to cells, and the undissolved components may precipitate or aggregate in the cell culture medium. The unemulsified salicylic acid forms a strong acidic microenvironment locally, causing cell acidosis, and then leading to a significant decrease in cell viability.

[0077] Antibacterial test: Fresh bacterial solutions of Staphylococcus aureus, Escherichia coli and Candida albicans were prepared, and the bacterial solution concentration was 1×10 8 CFU / mL. Add 1 mL of the bacterial solution to every 100 mL of the culture medium. Three plates were prepared for each strain. A positive control group (Examples 1-3, the filter paper was directly immersed in the cosmetic solution and then air-dried naturally) and a negative control group (physiological saline) were set. Incubate at 37 °C for 24 h, and incubate Candida albicans at 27 °C for 48 h. Measure and record the size of the inhibition zone. The results are as Figure 2 shown.

[0078] From Figure 2 the results, it can be seen that the cosmetics prepared by the present invention have excellent antibacterial properties, can effectively inhibit bacteria, and can be used safely.

[0079] Anti-inflammatory performance test: RAW264.7 (mouse macrophages) were inoculated in a sterile culture medium of DMEM + 10% fetal bovine serum at a temperature of 37 °C and a CO2 concentration of 5%. After culturing for 48 h, it was diluted to a concentration of 1×10 5A cell solution of [[X]] cells / mL was divided into 18 groups (1 mL per group). Cosmetic samples prepared in Example 2 and Comparative Examples 1-4 were taken, and each sample was divided into 3 portions, each portion being 1 mL (0.1 mL cosmetic sample + 0.9 mL PBS buffer). These samples were sequentially added to the cell solutions of 15 groups, and the remaining 3 groups were used as control groups without any treatment. After mixing, the cells were cultured for another 24 h, and the cell culture supernatant was collected. For each group, 100 μL of the sample was added to an ELISA plate pre-coated with TNF-α antibody and allowed to stand at room temperature for 2 h. After washing 5 times with PBS buffer, 100 μL of a secondary antibody labeled with horseradish peroxidase (HRP) diluted 1000-fold was added and allowed to stand at room temperature for 1 h. After washing three times with PBS buffer, 100 μL of 0.1 mg / mL TMB solution was added and allowed to stand for 15 min. Then 100 μL of 1 moL / L hydrochloric acid was added, and the absorbance was measured at 450 nm using an enzyme-linked immunosorbent assay (ELISA) reader. The anti-inflammatory effect was calculated [Anti-inflammatory effect (%) = (Average TNF-α concentration in the control group - Average TNF-α concentration in the example group) / Average TNF-α concentration in the control group × 100%]. The results are as Figure 3 shown.

[0080] As can be Figure 3 seen from the results, 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 copolyphosphatidylcholine as an emulsifier and micelle carrier may lead to a decrease in the utilization rate of the active ingredient, resulting in the degradation of the active ingredient and thus a significant decrease in the anti-inflammatory effect. From the results of Comparative Example 2 and Example 2, it can be seen that dipeptide diamino butyryl benzylamide diacetate has an anti-inflammatory and repair effect, can help inhibit the secretion of inflammatory factors, and is particularly important for skin barrier repair. However, it cannot exert its synergistic effect with other anti-inflammatory components, and its lack may lead to a decrease in anti-inflammatory performance. From the results of Comparative Example 3 and Example 2, it can be seen that zinc gluconate has an obvious anti-inflammatory effect, and the lack of the synergistic effect of zinc gluconate may lead to 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 components without using an emulsifier significantly affects the stability and permeability of the active ingredient, resulting in a significant decrease in the anti-inflammatory effect.

[0081] DPPH scavenging rate test: Take 2 mL of DPPH solution and 2 mL of the sample solution to be tested (for the oil-control and anti-inflammatory cosmetic samples in Example 2 and Comparative Examples 1-4, take 0.1 mL and dissolve it in 5 mL of absolute ethanol respectively), mix well, place in the dark for 30 min, use the absolute ethanol solution as a reference, measure the absorbance value at 517 nm. The DPPH solution is a solution with a concentration of 0.1 mM prepared with absolute ethanol as the solvent, and calculate the DPPH radical scavenging rate (scavenging rate (%) = [1 - (absorbance of the sample and DPPH mixture - absorbance of the sample solution without DPPH / absorbance of the DPPH solution only)] × 100%), and the results are as Figure 4 shown.

[0082] As can be Figure 4 seen from the results, the DPPH radical scavenging efficiency of the cosmetics prepared by the present invention is extremely good, and it has excellent antioxidant properties; from the results of Comparative Example 1 and Example 2, it can be seen that without micelle encapsulation, the fat-soluble components vitamin E and tea tree oil cannot be effectively dispersed, the antioxidant components are rapidly 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 ability to scavenge free radicals, which leads to a weakening of the antioxidant effect; from the results of Comparative Example 4 and Example 2, it can be seen that direct mixing may cause the active ingredients to be difficult to disperse evenly, and various active ingredients cannot effectively play their roles, resulting in a significant decrease in the free radical scavenging efficiency.

[0083] Stability test: Seal the oil-control and anti-inflammatory cosmetic samples prepared in Example 2 and Comparative Examples 1 and 4 of the present invention according to the commercial packaging, place them at a temperature of 40 ± 2 °C and a relative humidity of 75 ± 5% for 6 months, and take samples once each at the 1st, 2nd, 3rd, and 6th months during the test period to test the pH value, and the results are as Figure 5 shown.

[0084] As can be Figure 5 seen from the results, the pH of the cosmetics prepared by the present invention changes stably over a long time, without obvious fluctuations, has excellent stability, and can be effectively stored for a long time; from the results of Comparative Example 1 and Example 2, it can be seen that due to the lack of the stabilizing effect of polyvinyl alcohol copolymerized phosphatidylcholine on the emulsion, this may lead to a large fluctuation in pH; from the results of Comparative Example 4 and Example 2, it can be seen that due to direct mixing, the active ingredients may not be effectively preserved, the stability of the preparation is significantly affected, and the active ingredients degrade, which leads to a significant fluctuation in pH.

[0085] Oil control test: 30 volunteers with oily skin, aged between 20 and 35 years old, were randomly divided into an experimental group and a control group, with 10 people in each group, divided into experimental groups 1, 2 and the control group. Before the start of the test, the initial sebum secretion of all subjects was measured using a Sebumeter. Experimental groups 1 and 2 used the oil-control and anti-inflammatory cosmetics prepared in Example 2 and Comparative Example 4 once a day after washing their faces with water. The test lasted for four weeks, and measurements were taken at the same time point (10 am) every week to record the sebum secretion, 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 Figure 6 shown. At the same time, the cosmetics of Example 2 and Comparative Example 4 were scored, and the results were averaged (the full score of the score is 5 points, and the lower the score, the more serious the discomfort). The results are shown in Table 1.

[0086] Table 1. Score of the experience of using cosmetics

[0087]

[0088] From Figure 6 and the results in Table 1, it can be seen that the oil-control and anti-inflammatory cosmetics prepared by the present invention have excellent oil control performance, and have excellent use experience. It will not cause obvious discomfort to the skin during use and there is no allergic phenomenon. It can be effectively used for a long time to inhibit skin oil secretion, and at the same time 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 due to 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.

[0089] Spectrum test: The spectrum of polyvinyl alcohol copolyphosphatidylcholine prepared in Example 2 was measured using an FTIR spectrometer, and the results are as Figure 7 shown.

[0090] From Figure 7 the results, it can be seen that obvious stretching vibration peaks of ester groups (C=O) and vibration peaks of phosphate ester groups (P=O) are shown in the spectrum, and at the same time, the C-O-C stretching vibration peak of polyvinyl alcohol is shown, indicating that polyvinyl alcohol copolyphosphatidylcholine was successfully and effectively prepared.

[0091] Although the embodiments of the present invention have been shown and described, for those of ordinary skill in the art, it can be understood that various changes, modifications, substitutions and variations can be made to these embodiments without departing from the principles and spirit of the present invention. The scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. An oil-control and anti-inflammatory cosmetic, characterized in that, It comprises an active ingredient and a matrix ingredient; the composition of the active ingredient includes the following raw materials 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 glucan sodium, 0.2 - 0.5 part of vitamin E, and 0.5 - 0.7 part of salicylic acid; the composition of the matrix ingredient includes the following raw materials by weight: 1 - 2 parts of polyvinyl alcohol copoly phosphatidylcholine, 0.5 - 1 part of carboxylated cholesterol, 4 - 5 parts of emulsifier, 0.2 - 0.5 part of sodium hyaluronate, 4 - 5 parts of coconut oil, 2 - 3 parts of glycerol, 0.1 - 0.2 part of citric acid, 0.3 - 0.5 part of polyvinylpyrrolidone, 0.5 - 0.6 part of phenoxyethanol, and 70 - 80 parts of deionized water; The specific preparation steps of the polyvinyl alcohol copoly 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 absolute ethanol, stir and dissolve evenly to obtain a phosphatidylcholine solution; A2: Mix the polyvinyl alcohol solution and the phosphatidylcholine solution prepared in step A1, dropwise add glutaraldehyde and stir, while adding sulfuric acid, control the reaction temperature, continuously stir, add NaHCO3 solution to neutralize and terminate the reaction, wash repeatedly with deionized water, and then vacuum dry to constant weight to obtain polyvinyl alcohol copoly phosphatidylcholine; The emulsifier is any one of triglyceride caprylic / capric acid, PEG - 7, and Tween - 80; The specific preparation steps of the oil - control and anti - inflammatory cosmetic are as follows: S1: Mix coconut oil, tea tree oil, capryloyl glycine, and vitamin E, heat under a nitrogen atmosphere, add one - fifth of the weight part of the emulsifier, and stir to obtain an oil phase; S2: Dissolve polyvinyl alcohol copoly phosphatidylcholine in high - temperature deionized water, add carboxylated cholesterol after cooling, stir and dissolve evenly, and then successively add salicylic acid, carboxymethyl glucan sodium, zinc gluconate solution, sodium hyaluronate, dipeptide diaminobutyryl benzylamide diacetate, polyvinylpyrrolidone, and glycerol, stir until completely dissolved and evenly mixed, and then add citric acid to adjust the pH to obtain an aqueous phase; S3: Add the remaining weight part of the emulsifier to the aqueous phase prepared in step S2, stir and mix evenly, slowly drop the oil phase prepared in step S1, perform pre - stirring, then increase the rotation speed for stirring, homogenize, and then continuously stir and slowly cool to room temperature to obtain an emulsion; S4: Add phenoxyethanol to the emulsion prepared in step S3, and continuously stir to obtain the cosmetic.

2. The oil-control and anti-inflammatory cosmetic according to claim 1, wherein In step A1, the dosage ratio of polyvinyl alcohol to deionized water is 1 - 2 g:20 mL; the dosage ratio of phosphatidylcholine to absolute ethanol is 1 - 2 g:20 mL.

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

4. The oil-control and anti-inflammatory cosmetic according to claim 3, characterized in that, The specific preparation steps of the carboxylated cholesterol are as follows: B1: Add cholesterol into 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, raise the temperature, stir and react, and cool to room temperature to obtain a mixed solution; B2: Add a sodium hydroxide solution to the mixed solution prepared in step B1 to neutralize the pH to neutral, separate the organic phase and the aqueous phase with a separatory funnel, take the organic phase, rotary evaporate to remove the solvent, wash with absolute ethanol, and vacuum dry to obtain carboxylated cholesterol.

5. The oil-control and anti-inflammatory cosmetic according to claim 4, wherein In step B1, the dosage ratio of cholesterol to dichloromethane is 1 g: 20-30 mL; the mass dosage ratio of maleic anhydride, p-toluenesulfonic acid to cholesterol is 0.6-0.8: 0.005-0.01:

1.

6. The oil-control and anti-inflammatory cosmetic according to claim 5, characterized in that, In step S3, when the oil phase and the aqueous phase are mixed, the oil phase is maintained at a temperature of 45-50 °C, and the aqueous phase is maintained at a temperature of 40-45 °C; for the homogenization treatment, a temperature of 40 °C is maintained each time.

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