Anti-mite and anti-dandruff shampoo and preparation method thereof

Abstract

The invention relates to the technical field of daily chemical products, and discloses acarus-killing and dandruff-removing shampoo and a preparation method thereof. The preparation method comprises the following steps: carrying out surface modification on the eugenol / functionalized mesoporous nano silicon dioxide composite material with antibacterial, acarus-killing and anti-dandruff effects by adopting lipidosome, further carrying out surface modification on cholesterol modified hyaluronic acid by adopting a post-insertion method, and mixing the obtained antibacterial acarus-killing agent with an anti-dandruff agent and water to obtain the acarus-killing and anti-dandruff composition. The shampoo obtained by compounding and mixing the cationic polymer, the surfactant, the thickening agent, the essence, the mite-removing and dandruff-removing composition and the water is excellent in antibacterial and mite-removing effects and has a good dandruff-removing effect.

Description

Technical Field

[0001] The invention relates to the technical field of daily chemical products, and in particular to a mite and dandruff-removing shampoo and a preparation method thereof. Background Art

[0002] Dandruff is a phenomenon of excessive flaking caused by excessive proliferation of keratinocytes on the scalp. The main cause of dandruff is the excessive proliferation of Malassezia, a type of lipophilic fungus that parasitizes on the surface of human and animal skin. Its fungus contains enzymes that can decompose lipids. When the sebaceous glands of the skin secrete vigorously, it can hydrolyze most of the triglycerides in the sebum into free fatty acids. The unsaturated fatty acids produced by it will stimulate the skin barrier and cause the stratum corneum to fall off, thereby triggering an inflammatory response. Demodicid mites belong to the Demodicidae family of the order Acarina. Demodex ), is a type of permanent parasitic mite that parasitizes the hair follicles, sebaceous glands or internal organs of many mammals. Mechanical stimulation of the worm body and chemical stimulation of its secretions and excretions can cause inflammatory reactions in skin tissue. Human Demodex mites destroy epithelial cells and glandular cells, causing hair follicle expansion and epithelial degeneration. The manifestations of skin lesions are diffuse flushing of the local skin, abnormal sebum exudation, significant enlargement of hair follicles, rough surface, and even uneven. In diseases such as hair loss, folliculitis, seborrheic dermatitis, acne, rosacea, and blepharitis, the parasitism of Demodex mites is one of the main causes.

[0003] At present, there are three main types of anti-dandruff agents commonly used in anti-dandruff products: keratin exfoliants, cell growth inhibitors and antifungal preparations. Keratin exfoliants have a certain degree of exfoliation effect, but they are highly irritating and can damage the stratum corneum if used for a long time; cell growth inhibitors improve keratinization and desquamation symptoms by reducing the turnover rate of stratum corneum cells, but they make hair dry and easily cause inflammatory reactions after use; antifungal preparations mainly include piroctone ethanolamine salt, climbazole, etc., but there are still defects in their application and certain limitations.

[0004] Prior art, such as Chinese patent application CN118340710A, discloses an application of an anti-dandruff oil-control composition in the preparation of a hair care product and a hair care product. When the anti-dandruff oil-control composition is added to the hair care product, the components can be compounded to enhance each other's effectiveness, which is beneficial to the repair and conditioning of the scalp skin. However, the anti-dandruff oil-control composition prepared by the invention adopts a compound of multiple active components, and the mite removal effect and sustained-release transdermal effect of the active ingredients need to be improved. Summary of the invention

[0005] The purpose of the present invention is to overcome the deficiencies of the prior art and provide a mite and dandruff removing shampoo and a preparation method thereof. By adding a mite and dandruff removing composition, the shampoo has excellent antibacterial and mite removing effects and good dandruff removing effects.

[0006] In order to achieve the above object, the technical solution adopted by the present invention is as follows: a method for preparing a mite and dandruff removing composition, comprising the following steps: Step (1), mixing amino mesoporous nano-silica, dopamine hydrochloride, and solvent B, ultrasonically dispersing, adding ammonium persulfate, reacting, centrifuging, and washing after the reaction is completed to obtain polydopamine-modified mesoporous nano-silica; mixing polydopamine-modified mesoporous nano-silica, eugenol, and ethanol, loading, centrifuging, and washing to obtain an intermediate product; mixing the intermediate product, alkylated hydrophobically modified polyethyleneimine, water, and ethanol, reacting, centrifuging, filtering, and washing to obtain a eugenol / functionalized mesoporous nano-silica composite material; Step (2), mixing eugenol / functionalized mesoporous nano-silica composite material, soybean lecithin, cholesterol, and solvent A, ultrasonically dispersing, rotary evaporating, adding cholesterol-modified hyaluronic acid suspension, hydrating, ultrasonically treating, centrifuging to remove supernatant, filtering membrane, and obtaining an antibacterial and mite-removing agent; Step (3), mixing the antibacterial and anti-mite agent, the anti-dandruff agent and water evenly to obtain an anti-mite and anti-dandruff composition.

[0007] Preferably, in step (1), the mass ratio of amino mesoporous nano-silica, dopamine hydrochloride, solvent B, and ammonium persulfate is 1: 0.2-0.22: 480-550: 0.24-0.26; when preparing polydopamine-modified mesoporous nano-silica, the reaction conditions are: stirring the reaction at a speed of 80-100 r / min and a temperature of 25-30°C for 8-12 hours.

[0008] Furthermore, the solvent B is a HEPES buffer solution.

[0009] Preferably, in step (1), the mass ratio of polydopamine-modified mesoporous nano-silica, eugenol, and ethanol is 0.1:10-12:80-100; the loading conditions are: stirring the loading at room temperature for 12-20 hours; the mass ratio of the intermediate product, alkylated hydrophobically modified polyethyleneimine, water, and ethanol is 1:1-1.2:40-60:40-60; when preparing the eugenol / functionalized mesoporous nano-silica composite material, the reaction conditions are: stirring the reaction at a speed of 80-100 r / min and a temperature of 25-30°C for 20-26 hours.

[0010] Preferably, in step (2), the mass ratio of eugenol / functionalized mesoporous nano-silica composite material, soybean lecithin, cholesterol, solvent A, and cholesterol-modified hyaluronic acid suspension is 1:14-15:6-7:180-200:900-1000, and solvent A is prepared by mixing chloroform and methanol in a volume ratio of 3:1-2.

[0011] Preferably, in step (2), the rotary evaporation conditions are: rotary evaporation at 40-50°C for 25-30 min; the hydration treatment conditions are: hydration treatment at 45-55°C for 30-60 min; the ultrasonic treatment conditions are: ultrasonic treatment at 0°C for 10 min; and the filter membrane is a 0.6-0.8 μm filter membrane.

[0012] Preferably, in step (2), the cholesterol-modified hyaluronic acid suspension is prepared by the following steps: mixing and dissolving cholesterol, N,N'-dicyclohexylcarbodiimide, 4-dimethylaminopyridine and N,N-dimethylformamide to obtain a cholesterol mixed solution; mixing sodium hyaluronate, water and Tween 80 evenly, adding the cholesterol mixed solution dropwise, reacting after the addition is complete, and purifying after the reaction is complete to obtain cholesterol-modified hyaluronic acid; mixing the cholesterol-modified hyaluronic acid and PBS buffer solution evenly to obtain a cholesterol-modified hyaluronic acid suspension.

[0013] Preferably, in step (2), when preparing the cholesterol-modified hyaluronic acid suspension: the mass ratio of cholesterol, N,N'-dicyclohexylcarbodiimide, 4-dimethylaminopyridine, and N,N-dimethylformamide is 3.8-4:4.9-5:0.24-0.25:190-210; the mass ratio of sodium hyaluronate, water, and Tween 80 is 0.4-0.5:100-120:5; the mass ratio of cholesterol to sodium hyaluronate is 0.95-1:1; the reaction conditions are: reaction at a temperature of 20-25°C for 40-48h; the mass ratio of cholesterol-modified hyaluronic acid to PBS buffer solution is 1:900-1000.

[0014] Preferably, in step (2), when preparing the cholesterol-modified hyaluronic acid suspension: the purification operation includes: dialyzing the mixture with water in a dialysis bag with a molecular weight cutoff of 12 kDa for 72 hours, centrifuging and filtering the mixture after the treatment, and freeze-drying the filtrate at -40°C for 48 hours.

[0015] Preferably, in step (3), the mass ratio of the antibacterial and decarcinogenic agent, the antidandruff agent, and water is 30-40:1-1.5:70; the antidandruff agent is preferably one of piroctone ethanolamine and climbazole.

[0016] Preferably, a mite and anti-dandruff composition is obtained by the preparation method of the mite and anti-dandruff composition as described above.

[0017] The invention discloses a method for preparing an anti-dandruff shampoo by using the anti-dandruff shampoo. The method comprises the following steps: mixing a cationic polymer and water evenly and then heating the mixture, adding a surfactant and a thickener, stirring the mixture while keeping the mixture warm, cooling the mixture, adding essence and the anti-dandruff shampoo, continuing to stir the mixture evenly, adding a regulator to adjust the pH value, adjusting the viscosity, cooling the mixture and discharging the mixture to obtain the anti-dandruff shampoo.

[0018] Preferably, the weight percentages of the components in the mite and dandruff removing shampoo are: 2-3% cationic polymer, 25-27% surfactant, 1-1.5% thickener, 0.3-0.5% flavor, 10-15% mite and dandruff removing composition, and the balance is water; the cationic polymer is preferably one or two of polyquaternium-10 and guar hydroxypropyltrimethylammonium chloride; the surfactant is preferably two or more of ammonium laureth sulfate, ammonium lauryl sulfate, and cocamidopropyl betaine; the thickener is preferably isostearamide MIPA.

[0019] Preferably, an anti-dandruff and mite shampoo is obtained by the preparation method of the anti-dandruff and mite shampoo as described above.

[0020] Compared with the prior art, the invention has the following beneficial effects: eugenol has biological activities such as antibacterial and anti-inflammatory, has excellent killing effects on Demodex and Malassezia, and can be used in combination with traditional antidandruff agents to improve the bactericidal and antidandruff effects; in the invention, dopamine is polymerized on the surface of amino mesoporous nano-silica to obtain polydopamine-modified mesoporous nano-silica, and when the mesoporous nano-silica is used as a carrier to load eugenol, since polydopamine has rich functional groups and aromatic ring structures, efficient loading of the antibacterial active substance eugenol can be achieved through hydrogen bonding and π-π stacking, thereby improving the loading amount and stability of eugenol; liposomes are nano-carriers with a phospholipid bilayer structure composed of phospholipids and cholesterol, and the special phospholipid bilayer structure can better penetrate the intercellular spaces of the stratum corneum, and can be used as a carrier to achieve the transdermal effect of the active ingredient, so that the active ingredient can play a role for a long time; at the same time, since the phospholipids in the liposomes have a strong hydration ability, the hydration of the stratum corneum can be enhanced. The present invention utilizes the Schiff base reaction and Michael addition reaction between polydopamine on the surface of polydopamine-modified mesoporous nano-silica loaded with eugenol and polyethyleneimine to introduce alkylated hydrophobically modified polyethyleneimine into the carrier surface to obtain a eugenol / functionalized mesoporous nano-silica composite material. The antibacterial property of the composite material is improved by introducing polyethyleneimine, and at the same time, since the long-chain alkyl hydrophobic chain segments are modified on the surface of the composite material, the hydrophobic interaction between the long-chain alkyl hydrophobic chain segments and phospholipids can be utilized to realize lipid assembly. Soybean lecithin and cholesterol are used as liposome matrix materials for liposomes by a thin film hydration method. The surface of the phenol / functionalized mesoporous nano-silica composite material is modified, and then the cholesterol-modified hyaluronic acid is embedded in the lipid bilayer of the liposome by the post-insertion method to obtain an antibacterial and anti-mite agent with excellent anti-dandruff, antibacterial and acaricidal properties; wherein, the cholesterol-modified hyaluronic acid is prepared by introducing the cholesterol hydrophobic structure into the hyaluronic acid structure by a chemical grafting method, and the hydrophobic end of the prepared amphiphilic polymer has a cholesterol structure and can be embedded in the lipid bilayer of the liposome, while the hydrophilic end has a hyaluronic acid molecular structure, which improves the water retention performance of the material and improves the dispersibility of the antibacterial and anti-mite agent in water.

[0021] The present invention prepares an anti-mite and anti-dandruff composition by compounding an anti-bacterial and anti-mite agent, an anti-dandruff agent and solvent water, and introduces the anti-mite and anti-dandruff composition into a shampoo formula as an anti-mite and anti-dandruff active ingredient. The prepared shampoo has excellent anti-bacterial and anti-mite effects and good anti-dandruff effects. During use, the shampoo can be allowed to stay on the scalp for 5-10 minutes according to actual needs to achieve better anti-mite and anti-dandruff effects. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 This is a process flow chart for preparing the mite and dandruff-removing shampoo of the present invention; Figure 2It is a bar graph of the mite killing time of the shampoos prepared in Examples 4-6 and Comparative Examples 2-3 of the present invention in the mite killing performance test; Figure 3 It is a bar graph of the antibacterial rates of the shampoos prepared in Examples 4-6 and Comparative Examples 2-3 of the present invention in the anti-dandruff performance test. DETAILED DESCRIPTION

[0023] The technical solutions in the embodiments 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, rather than all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention.

[0024] Example 1 This embodiment discloses a method for preparing a mite and dandruff removing composition, comprising the following steps: Step (1), amino mesoporous nano-silica, dopamine hydrochloride, and HEPES buffer solution are mixed, ultrasonically dispersed for 3 minutes, ammonium persulfate is added, and the mixture is stirred at a speed of 80 r / min and a temperature of 25° C. for 12 hours. After the reaction is completed, the mixture is centrifuged, and the centrifugal precipitate is taken, and water 8 times the mass of the centrifugal precipitate is added to wash the mixture three times to obtain polydopamine-modified mesoporous nano-silica; wherein the mass ratio of amino mesoporous nano-silica, dopamine hydrochloride, HEPES buffer solution, and ammonium persulfate is 1:0.2:480:0.24; the polydopamine-modified mesoporous nano-silica is added to the mixture, and the mixture is stirred at a speed of 80 r / min and a temperature of 25° C. for 12 hours. Silicon oxide, eugenol, and ethanol are mixed in a mass ratio of 0.1:10:80, and stirred for loading at room temperature for 12 hours. After loading, centrifuge, take the centrifugal precipitate, add water 8 times the mass of the centrifugal precipitate to wash three times to obtain an intermediate product, mix the intermediate product, alkylated hydrophobically modified polyethyleneimine, water, and ethanol in a mass ratio of 1:1:60:40, stir and react at a speed of 80r / min and a temperature of 25°C for 26 hours, centrifuge, filter, take the filter cake, add water 5 times the mass of the filter cake to wash, and obtain a eugenol / functionalized mesoporous nano-silica composite material; Step (2), mixing eugenol / functionalized mesoporous nano-silica composite material, soybean lecithin, cholesterol, and solvent, ultrasonically dispersing for 10 minutes, rotary evaporating at 40°C for 30 minutes, adding cholesterol-modified hyaluronic acid suspension, hydrating at 45°C for 60 minutes, ultrasonically treating at 0°C for 10 minutes after the treatment, centrifuging to remove the supernatant, filtering through a 0.6 μm filter membrane, and obtaining an antibacterial and mite-removing agent; wherein the mass ratio of eugenol / functionalized mesoporous nano-silica composite material, soybean lecithin, cholesterol, solvent, and cholesterol-modified hyaluronic acid suspension is 1:14:7:180:900, and the solvent is prepared by mixing chloroform and methanol in a volume ratio of 3:1; the cholesterol-modified hyaluronic acid suspension comprises the following steps: mixing cholesterol, N,N'-dicyclohexylcarbodiimide, 4-dimethylaminopyridine and N,N-dimethylformamide are mixed and dissolved in a mass ratio of 3.9:4.9:0.24:200 to obtain a cholesterol mixture; sodium hyaluronate, water, and Tween 80 are mixed at a mass ratio of 0.45:110:5 at 25°C, and the cholesterol mixture is added dropwise, the mass ratio of cholesterol to sodium hyaluronate is 0.95:1, and the dropping time is 10 minutes. After the dropping is completed, the reaction is carried out at 20°C for 48 hours. After the reaction is completed, water is used for dialysis treatment in a dialysis bag with a molecular weight cutoff of 12kDa for 72 hours. After the treatment is completed, centrifugation, filtration, and the filtrate is taken, and freeze-dried at -40°C for 48 hours to obtain cholesterol-modified hyaluronic acid; cholesterol-modified hyaluronic acid and PBS buffer solution are mixed at a mass ratio of 1:900 to obtain a cholesterol-modified hyaluronic acid suspension; Step (3), mixing the antibacterial and anti-mite agent, the anti-dandruff agent and water in a mass ratio of 30:1:70 to obtain an anti-mite and anti-dandruff composition; wherein the anti-dandruff agent is piroctone ethanolamine salt.

[0025] Example 2 This embodiment discloses a method for preparing a mite and dandruff removing composition, comprising the following steps: Step (1), amino mesoporous nano-silica, dopamine hydrochloride, and HEPES buffer solution are mixed, ultrasonically dispersed for 5 minutes, ammonium persulfate is added, and the mixture is stirred at a speed of 100 r / min and a temperature of 25° C. for 10 hours. After the reaction is completed, the mixture is centrifuged, and the centrifugal precipitate is taken, and water 8 times the mass of the centrifugal precipitate is added to wash the mixture three times to obtain polydopamine-modified mesoporous nano-silica; wherein the mass ratio of amino mesoporous nano-silica, dopamine hydrochloride, HEPES buffer solution, and ammonium persulfate is 1:0.21:520:0.25; the polydopamine-modified mesoporous nano-silica is added to the mixture to obtain the polydopamine-modified mesoporous nano-silica. Silicon oxide, eugenol, and ethanol are mixed in a mass ratio of 0.1:11:90, and stirred for loading at room temperature for 16 hours. After loading, centrifuge, take the centrifugal precipitate, add water 8 times the mass of the centrifugal precipitate to wash three times to obtain an intermediate product, mix the intermediate product, alkylated hydrophobically modified polyethyleneimine, water, and ethanol in a mass ratio of 1:1.1:50:50, stir and react at a speed of 80r / min and a temperature of 25°C for 24 hours, centrifuge, filter, take the filter cake, add water 5 times the mass of the filter cake to wash, and obtain a eugenol / functionalized mesoporous nano-silica composite material; Step (2), mixing eugenol / functionalized mesoporous nano-silica composite material, soybean lecithin, cholesterol, and solvent, ultrasonically dispersing for 10 minutes, rotary evaporating at 40°C for 30 minutes, adding cholesterol-modified hyaluronic acid suspension, hydrating at 50°C for 40 minutes, ultrasonically treating at 0°C for 10 minutes after the treatment, centrifuging to remove the supernatant, filtering through a 0.7 μm filter membrane, and obtaining an antibacterial and mite-removing agent; wherein the mass ratio of eugenol / functionalized mesoporous nano-silica composite material, soybean lecithin, cholesterol, solvent, and cholesterol-modified hyaluronic acid suspension is 1:14.5:6.5:190:950, and the solvent is prepared by mixing chloroform and methanol in a volume ratio of 3:1.5; the cholesterol-modified hyaluronic acid suspension comprises the following steps: the preparation of cholesterol-modified hyaluronic acid is the same as in Example 1; cholesterol-modified hyaluronic acid and PBS buffer solution are uniformly mixed in a mass ratio of 1:950 to obtain a cholesterol-modified hyaluronic acid suspension; Step (3), mixing the antibacterial and anti-mite agent, the anti-dandruff agent and water in a mass ratio of 35:1.3:70 to obtain an anti-mite and anti-dandruff composition; wherein the anti-dandruff agent is piroctone ethanolamine salt.

[0026] Example 3 This embodiment discloses a method for preparing a mite and dandruff removing composition, comprising the following steps: Step (1), amino mesoporous nano-silica, dopamine hydrochloride, and HEPES buffer solution are mixed, ultrasonically dispersed for 5 minutes, ammonium persulfate is added, and the mixture is stirred at a speed of 100 r / min and a temperature of 30° C. for 8 hours. After the reaction is completed, the mixture is centrifuged, and the centrifugal precipitate is taken, and water 10 times the mass of the centrifugal precipitate is added to wash the mixture three times to obtain polydopamine-modified mesoporous nano-silica; wherein the mass ratio of amino mesoporous nano-silica, dopamine hydrochloride, HEPES buffer solution, and ammonium persulfate is 1:0.22:550:0.26; the polydopamine-modified mesoporous nano-silica is added to the mixture, and the mixture is stirred at a speed of 100 r / min and a temperature of 30° C. for 8 hours. Silicon dioxide, eugenol, and ethanol are mixed in a mass ratio of 0.1:12:100, and stirred at room temperature for loading for 20 hours. After loading, centrifuge, take the centrifugal precipitate, add water 10 times the mass of the centrifugal precipitate to wash three times to obtain an intermediate product, mix the intermediate product, alkylated hydrophobically modified polyethyleneimine, water, and ethanol in a mass ratio of 1:1.2:40:60, stir and react at a speed of 100 r / min and a temperature of 30°C for 20 hours, centrifuge, filter, take the filter cake, add water 8 times the mass of the filter cake to wash, and obtain a eugenol / functionalized mesoporous nano-silica composite material; Step (2), mixing eugenol / functionalized mesoporous nano-silica composite material, soybean lecithin, cholesterol, and solvent, ultrasonically dispersing for 10 minutes, rotary evaporating at 50°C for 25 minutes, adding cholesterol-modified hyaluronic acid suspension, hydrating at 55°C for 30 minutes, ultrasonically treating at 0°C for 10 minutes, centrifuging to remove the supernatant, and filtering through a 0.8 μm filter membrane to obtain an antibacterial and mite-removing agent; wherein the mass ratio of eugenol / functionalized mesoporous nano-silica composite material, soybean lecithin, cholesterol, solvent, and cholesterol-modified hyaluronic acid suspension is 1:15:6:200:1000, and the solvent is prepared by mixing chloroform and methanol in a volume ratio of 3:2; the cholesterol-modified hyaluronic acid suspension comprises the following steps: the preparation of cholesterol-modified hyaluronic acid is the same as in Example 1; cholesterol-modified hyaluronic acid and PBS buffer solution are uniformly mixed in a mass ratio of 1:1000 to obtain a cholesterol-modified hyaluronic acid suspension; Step (3), mixing the antibacterial and anti-mite agent, the anti-dandruff agent and water in a mass ratio of 40:1.5:70 to obtain an anti-mite and anti-dandruff composition; wherein the anti-dandruff agent is climbazole.

[0027] Example 4 The present embodiment discloses a method for preparing a mite and dandruff removing shampoo, comprising the following steps: uniformly mixing a cationic polymer and water, heating to 70°C, adding a surfactant and a thickener, stopping heating when the temperature continues to rise to 75°C, stirring at the temperature for 10 minutes, cooling to 40°C, adding an essence and the mite and dandruff removing composition prepared in Example 1, continuing stirring until the mixture is uniformly mixed, adding a regulating agent citric acid to adjust the pH value to 6.2, adjusting the viscosity of the system, discharging the material when the temperature drops to below 40°C, and obtaining the mite and dandruff removing shampoo; wherein the weight percentage of each component in the mite and dandruff removing shampoo is: 2% of the cationic polymer, 27% of the surfactant, 1.5% of the thickener, 0.3% of the essence, 10% of the mite and dandruff removing composition, and the remainder is water; the cationic polymer is polyquaternium-10; the surfactant is prepared by mixing ammonium laureth sulfate, ammonium lauryl sulfate, and cocamidopropyl betaine in a mass ratio of 14:7:5; and the thickener is isostearamide MIPA.

[0028] Example 5 The present embodiment discloses a method for preparing a mite and dandruff removing shampoo, comprising the following steps: uniformly mixing a cationic polymer and water, heating to 80°C, adding a surfactant and a thickener, stirring at the temperature for 10 minutes, cooling to 40°C, adding an essence and the mite and dandruff removing composition prepared in Example 2, continuing to stir until uniformly mixed, adding a regulating agent citric acid to adjust the pH value to 6, adjusting the viscosity of the system, discharging the material when the temperature is lowered to below 40°C, and obtaining the mite and dandruff removing shampoo; wherein the weight percentage of each component in the mite and dandruff removing shampoo is: 2.5% of the cationic polymer, 26% of the surfactant, 1.5% of the thickener, 0.3% of the essence, 13% of the mite and dandruff removing composition, and the remainder is water; the cationic polymer is polyquaternium-10; the surfactant is prepared by mixing ammonium laureth sulfate and cocamidopropyl betaine in a mass ratio of 16:7; and the thickener is isostearamide MIPA.

[0029] Example 6 The present embodiment discloses a method for preparing a mite and dandruff removing shampoo, comprising the following steps: uniformly mixing a cationic polymer and water, heating to 80°C, adding a surfactant and a thickener, stirring at the temperature for 10 minutes, cooling to 40°C, adding an essence and the mite and dandruff removing composition prepared in Example 3, continuing to stir until the mixture is uniform, adding a regulating agent citric acid to adjust the pH value to 6.5, adjusting the viscosity of the system, discharging the material when the temperature is lowered to below 40°C, and obtaining the mite and dandruff removing shampoo; wherein the weight percentage of each component in the mite and dandruff removing shampoo is: 3% of the cationic polymer, 25% of the surfactant, 1% of the thickener, 0.5% of the essence, 15% of the mite and dandruff removing composition, and the balance is water; the cationic polymer is guar hydroxypropyltrimethylammonium chloride; the surfactant is prepared by mixing ammonium laureth sulfate and cocamidopropyl betaine in a mass ratio of 16:7; and the thickener is isostearamide MIPA.

[0030] Comparative Example 1 This comparative example discloses a method for preparing a mite and dandruff removing composition, comprising the following steps: Step (1), mixing mesoporous nano-silica, eugenol, and ethanol in a mass ratio of 0.1:10:80, stirring and loading at room temperature for 12 hours, centrifuging after the loading is completed, taking the centrifugal precipitate, adding water 8 times the mass of the centrifugal precipitate and washing it three times to obtain a eugenol / mesoporous nano-silica composite material; Step (2), mixing eugenol / mesoporous nano-silica composite material, soybean lecithin, cholesterol and solvent, ultrasonically dispersing for 10 minutes, rotary evaporating at 40°C for 30 minutes, adding cholesterol-modified hyaluronic acid suspension, hydrating at 45°C for 60 minutes, ultrasonically treating at 0°C for 10 minutes after the treatment, centrifuging to remove the supernatant, filtering through a 0.6 μm filter membrane, and obtaining an antibacterial and mite-removing agent; wherein the mass ratio of eugenol / mesoporous nano-silica composite material, soybean lecithin, cholesterol, solvent and cholesterol-modified hyaluronic acid suspension is 1:14:7:180:900, and the solvent is prepared by mixing chloroform and methanol in a volume ratio of 3:1; the cholesterol-modified hyaluronic acid suspension comprises the following steps: the preparation of cholesterol-modified hyaluronic acid is the same as that in Example 1; the cholesterol-modified hyaluronic acid and PBS buffer solution are uniformly mixed in a mass ratio of 1:900 to obtain a cholesterol-modified hyaluronic acid suspension; Step (3), mixing the antibacterial and anti-mite agent, the anti-dandruff agent and water in a mass ratio of 30:1:70 to obtain an anti-mite and anti-dandruff composition; wherein the anti-dandruff agent is piroctone ethanolamine salt.

[0031] Comparative Example 2 The present comparative example discloses a method for preparing shampoo, comprising the following steps: uniformly mixing a cationic polymer and water, heating to 70°C, adding a surfactant and a thickener, stopping heating when the temperature continues to rise to 75°C, stirring at the temperature for 10 minutes, cooling to 40°C, adding an essence and the mite and dandruff removing composition prepared in comparative example 1, continuing stirring until the mixture is uniform, adding a regulator citric acid to adjust the pH value to 6.2, adjusting the viscosity of the system, discharging the material when the temperature drops to below 40°C, and obtaining the shampoo; wherein the weight percentage of each component in the shampoo is: 2% of the cationic polymer, 25% of the surfactant, 1.5% of the thickener, 0.3% of the essence, 10% of the mite and dandruff removing composition, and the balance being water; the cationic polymer is polyquaternium-10; the surfactant is prepared by mixing ammonium laureth sulfate, ammonium lauryl sulfate, and cocamidopropyl betaine in a mass ratio of 14:7:5; and the thickener is isostearamide MIPA.

[0032] Comparative Example 3 The comparative example discloses a preparation method of shampoo, comprising the following steps: uniformly mixing a cationic polymer and water, heating to 70°C, adding a surfactant and a thickener, stopping heating when the temperature continues to rise to 75°C, stirring at the temperature for 10 minutes, cooling to 40°C, adding an essence and a mite and dandruff removing composition, continuing stirring until the mixture is uniform, adding a regulator citric acid to adjust the pH value to 6.2, adjusting the viscosity of the system, discharging the material when the temperature drops to below 40°C, and obtaining the shampoo; wherein the weight percentage of each component in the shampoo is: 2% of the cationic polymer, 25% of the surfactant, 1.5% of the thickener, 0.3% of the essence, 10% of the mite and dandruff removing composition, and the balance is water; the mite and dandruff removing composition is prepared by mixing piroctone ethanolamine salt and water in a mass ratio of 1:100; the cationic polymer is polyquaternium-10; the surfactant is prepared by mixing ammonium laureth sulfate, ammonium lauryl sulfate, and cocamidopropyl betaine in a mass ratio of 14:7:5; and the thickener is isostearamide MIPA.

[0033] In the above examples and comparative examples: alkylated hydrophobically modified polyethyleneimine (PEI-C 12) is homemade and prepared by the following steps: dissolving 1g polyethyleneimine (Mw=1800) in 100ml of a dichloromethane / methanol mixed solvent, adding dropwise a dichloromethane / methanol solution of 1-bromododecane, the total amount of 1-bromododecane added is 0.3g, the dropping speed is 10ml / h, after the dropping is completed, reacting in a light-proof environment at 40°C for 24h, after the reaction is completed, removing the solvent by rotary evaporation to obtain a crude reaction product, mixing the crude reaction product with water, dialyzing it in a dialysis bag with a molecular weight cutoff of 1000 with a 40wt% ethanol aqueous solution for 5h, and then dialyzing it with water for 24h, after the treatment is completed, freeze-drying it at -40°C for 48h to obtain an alkylated hydrophobically modified polyethyleneimine; amino mesoporous nano-silica comes from Zhongke Keyou Nanotechnology Co., Ltd., product name amino mesoporous silica nanoparticles, specification 100nm, average pore size 1 0nm; mesoporous nano-silica comes from Zhongke Keyou Nanotechnology Co., Ltd., product name mesoporous silica nanoparticles, specification 100nm, average pore size 10nm; dopamine hydrochloride comes from Aladdin Biochemical Technology Co., Ltd., CAS number: 62-31-7; HEPES buffer solution comes from McLean Biochemical Technology Co., Ltd., specification 25mmol / L, pH=7.4; eugenol comes from McLean Biochemical Technology Co., Ltd., CAS number: 97-53-0; soybean lecithin comes from Aladdin Biochemical Technology Co., Ltd., product number S755201; cholesterol comes from McLean Biochemical Technology Co., Ltd., CAS number: 57-88-5; sodium hyaluronate comes from West Asia Chemical Co., Ltd., CAS number: 9067-32-7; PBS buffer solution comes from McLean Biochemical Technology Co., Ltd., specification 0.01mmol / L, pH=7.4.

[0034] Test example (1) Load performance test The loading amount of eugenol in the antibacterial and mite-removing agents prepared in Examples 1-3 and Comparative Example 1 was calculated. The testing method was as follows: take the polydopamine-modified mesoporous nano-silica prepared in Examples 1-3, respectively recorded as samples 1-3; take the mesoporous nano-silica in the comparative example, recorded as sample 4; take 20 mg of each of samples 1-4, place them in 10 mL of a 10 vol% eugenol ethanol solution, load them at 30°C, and when the adsorption reaches equilibrium, take part of the suspension, and use an ultraviolet spectrophotometer to detect the absorbance, calculate the loading capacity of samples 1-4 for eugenol and the utilization rate of eugenol, and the specific test results are shown in Table 1: wherein, the formula for the loading capacity is: sample loading amount (mg / mg) = (mass of eugenol loaded on the sample / mass of the sample); the formula for the utilization rate is: utilization rate of eugenol (%) = (mass of eugenol loaded on the sample / total input amount of eugenol) × 100%.

[0035]

[0036] It can be seen from the test results in Table 1 that in the anti-mite and anti-dandruff shampoo prepared by the present invention, the antibacterial and anti-mite agent has a high efficiency loading performance for eugenol.

[0037] Polydopamine has rich functional groups and aromatic ring structures, and can achieve efficient loading of the antibacterial active substance eugenol through hydrogen bonding and π-π stacking, thereby improving the loading amount and stability of eugenol; Sample 4 uses the mesoporous nano-silica in Comparative Example 1, and only uses mesoporous nano-silica as a carrier without surface modification of polydopamine, so the loading amount of eugenol is reduced, so the eugenol loading amount of Sample 4 prepared by Comparative Example 1 is not as good as that of Sample 1-3 prepared by Examples 1-3.

[0038] (2) Mite removal performance test The mite removal performance of the shampoos prepared in Examples 4-6 and Comparative Examples 2-3 was tested, and the specific test results are shown in Table 2:

[0039] The detection of the indicators in Table 2 is based on the following standards: the mite removal performance is represented by the mite killing time, and the test method is as follows: Demodex mites are placed in 3.5 cm culture dishes, with 6 mites placed in each culture dish, and 0.5 ml of shampoo prepared in Examples 4-6 and Comparative Examples 2-3 are added to the culture dishes respectively, which are recorded as samples 1-5, and samples 1-5 are placed in a constant temperature and humidity incubator at a temperature of 25°C and a humidity of 70%, and observed under a microscope until all the mites are dead, and the time to kill all the mites is calculated; wherein, the standard for determining death is: under a microscope, the insect body feet remain motionless, there is no recovery phenomenon after slight heating, or the insect body surface shrinks, changes color, deforms, and the contents leak out, etc., which can be determined as death.

[0040] It can be seen from the test results in Table 2 that the mite and dandruff removing shampoo prepared by the present invention has excellent mite removing effect.

[0041] Eugenol has antibacterial and anti-inflammatory biological activities, has excellent killing effects on mites and Malassezia, and can be used in combination with traditional anti-dandruff agents to improve the bactericidal and anti-dandruff effects. When the present invention uses the prepared polydopamine-modified mesoporous nano-silica as a carrier to load eugenol, since polydopamine has rich functional groups and aromatic ring structures, it can achieve efficient loading of the antibacterial active substance eugenol through hydrogen bonding and π-π stacking, thereby improving the loading amount and stability of eugenol.

[0042] In sample 4 prepared from comparative example 2, the antibacterial and anti-mite agent in the anti-mite and anti-dandruff composition only uses mesoporous nano-silica as a carrier, without surface-modified polydopamine and alkylated hydrophobically modified polyethyleneimine, the loading amount of eugenol is reduced, and the mite removal effect is reduced, so the mite removal performance of sample 4 prepared from comparative example 2 is not as good as that of the embodiment; In sample 5 prepared from comparative example 3, no antibacterial and anti-mite agent is added. Although the anti-dandruff agent still has a certain mite-killing effect, due to the lack of the highly efficient mite-killing effect of eugenol, the mite-killing performance of sample 5 prepared from comparative example 3 is not as good as that of the embodiment.

[0043] (3) Anti-dandruff performance test The anti-dandruff performance of the shampoos prepared in Examples 4-6 and Comparative Examples 2-3 was tested, and the specific test results are shown in Table 3:

[0044] The detection of the indicators in Table 3 is based on the following standards: the antidandruff performance is represented by the antibacterial rate of Malassezia, the species is Malassezia furfur, and reference QB / T 2738-2012 "Evaluation method for antibacterial and antibacterial effects of daily chemical products" is selected, and the suspension quantitative method is used to calculate the antibacterial rate of Examples 4-6 and Comparative Examples 2-3 against Malassezia.

[0045] It can be seen from the test results in Table 3 that the anti-mite and anti-dandruff shampoo prepared by the present invention has excellent anti-Malassezia effect and has an anti-dandruff effect.

[0046] Comparative Example 2 uses the mite and dandruff removal composition prepared in Comparative Example 1, in which the antibacterial and mite removal agent only uses mesoporous nano-silica as a carrier, and is not surface-modified with polydopamine and alkylated hydrophobically modified polyethyleneimine. The loading amount of eugenol is reduced, and the antibacterial rate against Malassezia is reduced. Therefore, the antidandruff performance and anti-Malassezia performance of Comparative Example 2 are not as good as those of the embodiment; the mite and dandruff removal composition used in Comparative Example 3 does not contain an antibacterial and mite removal agent. Although the antidandruff agent has an inhibitory effect on Malassezia, due to the lack of the addition effect of eugenol, the antidandruff performance and anti-Malassezia performance of Comparative Example 3 are not as good as those of the embodiment.

[0047] (4) Stability performance test The stability of the shampoos prepared in Examples 4-6 and Comparative Examples 2-3 was tested. The testing method was as follows: the shampoos prepared in Examples 4-6 and Comparative Examples 2-3 were placed in a constant temperature incubator at 0°C, room temperature, and 40°C for 1 month to observe whether the shampoos were stratified. The specific test results are shown in Table 4:

[0048] It can be seen from the test results in Table 4 that the anti-mite and anti-dandruff shampoo prepared by the present invention has good stability in various temperature environments.

[0049] In the antibacterial and mite-removing agent of the present invention, the loading amount and stability of eugenol are improved when mesoporous nano-silica and polydopamine are used to load eugenol, and further surface modification of liposomes further improves the dispersibility of the material in water, so the shampoos prepared in Examples 4-6 and Comparative Examples 2-3 have good stability.

[0050] 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. A method for preparing a mite and dandruff removing shampoo, characterized in that: The following steps are involved: Step (1), mixing eugenol / functionalized mesoporous nano-silica composite material, soybean lecithin, cholesterol, and solvent A, ultrasonically dispersing, rotary evaporating, adding cholesterol-modified hyaluronic acid suspension, hydrating, ultrasonically treating, centrifuging, filtering membrane, and obtaining an antibacterial and anti-mite agent; uniformly mixing the antibacterial and anti-mite agent, anti-dandruff agent, and water to obtain an anti-mite and anti-dandruff composition; Step (2), mixing the cationic polymer and water evenly and then heating, adding a surfactant and a thickener, stirring while keeping the temperature high, cooling, adding essence and the mite and dandruff removing composition, continuing to stir evenly, adjusting the pH value and viscosity, cooling and discharging the material, and obtaining the mite and dandruff removing shampoo.

2. The method for preparing a mite and dandruff removing shampoo according to claim 1, characterized in that: The eugenol / functionalized mesoporous nano-silica composite material in step (1) is prepared by the following steps: S11, mixing amino mesoporous nano-silica, dopamine hydrochloride and solvent B, ultrasonically dispersing, adding ammonium persulfate, reacting, centrifuging and washing after the reaction, to obtain polydopamine-modified mesoporous nano-silica; S12, mixing polydopamine-modified mesoporous nano-silica, eugenol, and ethanol, loading, centrifuging, and washing after loading to obtain an intermediate product; S13, mixing the intermediate product, alkylated hydrophobically modified polyethyleneimine, water and ethanol, reacting, and after the reaction, centrifuging, filtering and washing to obtain a eugenol / functionalized mesoporous nano-silica composite material.

3. The method for preparing a mite and dandruff removing shampoo according to claim 2, characterized in that: When preparing the eugenol / functionalized mesoporous nano-silica composite material: In S11, the mass ratio of amino mesoporous nano-silica, dopamine hydrochloride, solvent B, and ammonium persulfate is 1: 0.2-0.22: 480-550: 0.24-0.26; the reaction conditions are: stirring the reaction at a speed of 80-100 r / min and a temperature of 25-30°C for 8-12 hours; In S12: the mass ratio of polydopamine-modified mesoporous nano-silica, eugenol, and ethanol is 0.1:10-12:80-100; the loading conditions are: stirring the loading at room temperature for 12-20 hours; In S13: the mass ratio of the intermediate product, alkylated hydrophobically modified polyethyleneimine, water and ethanol is 1:1-1.2:40-60:40-60; the reaction conditions are: stirring the reaction at a speed of 80-100 r / min and a temperature of 25-30°C for 20-26 hours.

4. The method for preparing a mite and dandruff removing shampoo according to claim 1, characterized in that: The cholesterol-modified hyaluronic acid suspension in step (1) is prepared by the following steps: mixing and dissolving cholesterol, N,N'-dicyclohexylcarbodiimide, 4-dimethylaminopyridine and N,N-dimethylformamide to obtain a cholesterol mixed solution; mixing sodium hyaluronate, water and Tween 80 evenly, adding the cholesterol mixed solution dropwise, reacting after the addition is complete, and purifying after the reaction is complete to obtain cholesterol-modified hyaluronic acid; mixing the cholesterol-modified hyaluronic acid and PBS buffer solution evenly to obtain a cholesterol-modified hyaluronic acid suspension.

5. The method for preparing the anti-mite and anti-dandruff shampoo according to claim 4, characterized in that: When preparing the cholesterol-modified hyaluronic acid suspension: the mass ratio of cholesterol, N,N'-dicyclohexylcarbodiimide, 4-dimethylaminopyridine, and N,N-dimethylformamide is 3.8-4:4.9-5:0.24-0.25:190-210; the mass ratio of sodium hyaluronate, water, and Tween 80 is 0.4-0.5:100-120:5; the mass ratio of cholesterol to sodium hyaluronate is 0.95-1:1; the reaction conditions are: reacting at a temperature of 20-25°C for 40-48h; the mass ratio of cholesterol-modified hyaluronic acid to PBS buffer solution is 1:900-1000.

6. The method for preparing the anti-mite and anti-dandruff shampoo according to claim 1, characterized in that: In the step (1), the mass ratio of eugenol / functionalized mesoporous nano-silica composite material, soybean lecithin, cholesterol, solvent A, and cholesterol-modified hyaluronic acid suspension is 1:14-15:6-7:180-200:900-1000, and solvent A is prepared by mixing chloroform and methanol in a volume ratio of 3:1-2.

7. The method for preparing the anti-mite and anti-dandruff shampoo according to claim 1, characterized in that: In the step (1), the rotary evaporation conditions are: rotary evaporation at 40-50°C for 25-30 min; the hydration treatment conditions are: hydration treatment at 45-55°C for 30-60 min; the ultrasonic treatment conditions are: ultrasonic treatment at 0°C for 8-10 min; and the filter membrane is a 0.6-0.8 μm filter membrane.

8. The method for preparing the anti-mite and anti-dandruff shampoo according to claim 1, characterized in that: In the step (1), the mass ratio of the antibacterial and decarcinogenic agent, the antidandruff agent and water is 30-40:1-1.5:70; the antidandruff agent is selected from one of piroctone ethanolamine and climbazole.

9. The method for preparing an anti-mite and anti-dandruff shampoo according to claim 1, characterized in that: In the step (2), the weight percentages of the components in the mite and dandruff removing shampoo are: 2-3% cationic polymer, 25-27% surfactant, 1-1.5% thickener, 0.3-0.5% flavor, 10-15% mite and dandruff removing composition, and the balance is water; the cationic polymer is selected from one or two of polyquaternium-10 and guar hydroxypropyltrimethylammonium chloride; the surfactant is selected from two or more of ammonium laureth sulfate, ammonium lauryl sulfate, and cocamidopropyl betaine; and the thickener is selected from isostearamide MIPA.

10. An anti-dandruff and mite shampoo prepared by the method for preparing an anti-dandruff and mite shampoo according to any one of claims 1 to 9.

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