An oil-controlling and acne-removing nanocomposition, its preparation method and application

Abstract

This invention belongs to the field of cosmetic technology, specifically relating to an oil-controlling and acne-removing nanocomposition, its preparation method, and its application. The oil-controlling and acne-removing nanocomposition provided by this invention comprises magnolol, azelaic acid, kaempferol, an anti-allergen, an active ingredient for fading acne scars, an emulsifier, a co-emulsifier, lipids, and water. The active ingredients are magnolol, azelaic acid, kaempferol, the anti-allergen, and the active ingredient for fading acne scars. The optimal oil-controlling and acne-removing effect is achieved when the mass ratio of magnolol, azelaic acid, and kaempferol is (7.6–8.4):(4.7–5.3):(0.9–1.1).

Description

TECHNICAL FIELD

[0001] The present application belongs to the technical field of cosmetics, and particularly relates to an oil-control and acne-removing nano composition, a preparation method and application thereof. BACKGROUND

[0002] Acne vulgaris, commonly known as acne, is a chronic inflammatory disease of the pilosebaceous unit. Since it often occurs in adolescents, it is also commonly known as "adolescent acne". With the development of society, affected by factors such as life and work pressure and environmental pollution, the incidence of acne is on the rise, and the age of onset is also widening.

[0003] The causes of acne formation include: (1) excessive sebum secretion, rapid rise in the level of male hormones, especially testosterone, which promotes the development of sebaceous glands and produces a large amount of sebum; (2) abnormal keratinization, excessive keratinization of the pilosebaceous duct, narrowing or obstruction of the duct orifice, and difficulty in sebum excretion, resulting in comedones; (3) pathogenic bacteria proliferation, large amounts of Propionibacterium acnes and Staphylococcus aureus proliferate, and skin acne breaks out; (4) inflammatory reaction, comedones break, pilosebaceous glands are damaged, and then pus forms.

[0004] Acne seriously affects people's appearance and has an important impact on normal people's employment, social interaction, and marriage and childbirth. At present, there are various acne-removing products, but their quality is uneven, and there are generally problems such as insignificant effect, slow efficacy, and high irritation. SUMMARY

[0005] The present application provides an oil-control and acne-removing nano composition with excellent oil-control and acne-removing effect, and a preparation method and application thereof.

[0006] In order to achieve the above-mentioned purpose of the application, the present application provides the following technical solutions:

[0007] The present application provides an oil-control and acne-removing nano composition, which comprises magnolol, azelaic acid, kaempferol, an anti-allergic agent, a pimple mark lightening active substance, an emulsifier, a co-emulsifier, a lipid, and water;

[0008] calculated based on 100% of the total mass,

[0009] The mass percentage of magnolol in the oil-control and acne-removing nano composition is 1% to 10%;

[0010] The mass percentage of the anti-allergic agent in the oil-control and acne-removing nano composition is 0.1% to 5%;

[0011] The mass percentage of the pimple mark lightening active substance in the oil-control and acne-removing nano composition is 0.1% to 10%;

[0012] The mass percentage of the emulsifier in the oil-control and acne-removing nano composition is 5% to 40%;

[0013] The mass percentage of the co-emulsifier in the oil-controlling and acne-removing nano composition is 5-40%;

[0014] The mass percentage of the lipid in the oil-controlling and acne-removing nano composition is 5-30%;

[0015] The mass ratio of magnolol, azelaic acid and kaempferol in the oil-controlling and acne-removing nano composition is (7.6-8.4):(4.7-5.3):(0.9-1.1), with water as the balance.

[0016] Preferably, the anti-sensitivity agent includes one or more of glycyrrhetinic acid, glycyrrhizic acid salt, bisabolol and beta-glucan.

[0017] Preferably, the acne mark lightening active ingredient includes one or more of nicotinamide, heparin sodium, carnosine and decarboxy carnosine.

[0018] Preferably, the mass ratio of magnolol, azelaic acid and kaempferol is 8:5:1.

[0019] Preferably, the emulsifier includes one or more of polyoxyethylene sorbitan fatty acid ester, polyglyceryl fatty acid ester, polyoxyethylene fatty acid ester, PEG-8 caprylic / capric glycerides, polyoxyethylene hydrogenated castor oil, fatty alcohol polyoxyethylene ether, coco-glucoside, lecithin, PEG-30 dipolyhydroxystearate and ceteareth.

[0020] The co-emulsifier includes one or more of glycerol, diethylene glycol monoethyl ether, polyethylene glycol-400, 1,3-butanediol, 1,2-propanediol, dipropylene glycol, 1,2-hexanediol, 1,2-pentanediol, ethoxydiglycol, ethoxydiglycol oleate and octyldodecanol.

[0021] The lipid includes one or more of isopropyl myristate, isopropyl palmitate, caprylic / capric triglyceride, caprylic / capric polyethylene glycol glyceride, polyethylene glycol laurate glyceride, polyethylene glycol stearate glyceride, linoleic acid glyceride, propylene glycol monocaprylate, propylene glycol dicaprylocaprate, glyceryl stearate, acetylated monoglyceride, caprylocaproyl macadamia nut oil, cetyl alcohol, stearyl alcohol and cetearyl alcohol.

[0022] The present application also provides a preparation method of the oil-controlling and acne-removing nano composition.

[0023] Mixing magnolol, azelaic acid, kaempferol, an anti-sensitivity agent, an emulsifier, a co-emulsifier and a lipid to obtain an oil phase;

[0024] Mixing an acne mark lightening active ingredient and water to obtain an aqueous phase;

[0025] adding the water phase into the oil phase, and after mixing, micronization treatment is performed to obtain a micron-level dispersion;

[0026] The micron-level dispersion is subjected to nanometerization treatment to obtain the oil-control and acne-removing nanometer composition.

[0027] Preferably, the micronization treatment is achieved by high-speed shearing emulsification.

[0028] The high-speed shearing emulsification is performed at a speed of 5000-10000 rpm for 1-10 min.

[0029] Preferably, the nanometerization treatment is achieved by high-pressure homogenization treatment or high-speed microjet treatment.

[0030] The high-pressure homogenization treatment is performed at a pressure of 300-1200 bar for 2-10 times.

[0031] The high-pressure microjet treatment is performed at a pressure of 200-2000 bar for 2-10 times.

[0032] The application further provides application of the oil-control and acne-removing nanometer composition in the preparation of cosmetics.

[0033] Beneficial effects:

[0034] The application provides an oil-control and acne-removing nanometer composition, which comprises magnolol, azelaic acid, kaempferol, an anti-allergic agent, a pimple mark lightening active substance, an emulsifier, a co-emulsifier, a lipid and water. DETAILED DESCRIPTION

[0035] The oil-control and acne-removing nanometer composition comprises magnolol, azelaic acid, kaempferol, an anti-allergic agent, a pimple mark lightening active substance, an emulsifier, a co-emulsifier, a lipid and water.

[0036] The mass percentage content of magnolol in the oil-controlling and acne-removing nano composition is 1-10%;

[0037] The mass percentage content of anti-allergic agent in the oil-controlling and acne-removing nano composition is 0.1-5%;

[0038] The mass percentage content of acne mark lightening active substance in the oil-controlling and acne-removing nano composition is 0.1-10%;

[0039] The mass percentage content of emulsifier in the oil-controlling and acne-removing nano composition is 5-40%;

[0040] The mass percentage content of co-emulsifier in the oil-controlling and acne-removing nano composition is 5-40%;

[0041] The mass percentage content of lipid in the oil-controlling and acne-removing nano composition is 5-30%;

[0042] The mass ratio of magnolol, azelaic acid and kaempferol in the oil-controlling and acne-removing nano composition is (7.6-8.4):(4.7-5.3):(0.9-1.1).

[0043] In the present application, the mass percentage content of magnolol in the oil-controlling and acne-removing nano composition is 1-10%, preferably 2-8%, further preferably 3-6%, more preferably 3.8-5%, and most preferably 4%. The magnolol has the effects of anti-inflammation and anti-oxidation, and can effectively inhibit the overgrowth of pathogenic bacteria such as Propionibacterium acnes.

[0044] In the present application, the oil-controlling and acne-removing nano composition comprises azelaic acid. The mass ratio of magnolol to azelaic acid is (7.6-8.4):(4.7-5.3), preferably 8:5. The azelaic acid can effectively improve the skin keratinization, dredge pores, competitively inhibit the activity of 5α-reductase, inhibit the secretion of oil, and has a broad-spectrum bacteriostatic effect.

[0045] In the present application, the oil-controlling and acne-removing nano composition comprises kaempferol. The mass ratio of magnolol to kaempferol is (7.6-8.4):(0.9-1.1), preferably 8:1. The kaempferol can competitively inhibit 5α-reductase, regulate androgen secretion, and prevent the clogging and dilation of pores caused by excessive sebum production.

[0046] In the present application, the mass ratio of magnolol, azelaic acid and kaempferol in the oil-controlling and acne-removing nano composition is (7.6-8.4):(4.7-5.3):(0.9-1.1), preferably 8:5:1 or 8.4:5.3:1.1 or 7.6:4.7:0.9. The present application limits the mass ratio of magnolol, azelaic acid and kaempferol, and the oil-controlling and acne-removing effects are significantly better than other ratios.

[0047] In the present application, the mass percentage of the acne mark lightening active ingredient in the oil-controlling acne-removing nano composition is 0.1% to 10%, preferably 0.5% to 8%, further preferably 1% to 7%, more preferably 2% to 6%, and most preferably 3% to 5%. The acne mark lightening active ingredient in the present application preferably comprises one or more of niacinamide, heparin sodium, carnosine, and decarboxy carnosine, and further preferably niacinamide. The acne mark lightening active ingredient in the present application can promote skin metabolism, remove excess keratin, inhibit melanin transfer, lighten acne marks, and even skin tone.

[0048] In the present application, the mass percentage of the anti-allergic agent in the oil-controlling acne-removing nano composition is 0.1% to 5%, preferably 0.2% to 4%, further preferably 0.5% to 3%, more preferably 1% to 2%, and most preferably 1.5%. The anti-allergic agent in the present application preferably comprises one or more of glycyrrhetinic acid, glycyrrhizic acid salt, bisabolol, and beta-glucan, and further preferably glycyrrhetinic acid. The anti-allergic agent in the present application can inhibit the production of inflammatory factors, reduce skin inflammation, and improve skin immunity.

[0049] In the present application, the mass percentage of the emulsifier in the oil-controlling acne-removing nano composition is preferably 5% to 40%, further preferably 8% to 20% or 25% to 35%, and more preferably 10% to 16% or 30%. The emulsifier in the present application preferably comprises one or more of polyoxyethylene sorbitan fatty acid ester, polyglyceryl fatty acid ester, polyoxyethylene fatty acid ester, PEG-8 caprylic / capric glycerides, polyoxyethylene hydrogenated castor oil, fatty alcohol polyoxyethylene ether, cocoglucopolsaccharide, lecithin, PEG-30 dipolyhydroxystearate, and ceteareth, further preferably a mixture of polyoxyethylene sorbitan fatty acid ester, polyglyceryl fatty acid ester, and lecithin, or a mixture of polyoxyethylene hydrogenated castor oil and caprylic / capric glycerides, or a mixture of fatty alcohol polyoxyethylene ether and cocoglucopolsaccharide. In the mixture of polyoxyethylene sorbitan fatty acid ester, polyglyceryl fatty acid ester, and lecithin, the mass ratio of polyoxyethylene sorbitan fatty acid ester, polyglyceryl fatty acid ester, and lecithin is preferably 5:10:1; in the mixture of polyoxyethylene hydrogenated castor oil and caprylic / capric glycerides, the mass ratio of polyoxyethylene hydrogenated castor oil and caprylic / capric glycerides is preferably 1:1; and in the mixture of fatty alcohol polyoxyethylene ether and cocoglucopolsaccharide, the mass ratio of fatty alcohol polyoxyethylene ether and cocoglucopolsaccharide is 1:1.

[0050] In the present application, the mass percentage content of the co-emulsifier in the oil-controlling and acne-removing nano composition is preferably 5% to 40%, further preferably 8% to 20% or 25% to 35%, and more preferably 15% or 30%. The co-emulsifier in the present application preferably includes one or more of glycerin, diethylene glycol monoethyl ether, polyethylene glycol-400, 1,3-butanediol, 1,2-propanediol, dipropylene glycol, 1,2-hexanediol, 1,2-pentanediol, ethoxydiglycol, ethoxydiglycol oleate, and octyldodecanol, further preferably a mixture of dipropylene glycol and 1,2-hexanediol, or a mixture of 1,3-butanediol and 1,2-propanediol, or a mixture of 1,2-pentanediol and 1,2-hexanediol. In the mixture of dipropylene glycol and 1,2-hexanediol, the mass ratio of dipropylene glycol to 1,2-hexanediol is preferably 1:1; in the mixture of 1,3-butanediol and 1,2-propanediol, the mass ratio of 1,3-butanediol to 1,2-propanediol is preferably 1:1; and in the mixture of 1,2-pentanediol and 1,2-hexanediol, the mass ratio of 1,2-pentanediol to 1,2-hexanediol is preferably 1:2.

[0051] In the present application, the mass percentage content of the lipid in the oil-controlling and acne-removing nano composition is preferably 5% to 30%, further preferably 2% to 10% or 13% to 25%, and more preferably 5% to 8% or 15% to 20%. The lipid in the present application preferably includes one or more of isopropyl myristate, isopropyl palmitate, caprylic / capric triglyceride, caprylic / capric polyethylene glycol glyceride, polyethylene glycol laurate glyceride, polyethylene glycol stearate glyceride, linoleic acid glyceride, propylene glycol monocaprylate, propylene glycol dicaprylocaprate, glycerol stearate, acetylated monoglyceride, cocoa caprylocaprate, cetyl alcohol, stearyl alcohol, and cetylstearyl alcohol, further preferably caprylic / capric triglyceride, or a mixture of isopropyl myristate, propylene glycol monocaprylate, and propylene glycol dicaprylocaprate, or a mixture of isopropyl palmitate and glycerol stearate. In the mixture of isopropyl myristate, propylene glycol monocaprylate, and propylene glycol dicaprylocaprate, the mass ratio of isopropyl myristate, propylene glycol monocaprylate, and propylene glycol dicaprylocaprate is preferably 5:5:3. In the mixture of isopropyl palmitate and glycerol stearate, the mass ratio of isopropyl palmitate to glycerol stearate is preferably 1:1.

[0052] In the present application, the oil-controlling and acne-removing nano composition includes water, and the balance, in addition to the above-mentioned ingredients, is water, with the total mass percentage content of the oil-controlling and acne-removing nano composition being 100%.

[0053] The present application preferably provides a preparation method of the oil-controlling and acne-removing nano composition described in the above technical solution, including the following steps:

[0054] mixing magnolol, azelaic acid, kaempferol, an anti-allergic agent, an emulsifier, a co-emulsifier and a lipid to obtain an oil phase;

[0055] mixing a pimple mark lightening active and water to obtain an aqueous phase;

[0056] micronizing the mixture of the aqueous phase and the oil phase to obtain a micron-sized dispersion;

[0057] nanoizing the micron-sized dispersion to obtain an oil control and acne-removing nano composition.

[0058] The present application mixes magnolol, azelaic acid, kaempferol, an anti-allergic agent, an emulsifier, a co-emulsifier and a lipid to obtain an oil phase. In the present application, the temperature of the mixing is preferably 40-70℃, further preferably 50-60℃, and more preferably 55℃. The mixing in the present application is preferably carried out under a water bath so that the components are uniformly dispersed. The present application does not strictly require the time of the mixing, and the mixing can be stopped when the solution is transparent.

[0059] The present application mixes a pimple mark lightening active and water to obtain an aqueous phase. In the present application, the temperature of the mixing is preferably 40-70℃, further preferably 50-60℃, and more preferably 55℃. The mixing in the present application is preferably carried out under a water bath so that the components are uniformly dispersed. The present application does not strictly require the time of the mixing, and the mixing can be stopped when the solution is transparent.

[0060] After obtaining the oil phase and the aqueous phase, the present application mixes the aqueous phase into the oil phase to obtain a premix. The present application preferably stirs the aqueous phase into the oil phase. The stirring speed in the present application is preferably 300-600rpm, further preferably 400-500rpm; and the stirring time is preferably 10-40min, further preferably 20-30min, and more preferably 25min.

[0061] After obtaining the premix, the present application micronizes the premix to obtain a micron-sized dispersion. In the present application, the micronization is preferably achieved by high-speed shearing emulsification; the high-speed shearing emulsification speed is preferably 5000-10000rpm, further preferably 6000-8000rpm, and more preferably 7000rpm; and the high-speed shearing emulsification time is preferably 1-10min, further preferably 3-8min, and more preferably 5-7min.

[0062] After obtaining the micron-sized dispersion, the micron-sized dispersion is subjected to a nanonization treatment to obtain the oil-control and acne-removing nano composition. In the present application, the nanonization treatment is preferably achieved by high-pressure homogenization treatment or high-speed microjet treatment, and is further preferably achieved by high-pressure homogenization treatment. The pressure of the high-pressure homogenization treatment is preferably 300-1200 bar, further preferably 400-1000 bar, more preferably 500-8000 bar, and most preferably 600 bar. The number of times of the high-pressure homogenization treatment is preferably 2-10 times, further preferably 3-8 times, and more preferably 5 times. The pressure of the high-pressure microjet treatment is preferably 200-2000 bar, further preferably 300-1000 bar, more preferably 500-800 bar, and most preferably 600 bar. The number of times of the high-pressure microjet treatment is preferably 2-10 times, further preferably 3-8 times, and more preferably 5 times.

[0063] The oil-control and acne-removing nano composition of the present application has good oil-control and acne-removing effects, and can be used to prepare a cosmetic. The use of the oil-control and acne-removing nano composition in the preparation of a cosmetic also belongs to the protection scope of the present application.

[0064] In order to further illustrate the present application, a kind of oil-control and acne-removing nano composition provided by the present application and its preparation method and application are described in detail below in conjunction with examples, but they should not be understood as limiting the protection scope of the present application.

[0065] Example 1

[0066] An oil-control and acne-removing nano composition is prepared by the following method:

[0067] (1) 4% magnolol, 2.5% azelaic acid, 0.5% kaempferol, 1.5% glycyrrhetinic acid, 5% polyoxyethylene sorbitan fatty acid ester (polysorbate-80), 10% polyglyceryl fatty acid ester (polyglyceryl 10-laurate), 1% lecithin, 10% 1,2-pentanediol, 20% 1,2-hexanediol, and 5% caprylic acid / capric acid triglyceride are stirred and dissolved to a transparent solution under the condition of a 40-70℃ water bath to obtain an oil phase, which is ready for use;

[0068] (2) 6% nicotinamide is mixed with the rest of the water, and the mixture is stirred and dissolved to a transparent solution under the condition of a 40-70℃ water bath to obtain an aqueous phase, which is ready for use;

[0069] (3) The aqueous phase is added to the oil phase, which is stirred at a stirring speed of 300-600 rpm under the condition of a 40-70℃ water bath for 10-40 min, and then high-speed shearing emulsification is performed at 6000 rpm for 7 min to obtain a micron-sized dispersion.

[0070] (4) The micron-sized dispersion is subjected to high-pressure homogenization treatment under a pressure of 300 bar, and is circulated 10 times to obtain the oil-controlling and acne-removing nano composition.

[0071] The amount of each raw material is a mass percentage content.

[0072] Example 2

[0073] An oil-controlling and acne-removing nano composition is prepared by the following method:

[0074] (1) 4.2% magnolol, 2.65% azelaic acid, 0.55% kaempferol, 2% bisabalol, 10% polyoxyethylene hydrogenated castor oil, 10% PEG-8 caprylic / capric glycerides, 15% 1,3-butanediol, 15% 1,2-propanediol, 5% isopropyl myristate, 5% propylene glycol monocaprylate, and 3% dicaprylyl carbonate are stirred and dissolved into a transparent solution under the condition of a 40-70°C water bath to obtain an oil phase, which is ready for use;

[0075] (2) 7% sodium heparin and the rest of water are mixed and stirred and dissolved into a transparent solution under the condition of a 40-70°C water bath to obtain an aqueous phase, which is ready for use;

[0076] (3) The aqueous phase is added to the oil phase, which is stirred at a speed of 300-600 rpm for 10-40 min under the condition of a 40-70°C water bath, and is then subjected to high-speed shearing emulsification at 6000 rpm for 7 min to obtain a micron-sized dispersion.

[0077] (4) The micron-sized dispersion is subjected to high-pressure homogenization treatment under a pressure of 300 bar, and is circulated 10 times to obtain the oil-controlling and acne-removing nano composition.

[0078] The amount of each raw material is a mass percentage content.

[0079] Example 3

[0080] An oil-controlling and acne-removing nano composition is prepared by the following method:

[0081] (1) 3.8% magnolol, 2.35% azelaic acid, 0.45% kaempferol, 1% beta-glucan, 10% fatty alcohol polyoxyethylene ether, 10% cocoglycosyl polysaccharide, 10% dipropylene glycol, 10% 1,2-hexanediol, 5% isopropyl palmitate, and 5% glyceryl stearate are stirred and dissolved into a transparent solution under the condition of a 40-70°C water bath to obtain an oil phase, which is ready for use;

[0082] (2) 5% carnosine and the rest of water are mixed and stirred and dissolved into a transparent solution under the condition of a 40-70°C water bath to obtain an aqueous phase, which is ready for use;

[0083] (3) Add the water phase to the oil phase, stir at 40-70℃ water bath condition, at a stirring speed of 300-600 rpm for 10-40 min, then emulsify at high speed under the condition of 6000 rpm for 7 min, to prepare a micron-level dispersion.

[0084] (4) Homogenize the micron-level dispersion under the condition of 300 bar pressure, for 10 cycles, to obtain the oil-controlling acne-removing nano composition.

[0085] The amount of each raw material above is mass percentage content.

[0086] Comparative Examples 1-11

[0087] Comparative Examples 1-11 are the same as Example 1, except that the proportions of magnolol, azelaic acid and kaempferol are different when preparing the oil-controlling acne-removing nano composition, and the specific differences are listed in Table 1.

[0088] Table 1 Concentration of active ingredients (mass percentage content %) in Example 1 and Comparative Examples 1-11

[0089]

[0090]

[0091] Comparative Example 12

[0092] Prepare the oil-controlling acne-removing nano composition according to Example 5 in the prior art CN108785122A, wherein the mass percentage contents of magnolol, azelaic acid, kaempferol, glycyrrhetinic acid and decarboxy myo-inositol are 4%, 2%, 2%, 6% and 9%, respectively.

[0093] Test Example 1

[0094] Use a laser particle size analyzer to detect the particle size of the oil-controlling acne-removing nano composition obtained in the above examples and comparative examples, and the particle size is within 200 nm. The oil-controlling acne-removing nano composition is placed in a sealed container at room temperature for 60 days, and no agglomeration, discoloration or layering phenomenon occurs, and the particle size does not change significantly, indicating good stability.

[0095] Test Example 2

[0096] Effect on the release amount of inflammatory factors

[0097] Raw 264.7 cells cultured to the exponential growth phase with DMEM medium containing 10% FBS and 1% PS were diluted to 1×10 5The cells were inoculated in 24-well plates at 1 x 105cells / mL, 0.5 mL per well, and incubated for 24 h. Then, except for the control group, the cells in the other groups were treated with 2 μg / mL LPS to prepare an inflammation model. The sample test groups were treated with 0.5 mL of the nano-composition prepared in Example 1 or Comparative Examples 1-12 diluted 2000 times (with culture medium) and incubated at 37°C for another 24 h. The culture supernatant was collected and the expression of IL-6 and TNF-α was detected according to the instructions of the ELISA kit. The results are shown in Table 3.

[0098] Table 3 Effect on the release of inflammatory factors (n = 3)

[0099]

[0100]

[0101] Note: compared with the blank control group, ## p < 0.01; compared with the model group, ** p < 0.01; compared with Example 1, && p < 0.01.

[0102] As shown in Table 2, compared with the blank control group, the secretion of IL-6 and TNF-α in the model group was significantly increased after the addition of LPS (p < 0.01), indicating that the model was successfully constructed. Compared with the model group, the nano-composition prepared in Comparative Examples and Example 1 could significantly reduce the secretion of IL-6 and TNF-α (p < 0.01). Among them, the nano-composition prepared in Example 1 had the most significant effect on inhibiting the secretion of IL-6 and TNF-α by Raw264.7 cells, indicating that the ratio of magnolol, azelaic acid and kaempferol was 8:5:1, and the effect of inhibiting the expression of inflammatory factors was the best.

[0103] Test Example 3

[0104] Bacteriostatic experiment

[0105] The oil-controlling and acne-removing nano-composition obtained in Example 1 and Comparative Examples 1-12 was used as the test sample.

[0106] A few P. acnes (ATCC 6919) and S. aureus on the surface of the activated culture medium were taken with a swab, added with sterile normal saline, and dispersed in sterile normal saline by blowing with a sterile pipette. The concentration of the bacteria was adjusted to be similar to that of 0.5 McFarland turbidity tube (1.5 x 108CFU / mL). After fixing, a round filter paper sheet (d = 6 mm) was attached to the surface of the culture medium, and 5 μL of the sample to be tested was vertically added to the filter paper sheet. The flat plate with the attached drug sensitivity paper sheet was placed in a 37°C incubator, and incubated overnight. After taking out the flat plate, the diameter of the bacteriostatic ring was measured with a vernier caliper, the edge of the bacteriostatic ring was not visible to the naked eye, and the result was recorded. Table 3 shows the size of the bacteriostatic ring (n = 3).

[0107] Table 3 Size of the bacteriostatic ring in the paper sheet diffusion method (n = 3)

[0108]

[0109]

[0110] Note: compared with the blank control group, ** p < 0.01; compared with Example 1, # p < 0.05, ## p < 0.01.

[0111] According to Table 3, compared with the blank control group, the average diameter of the P. acnes and S. aureus bacteriostatic ring in the experimental group increased, and the bacteriostatic effect was obvious. Compared with the comparative example, after adding the same volume of the nano composition prepared in Example 1, the average diameter of the P. acnes and S. aureus bacteriostatic ring increased more significantly, which was 14.33 mm and 15.14 mm, respectively. It was shown that the effect of Example 1 on inhibiting P. acnes and S. aureus was better than that of the comparative example, and the nano composition prepared in Example 1 had better bacteriostatic efficacy when the ratio of magnolol, azelaic acid, and kaempferol in the nano composition was 8:5:1.

[0112] Test Example 4

[0113] Effect on 5α-reductase activity

[0114] The reaction system for establishing the 5α-reductase activity inhibition experiment was established. The reaction system 1 mL mixture contained 350 μL Tris-HCL buffer (pH 5.5), 25 μL of the nano-composition prepared in Comparative Examples 1-12 or Example 1 (the sample groups were all diluted 100 times, dissolved with 75% ethanol, and the blank control group was added with 25 μL of 75% ethanol), 100 μL of reduced coenzyme II tetrasodium salt solution (200 μg / mL), 25 μL of testosterone solution (25 μg / mL), 500 μL of 5α-reductase (1.2 mg / mL). After mixing, incubation was carried out at 37°C for 30 min, 2 mL of ethyl acetate was added to mix and terminate the reaction, 100 μL of internal standard solution was added, oscillation was carried out for 3 min, vortex was carried out for 30 s, and centrifugation (3000 r / min, 10 min) was carried out. The supernatant was taken, dried under nitrogen flow, dissolved with 1 mL of methanol, and then HPLC injection detection was carried out. The enzyme activity was determined according to the formula C 转化 = C 空白 -C 反应 (C 反应 is the measured testosterone concentration after the system reaction, C 空白 is the measured testosterone concentration after adding ethyl acetate to quench the enzyme activity before incubation) C 转化 value represents the 5α-reductase activity in the enzyme reaction system, and the higher the C 转化 value, the higher the enzyme activity. Testosterone conversion rate T (%) = C 转化 / C 空白 × 100%, and the inhibition rate I (%) of the drug on 5α-reductase = 1-T.

[0115] Table 4 5α-reductase activity inhibition results (n=3)

[0116]

[0117]

[0118] Note: compared with Example 1, * p<0.05, ** p<0.01.

[0119] As can be seen from Table 4, after adding the nano-composition prepared in Comparative Examples and Example 1 into the reaction system, the nano-composition prepared in Comparative Examples and Example 1 all showed obvious inhibition effect on 5α-reductase. The 5α-reductase inhibition rates of Comparative Example 2 and Comparative Example 3 and the nano-composition prepared in Example 1 were the strongest, reaching 87.42%, 86.46% and 87.36% respectively. The effect of Example 1 on inhibiting 5α-reductase activity was equivalent to that of Comparative Example 2 and Comparative Example 3, and was better than that of Comparative Example 1, Comparative Example 4-12, indicating that the nano-composition prepared in Example 1 had very good effect on inhibiting 5α-reductase activity when the ratio of magnolol, azelaic acid and kaempferol in the nano-composition was 8:5:1.

[0120] Test Example 5

[0121] Effects on sebum secretion

[0122] SZ95 cells (human sebaceous gland cells) cultured in DMEM medium containing 10% FBS and 1% PS to the exponential growth phase were used at 4 × 10⁻⁶ cells / year. 5 Cells were seeded at 2 mL / mL in 6-well plates and cultured for 24 h. Then, 2 mL of the nanocomposite prepared in Comparative Examples 1-12 or Example 1, diluted 2000 times (with culture medium), was added to the drug-treated group, and incubated at 37°C for another 24 h. The DMEM medium was discarded, and the cells were washed twice with PBS. The cells were then completely digested and transferred to 1.5 mL Eppendorf tubes. After centrifugation and discarding the supernatant, 1 mL of PBS was added, and the cells were gently washed by pipetting. Centrifugation was repeated, and the supernatant was discarded. Cells were gently pipetted using a pipette tip to prepare a single-cell suspension. 10 μL of Nile Red fluorescent dye was added to each tube to a final concentration of 100 ng / mL. The suspension was incubated at room temperature for 30 min, briefly vortexed, and filtered through a 300-mesh nylon filter into flow cytometry tubes. The average fluorescence intensity of the cells was detected using a flow cytometer. The results are shown in Table 5.

[0123] Table 5. Effects on lipid synthesis in SZ95 cells (n=3)

[0124]

[0125] Note: Compared with the blank control group, ** p<0.01; compared with Example 1, # p<0.05, ## p<0.01.

[0126] As shown in Table 5, compared with the blank control, the average fluorescence intensity of cells in the comparative examples and the nanocomposite prepared in Example 1 was significantly reduced, and the inhibition rate of cell lipid synthesis was significantly increased. Furthermore, compared with Comparative Examples 1 to 12, Example 1 showed a significantly reduced average fluorescence intensity and an inhibition rate of 57.1% for cell lipid synthesis. These experimental results indicate that the nanocomposite prepared in Example 1, with a ratio of magnolol, azelaic acid, and kaempferol of 8:5:1, exhibits a better effect in inhibiting cell lipid synthesis.

[0127] Application Example 1

[0128] 1. Preparation of blank serum

[0129] Dissolve 2.0% glycerol, 0.3% carbomer, 0.1% xanthan gum, 0.5% phenoxyethanol, and 97.2% purified water at room temperature by stirring to obtain a blank serum solution.

[0130] 2. Preparation of the test essence

[0131] The oil control acne nano composition obtained in Example 1 and Comparative Examples 1-12 was mixed with the blank essence in a mass ratio of 5:95, respectively, to obtain a test essence (the concentration of the oil control acne nano composition was 5%).

[0132] Test Example 6

[0133] Human oil control efficacy test experiment

[0134] A total of 140 volunteers were recruited, aged 20-55 years, healthy, no skin disease, non-pregnant or lactating, and no allergy to product ingredients. After being informed of the evaluation process, possible effects, risks, precautions, and signing the efficacy evaluation informed consent form, the efficacy evaluation test of different samples in Application Example 1 was performed, with 10 volunteers for each test sample. The volunteers used the test samples on the face twice a day at regular intervals, and no other products or drugs that could affect the skin condition were used during the test. The skin condition and feelings after use were recorded and fed back accurately. After using the test samples for two weeks, the volunteers' curative effect indexes were observed and compared. The German CK grease tester Sebumeter SM815 and Shanghai Fuhuan The facial oil content, facial acne mark diameter, and porphyrin content of the subjects were tested by the intelligent skin analysis system, and the results are shown in Table 6.

[0135] Table 6. Results of human oil control acne efficacy test (n=10)

[0136]

[0137] Note: Compared with the blank control group, ** p<0.01; compared with Example 1, # p<0.05, ## p<0.01.

[0138] As can be seen from Table 6, the blank serum of the blank group is used by the volunteers for two weeks, and the oil content value is reduced by 0.48%, the diameter of facial acne marks is reduced by 1.58%, and the content of facial porphyrin is reduced by 1.27%, and there is no obvious change in the above indexes, which shows that the blank serum has no improvement effect on skin oil control and acne removal. Compared with the blank group, the serum containing the oil control and acne removal nano composition of Comparative Examples 1-12 or Example 1 significantly reduces the skin oil, acne mark and porphyrin values after two weeks of use. Among them, the serum containing the oil control and acne removal nano composition of Comparative Examples 1-11 or Example 1 contains magnolol, azelaic acid and kaempferol 3 kinds of functional components, and the total content is 7%, only the proportion of the three components is different, and the magnolol, azelaic acid and kaempferol three components have the largest oil content reduction rate (28.49%), acne mark diameter reduction rate (21.42%) and porphyrin content reduction rate (53.13%) in the proportion of 8:5:1, showing good skin oil control and acne removal improvement effect; secondly, compared with the serum containing the oil control and acne removal nano composition of Comparative Example 12, the serum containing the oil control and acne removal nano composition of Example 1 also shows better acne removal and oil control effect. The above results show that the oil control and acne removal composition prepared in Example 1 has scientificity in the collocation of the three functional components, and the best oil control and acne removal effect is obtained by the collocation of different action mechanisms.

[0139] As can be seen from the above, the oil control and acne removal provided by the present application has very excellent oil control and acne removal effect.

[0140] Although the above examples make a detailed description of the present application, it is only a part of the embodiments of the present application, not all the embodiments, and people can also obtain other embodiments according to the present embodiment without creativity, which all belong to the protection scope of the present application.

Claims

1. An oil control acne-fighting nano-composition characterized in that, The oil-control acne-removing nano composition comprises magnolol, azelaic acid, kaempferol, an anti-allergic agent, a pimple mark lightening active, an emulsifier, a co-emulsifier, a lipid, and water; The mass percentage of the anti-allergic agent in the oil-control acne-removing nano composition is 0.1% to 5%; The mass percentage of the anti-allergic agent in the oil-control acne-removing nano composition is 0.1% to 5%; The mass percentage of the anti-allergic agent in the oil-control acne-removing nano composition is 0.1% to 5%; The mass percentage of the anti-allergic agent in the oil-control acne-removing nano composition is 0.1% to 5%; The mass percentage of the emulsifier in the oil-control acne-removing nano composition is 5 to 40%; The mass percentage of the co-emulsifier in the oil-control acne-removing nano composition is 5 to 40%; The mass percentage of the lipid in the oil-control acne-removing nano composition is 5 to 30%; The mass ratio of the magnolol, azelaic acid, and kaempferol in the oil-control acne-removing nano composition is (7.6 to 8.4) : (4.7 to 5.3) : (0.9 to 1.1).

2. The oil control acne-fighting nano-composition of claim 1, wherein, The anti-allergic agent comprises one or more of glycyrrhetinic acid, glycyrrhizic acid salt, bisabalol, and beta-glucan.

3. The oil control acne-fighting nano-composition of claim 1, wherein, The pimple mark lightening active comprises one or more of nicotinamide, heparin sodium, carnosine, and decarboxy carnosine.

4. The oil control acne-fighting nano-composition of claim 1, wherein, The mass ratio of the magnolol, azelaic acid, and kaempferol is 8:5:

1.

5. The oil control acne-fighting nano-composition of claim 1, wherein, The emulsifier comprises one or more of polyoxyethylene sorbitan fatty acid ester, polyglyceryl fatty acid ester, polyoxyethylene fatty acid ester, PEG-8 caprylic / capric glycerides, polyoxyethylene hydrogenated castor oil, fatty alcohol polyoxyethylene ether, coco-glucoside, lecithin, PEG-30 dipolyhydroxystearate, and ceteareth.

6. The oil control acne-fighting nano-composition of claim 1, wherein, The co-emulsifier comprises one or more of glycerol, diethylene glycol monoethyl ether, polyethylene glycol-400, 1,3-butanediol, 1,2-propanediol, dipropylene glycol, 1,2-hexanediol, 1,2-pentanediol, ethoxydiglycol, ethoxydiglycol oleate, and octyldodecanol.

7. The oil control acne-fighting nano-composition of claim 1, wherein, The lipid comprises one or more of isopropyl myristate, isopropyl palmitate, caprylic / capric triglyceride, caprylic / capric polyethylene glycol glyceride, polyethylene glycol laurate glyceride, polyethylene glycol stearate glyceride, linoleic acid glyceride, propylene glycol monocaprylate, propylene glycol dicaprylocaprate, glyceryl stearate, acetylated monoglyceride, caprylocapryl cocoa butter, cetyl alcohol, stearyl alcohol, and cetearyl alcohol.

8. A process for the preparation of the oil control acne-fighting nano-composition according to any one of claims 1 to 7, characterized in that, The method comprises the following steps: mixing the magnolol, azelaic acid, kaempferol, anti-allergic agent, emulsifier, co-emulsifier, and lipid to obtain an oil phase; mixing the pimple mark lightening active and water to obtain an aqueous phase; adding the aqueous phase to the oil phase, mixing, and then micronizing to obtain a micron-grade dispersion; nanoizing the micron-grade dispersion to obtain the oil-control acne-removing nano composition.

9. The production method according to claim 8, characterized by, The micronizing is achieved by high-speed shearing emulsification, and the nanoizing is achieved by high-pressure homogenization or high-speed microjet treatment.

10. Use of the oil-control acne-removing nano composition of any one of claims 1 to 7 or obtained by the preparation method of claims 8 or 9 in the preparation of a cosmetic.

Images