Preparation process of nicotinamide whitening and repairing mask

Abstract

The invention relates to the technical field of whitening and repairing, in particular to a preparation process of a nicotinamide whitening and repairing mask, which comprises the following steps: dissolving glycerol and 1, 3-propylene glycol in deionized water, adding disodium ethylene diamine tetraacetate, centella asiatica extract and purslane extract, uniformly stirring, and adjusting the pH value to obtain a phase A; adding a nicotinamide-beta-cyclodextrin-polyethylene glycol inclusion compound, a cross-linked hyaluronic acid microgel dispersion, a tranexamic acid liposome dispersion liquid, alpha-arbutin and panthenol, stirring, and adjusting the pH value to obtain essence; and finally, cooling, adding octyloxyglycerin, uniformly stirring, filtering, and dipping in membrane cloth to prepare the nicotinamide whitening and repairing mask. According to the nicotinamide-beta-cyclodextrin-polyethylene glycol inclusion compound, the stability of nicotinamide is effectively improved by utilizing a molecular inclusion technology, the stimulation risk caused by nicotinic acid produced by hydrolysis of the nicotinamide is avoided, and meanwhile, the percutaneous absorption rate of the nicotinamide is enhanced by virtue of the permeation enhancing effect of polyethylene glycol.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of whitening and repair, in particular to a preparation process of a niacinamide whitening and repair mask. BACKGROUND

[0002] As an important carrier of skin care, masks are favored by consumers due to their high permeability and strong efficacy. Among various skin care effects, whitening and repair is one of the most popular fields in the market. Niacinamide, as a derivative of vitamin B3, is a classic whitening ingredient that has been clinically proven. Its mechanism mainly achieves whitening by inhibiting the transport of melanin to keratinocytes, accelerating keratin turnover, and improving skin barrier. In addition, ingredients such as tranexamic acid and alpha-arbutin can synergistically enhance the whitening effect by inhibiting tyrosinase activity. To improve skin feel and repair performance, modern mask formulations often contain moisturizing agents such as glycerin and panthenol, as well as plant soothing extracts such as gota kola and gota kola. The existing technology usually simply mixes the above active ingredients with deionized water, thickening agents, preservatives, etc., and then loads them on a mask cloth to prepare a basic whitening mask.

[0003] However, the above-mentioned traditional preparation process still has obvious limitations. The core active ingredient niacinamide is prone to hydrolysis to form nicotinic acid during production and storage, causing skin redness, stinging, and other irritating reactions, resulting in decreased product mildness and poor efficacy stability, which affects the final whitening efficiency. In view of this, we propose a preparation process of a niacinamide whitening and repair mask. SUMMARY

[0004] The present application relates to the technical field of whitening and repair, in particular to a preparation process of a niacinamide whitening and repair mask.

[0005] The present application provides a preparation process of a niacinamide whitening and repair mask, comprising the following steps: S1.1, respectively, the following raw materials are weighed: deionized water, glycerin, 1,3-propanediol, gota kola extract, ethylenediaminetetraacetic acid disodium salt, niacinamide-beta-cyclodextrin-polyethylene glycol inclusion compound, tranexamic acid liposome dispersion, cross-linked hyaluronic acid microgel dispersion, panthenol, alpha-arbutin, gota kola extract and octyloxy glycerin; S1.2, glycerin and 1,3-propanediol are dissolved in deionized water, heated to 30-35℃, then ethylenediaminetetraacetic acid disodium salt, gota kola extract and gota kola extract are added, stirred at a speed of 300-500 rpm for 10-15 min, and the pH is adjusted to 5.6-6.0 with 0.05 mol / L sodium hydroxide to obtain phase A; S1.3, nicotinamide-β-cyclodextrin-polyethylene glycol inclusion compound, cross-linked hyaluronic acid microgel dispersion, tranexamic acid liposome dispersion, α-arbutin and panthenol are added into the A phase, stirring at a speed of 200-400 rpm for 15-30 min, adjusting pH to 5.6-6.0 with 0.05 mol / L sodium hydroxide, to obtain the essence; S1.4, when the essence is cooled to 30℃, add octyloxy glycerol, stirring at a speed of 200-400 rpm for 5-10 min, to obtain the mixed essence; the mixed essence is filtered through a 0.45 μm microporous filter membrane, immersed in a membrane cloth, to obtain a nicotinamide whitening and repairing mask.

[0006] As a preferred, in S1.1, the following raw materials are weighed respectively: deionized water 30-50 parts by weight, glycerol 3.0-8.0 parts by weight, 1,3-propanediol 2.0-5.0 parts by weight, asiaticoside extract 0.1-0.5 parts by weight, disodium ethylenediaminetetraacetate 0.01-0.1 parts by weight, nicotinamide-β-cyclodextrin-polyethylene glycol inclusion compound 3.0-6.0 parts by weight, tranexamic acid liposome dispersion 2.0-5.0 parts by weight, cross-linked hyaluronic acid microgel dispersion 0.5-2.0 parts by weight, panthenol 0.5-2.0 parts by weight, α-arbutin 0.2-0.5 parts by weight, purslane extract 0.1-0.5 parts by weight and octyloxy glycerol 0.1-0.5 parts by weight.

[0007] As a preferred, the preparation process of the nicotinamide-β-cyclodextrin-polyethylene glycol inclusion compound is as follows: β-cyclodextrin-polyethylene glycol copolymer is dissolved in deionized water to obtain a β-cyclodextrin-polyethylene glycol solution with a mass concentration of 5-10%; nicotinamide is added to the β-cyclodextrin-polyethylene glycol solution at a molar ratio, stirring at a speed of 300-400 rpm for 2 h at room temperature, and then placed in a 4℃ refrigerator for 12 h; finally, vacuum spray drying treatment is performed, with a pressure of 5-20 kPa, an inlet air temperature of 60-80℃ and an outlet air temperature of 40-50℃, to obtain the nicotinamide-β-cyclodextrin-polyethylene glycol inclusion compound.

[0008] As a preferred, the molar ratio of nicotinamide to β-cyclodextrin-polyethylene glycol copolymer is 1:1-1.5.

[0009] As a preferred, the preparation process of the tranexamic acid liposome dispersion is as follows: The lipid phase solution is injected into the aqueous tranexamic acid solution at a volume ratio of 1:5-10, stirring at a speed of 1000 rpm for 10-20 min to obtain a mixed solution; then the mixed solution is ultrasonically treated at a power of 200-400 W for 3-5 min, and then extruded through a 200 nm polycarbonate membrane to obtain the tranexamic acid liposome dispersion.

[0010] As preferred, the lipid phase solution is prepared by dissolving soybean phospholipid and cholesterol in ethanol at a mass ratio of 8:2 to obtain a lipid phase solution with a mass concentration of 0.5-1%; The aqueous solution of tranexamic acid is prepared by dissolving tranexamic acid in deionized water, and adjusting the pH to 6.0 with 0.05 mol / L sodium hydroxide to obtain an aqueous solution of tranexamic acid with a mass concentration of 1-3%.

[0011] As preferred, the preparation process of the cross-linked hyaluronic acid microgel dispersion is as follows: Sodium hyaluronate with a molecular weight of 80-150 kDa is dissolved in deionized water to obtain a solution with a mass concentration of 0.05-0.1%; 1,4-butanediol glycidyl ether is added, and the reaction is carried out at 10-25℃ for 2-4h; after the reaction is completed, dialysis is carried out, and the cross-linked product is precipitated with ethanol; the precipitate is spray dried to obtain a microgel powder; the powder is dispersed in deionized water again to prepare a dispersion with a mass concentration of 8-10% to obtain a cross-linked hyaluronic acid microgel dispersion.

[0012] As preferred, the amount of 1,4-butanediol glycidyl ether added accounts for 5-10% of the mass of hyaluronic acid.

[0013] As preferred, in S1.4, the impregnation method is as follows: the mask base cloth is laid flat in a tray, and a quantitative pump is used to inject 18-22g of essence liquid per piece, and the mask base cloth is soaked for 2-5min.

[0014] As preferred, the mask base cloth is any one of tencel fiber, silk or biological cellulose material.

[0015] Compared with the prior art, the beneficial effects of the present application are: In the preparation process of the nicotinamide whitening and repairing mask of the present application, the nicotinamide-β-cyclodextrin-polyethylene glycol inclusion compound utilizes molecular inclusion technology to effectively improve the stability of nicotinamide, avoids the irritation risk caused by the hydrolysis product nicotinic acid, and at the same time, with the aid of the penetration of polyethylene glycol, the transdermal absorption rate of nicotinamide is enhanced; the tranexamic acid liposome dispersion is prepared by using a phospholipid bilayer as a carrier to efficiently encapsulate water-soluble tranexamic acid, which greatly improves the transdermal ability and targeting of the active ingredient, so that the whitening ingredient can more easily reach the skin and play a role, and the degradation of the active ingredient is reduced; the cross-linked hyaluronic acid microgel dispersion forms a three-dimensional moisturizing network on the skin surface, not only providing long-lasting moisturizing, but also prolonging the action time of the active substance through the slow-release mechanism, and maintaining the stability of the formula system. DETAILED DESCRIPTION

[0016] The technical solutions in the embodiments of the present application will be clearly and completely described below in conjunction with the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments of the present application. Based on the embodiments of the present application, all other embodiments obtained by a person of ordinary skill in the art without creative effort fall within the protection scope of the present application.

[0017] Centella asiatica extract CAS:84696-21-9, purchased from Shaanxi Xintianyu Biotechnology Co., Ltd.

[0018] The active components of Centella asiatica extract mainly include triterpenoids (asiaticoside, madecassoside, madecassic acid, etc.), flavonoids (such as quercetin and kaempferol), volatile oil, polysaccharides, amino acids, etc.

[0019] Disodium ethylenediaminetetraacetate CAS:139-33-3, purchased from Hefei Tanlun Biotechnology Co., Ltd.

[0020] Portulaca oleracea extract CAS:90083-07-1, purchased from Fufeng Snoot Biotechnology Co., Ltd.

[0021] The active components of Portulaca oleracea extract mainly include flavonoids (such as quercetin), organic acids, polysaccharides, alkaloids, vitamin E, polyphenols, saponins, etc.

[0022] Octoxyglycerin CAS:70445-33-9, nicotinamide CAS:98-92-0, tranexamic acid CAS:1197-18-8, cholesterol CAS:57-88-5, sodium hyaluronate CAS:9067-32-7, 1,4-butanediol glycidyl ether CAS:2425-79-8, and α-arbutin CAS:84380-01-8, all purchased from Shanghai Yuanye Biotechnology Co., Ltd.

[0023] Preparation process of β-cyclodextrin-polyethylene glycol: under the conditions of nitrogen protection and ice bath, polyethylene glycol was dissolved in toluene, p-toluenesulfonyl chloride and pyridine were slowly added, and the reaction was carried out at low temperature; after the reaction was completed, p-toluenesulfonyl activated polyethylene glycol was obtained by precipitation, filtration, washing and vacuum drying; the p-toluenesulfonyl activated polyethylene glycol and β-cyclodextrin were dissolved in dimethyl sulfoxide at a molar ratio of 1:1, sodium hydroxide was added, and the mixture was stirred at 60-80°C in an oil bath under nitrogen protection for 24-48h; after the reaction was completed, the mixture was cooled to room temperature, dialyzed by ultrapure water, and freeze-dried to obtain β-cyclodextrin-polyethylene glycol copolymer.

[0024] β-cyclodextrin CAS: 7585-39-9, polyethylene glycol CAS: 25322-68-3 (molecular weight 2000-6000) were purchased from Shanghai Yuan Ye Biotechnology Co., Ltd.

[0025] Soybean phospholipid CAS: 69279-91-0 was purchased from Hanzhong Hansuoyuan Biotechnology Co., Ltd.

[0026] The mask base cloth is any one of Tencel fiber, silk or biological cellulose material, preferably biological cellulose.

[0027] Example 1: Preparation process of nicotinamide whitening and repairing mask, comprising the following steps: S1.1, respectively, the following raw materials: deionized water 30 parts by weight, glycerol 3.0 parts by weight, 1,3-propanediol 2.0 parts by weight, asiaticoside extract 0.1 parts by weight, ethylenediaminetetraacetic acid disodium 0.01 parts by weight, nicotinamide-β-cyclodextrin-polyethylene glycol inclusion compound 3.0 parts by weight, tranexamic acid liposome dispersion 2.0 parts by weight, cross-linked hyaluronic acid microgel dispersion 0.5 parts by weight, panthenol 0.5 parts by weight, α-arbutin 0.2 parts by weight, spilanthes extract 0.1 parts by weight and octoxyglycerol 0.1 parts by weight; S1.2, glycerol and 1,3-propanediol were dissolved in deionized water, heated to 35℃, then ethylenediaminetetraacetic acid disodium, asiaticoside extract and spilanthes extract were added, stirred at a speed of 400 rpm for 15 min, and the pH was adjusted to 6.0 with 0.05 mol / L sodium hydroxide to obtain phase A; S1.3, nicotinamide-β-cyclodextrin-polyethylene glycol inclusion compound, cross-linked hyaluronic acid microgel dispersion, tranexamic acid liposome dispersion, α-arbutin and panthenol were added to phase A, stirred at a speed of 200 rpm for 20 min, and the pH was adjusted to 6.0 with 0.05 mol / L sodium hydroxide to obtain the serum; S1.4, when the serum cooled to 30℃, add octoxyglycerol, stir at a speed of 200 rpm for 10 min, get mixed serum; the mixed serum was filtered through a 0.45 μm microporous filter; the biological cellulose mask base cloth was laid in the tray, and 20 g of serum was injected into each piece using a quantitative pump, and soaked for 5 min to obtain a nicotinamide whitening and repairing mask.

[0028] The preparation process of nicotinamide-β-cyclodextrin-polyethylene glycol inclusion compound is as follows: The β-cyclodextrin-polyethylene glycol copolymer was dissolved in deionized water to obtain a β-cyclodextrin-polyethylene glycol solution with a mass concentration of 5%; nicotinamide was added to the β-cyclodextrin-polyethylene glycol solution at a molar ratio of 1:1, stirred at a speed of 400 rpm for 2 h at room temperature, and then placed in a 4℃ refrigerator for 12 h of static setting; finally, vacuum spray drying was performed at a pressure of 15 kPa, with an inlet air temperature of 60℃ and an outlet air temperature of 40℃, to obtain a nicotinamide-β-cyclodextrin-polyethylene glycol inclusion compound.

[0029] The preparation process of the tranexamic acid liposome dispersion is as follows: The lipid phase solution was prepared by dissolving soybean phospholipid and cholesterol in ethanol at a mass ratio of 8:2 to obtain a lipid phase solution with a mass concentration of 0.5%; The aqueous solution of tranexamic acid was prepared by dissolving tranexamic acid in deionized water and adjusting the pH to 6.0 with 0.05 mol / L sodium hydroxide to obtain an aqueous solution of tranexamic acid with a mass concentration of 1%; The lipid phase solution was injected into the aqueous solution of tranexamic acid at a volume ratio of 1:5, and stirred at a speed of 1000 rpm for 20 min to obtain a mixture; then the mixture was ultrasonically treated at a power of 400 W for 5 min, and then extruded through a 200 nm polycarbonate membrane to obtain a tranexamic acid liposome dispersion.

[0030] The preparation process of the cross-linked hyaluronic acid microgel dispersion is as follows: Sodium hyaluronate with a molecular weight of 100 kDa was dissolved in deionized water to obtain a solution with a mass concentration of 0.05%; 5% of 1,4-butanediol glycidyl ether based on the mass of hyaluronic acid was added, and the reaction was carried out at 25℃ for 4 h; after the reaction was completed, dialysis was performed, and the cross-linked product was precipitated with ethanol; the precipitate was spray dried to obtain a microgel powder; the powder was redispersed in deionized water to prepare a dispersion with a mass concentration of 8% to obtain a cross-linked hyaluronic acid microgel dispersion.

[0031] Example 2: A preparation process of a nicotinamide whitening and repairing mask, comprising the following steps: S1.1, respectively, the following raw materials are weighed: deionized water 50 parts by weight, glycerol 8.0 parts by weight, 1,3-propanediol 5.0 parts by weight, asiaticoside extract 0.5 parts by weight, ethylenediaminetetraacetic acid disodium 0.1 parts by weight, nicotinamide-β-cyclodextrin-polyethylene glycol inclusion compound 6.0 parts by weight, tranexamic acid liposome dispersion 5.0 parts by weight, cross-linked hyaluronic acid microgel dispersion 2.0 parts by weight, panthenol 2.0 parts by weight, α-arbutin 0.5 parts by weight, purslane extract 0.5 parts by weight and octoxyglycerol 0.5 parts by weight; S1.2, glycerol and 1,3-propanediol were dissolved in deionized water, heated to 35℃, then added with disodium ethylenediaminetetraacetate, ginseng extract and purslane extract, stirred at a speed of 400 rpm for 15 min, adjusted to pH 6.0 with 0.05 mol / L sodium hydroxide, to obtain phase A; S1.3, nicotinamide-β-cyclodextrin-polyethylene glycol inclusion compound, cross-linked hyaluronic acid microgel dispersion, tranexamic acid liposome dispersion, alpha-arbutin and panthenol were added into phase A, stirred at a speed of 200 rpm for 20 min, adjusted to pH 6.0 with 0.05 mol / L sodium hydroxide, to obtain the serum; S1.4, when the serum cooled to 30℃, added with octyloxy glycerol, stirred at a speed of 200 rpm for 10 min, to obtain the mixed serum; the mixed serum was filtered through a 0.45 μm microporous filter membrane; the biological cellulose mask base cloth was laid in a tray, and 20 g of the serum was injected into each piece using a quantitative pump, and stood for 5 min for infiltration, to obtain the nicotinamide whitening and repairing mask.

[0032] The preparation process of the nicotinamide-β-cyclodextrin-polyethylene glycol inclusion compound is as follows: The β-cyclodextrin-polyethylene glycol copolymer was dissolved in deionized water to obtain a β-cyclodextrin-polyethylene glycol solution with a mass concentration of 10%; nicotinamide was added to the β-cyclodextrin-polyethylene glycol solution at a molar ratio of 1:1.5, stirred at a speed of 400 rpm for 2 h at room temperature, and then placed in a 4℃ refrigerator for 12 h; finally, vacuum spray drying was performed at a pressure of 15 kPa, with an inlet air temperature of 60℃ and an outlet air temperature of 40℃, to obtain the nicotinamide-β-cyclodextrin-polyethylene glycol inclusion compound.

[0033] The preparation process of the tranexamic acid liposome dispersion is as follows: The lipid phase solution was prepared by dissolving soybean phospholipid and cholesterol in ethanol at a mass ratio of 8:2 to obtain a lipid phase solution with a mass concentration of 1%; The tranexamic acid aqueous solution was prepared by dissolving tranexamic acid in deionized water, and adjusting the pH to 6.0 with 0.05 mol / L sodium hydroxide to obtain a tranexamic acid aqueous solution with a mass concentration of 3%; The lipid phase solution was injected into the tranexamic acid aqueous solution at a volume ratio of 1:10, stirred at a speed of 1000 rpm for 20 min, then the mixture was ultrasonically treated at a power of 400 W for 5 min, and then extruded through a 200 nm polycarbonate membrane to obtain the tranexamic acid liposome dispersion.

[0034] The preparation process of the cross-linked hyaluronic acid microgel dispersion is as follows: Sodium hyaluronate with a molecular weight of 100 kDa was dissolved in deionized water to obtain a 0.1% solution. 1,4-Butanediol glycidyl ether, accounting for 10% of the mass of hyaluronic acid, was added, and the mixture was reacted at 25°C for 4 hours. After the reaction was completed, the mixture was dialyzed, and the cross-linked product was precipitated with ethanol. The precipitate was spray-dried to obtain a microgel powder. The powder was redispersed in deionized water to prepare a 10% dispersion, thus obtaining a cross-linked hyaluronic acid microgel dispersion.

[0035] Example 3: A preparation process for a niacinamide whitening and repairing facial mask, comprising the following steps: S1.1 Weigh the following raw materials separately: 40 parts by weight of deionized water, 5.5 parts by weight of glycerin, 3.5 parts by weight of 1,3-propanediol, 0.3 parts by weight of Centella asiatica extract, 0.06 parts by weight of disodium ethylenediaminetetraacetate, 4.5 parts by weight of nicotinamide-β-cyclodextrin-polyethylene glycol inclusion complex, 3.5 parts by weight of tranexamic acid liposome dispersion, 1.2 parts by weight of cross-linked hyaluronic acid microgel dispersion, 1.2 parts by weight of panthenol, 0.3 parts by weight of α-arbutin, 0.3 parts by weight of purslane extract, and 0.3 parts by weight of octoxyglycerol; S1.2 Dissolve glycerol and 1,3-propanediol in deionized water, heat to 35°C, then add disodium ethylenediaminetetraacetate, Centella asiatica extract and Portulaca oleracea extract, stir at 400 rpm for 15 min, adjust pH to 6.0 with 0.05 mol / L sodium hydroxide to obtain phase A; S1.3 Add nicotinamide-β-cyclodextrin-polyethylene glycol inclusion complex, cross-linked hyaluronic acid microgel dispersion, tranexamic acid liposome dispersion, α-arbutin and panthenol to phase A, stir at 200 rpm for 20 min, and adjust the pH to 6.0 with 0.05 mol / L sodium hydroxide to obtain the essence. S1.4 When the essence is cooled to 30℃, add octyloxyglycerin and stir at 200rpm for 10min to obtain a mixed essence; filter the mixed essence through a 0.45μm microporous membrane; lay the bio-cellulose mask base flat in a tray, inject 20g of essence into each sheet using a metering pump, and let it stand to soak for 5min to obtain a niacinamide whitening and repairing mask.

[0036] The preparation process of nicotinamide-β-cyclodextrin-polyethylene glycol inclusion complex is as follows: The β-cyclodextrin-polyethylene glycol copolymer was dissolved in deionized water to obtain a β-cyclodextrin-polyethylene glycol solution with a mass concentration of 8%; nicotinamide was added to the β-cyclodextrin-polyethylene glycol solution at a molar ratio of 1:1.2, stirred at a speed of 400 rpm at room temperature for 2 h, and then placed in a 4℃ refrigerator for 12 h; finally, vacuum spray drying was performed at a pressure of 15 kPa, an inlet air temperature of 60℃, and an outlet air temperature of 40℃ to obtain a nicotinamide-β-cyclodextrin-polyethylene glycol inclusion compound.

[0037] The preparation process of the tranexamic acid liposome dispersion is as follows: The lipid phase solution was prepared by dissolving soybean phospholipid and cholesterol in ethanol at a mass ratio of 8:2 to obtain a lipid phase solution with a mass concentration of 0.6%; The aqueous tranexamic acid solution was prepared by dissolving tranexamic acid in deionized water and adjusting the pH to 6.0 with 0.05 mol / L sodium hydroxide to obtain an aqueous tranexamic acid solution with a mass concentration of 2%; The lipid phase solution was injected into the aqueous tranexamic acid solution at a volume ratio of 1:8, stirred at a speed of 1000 rpm for 20 min to obtain a mixture; then the mixture was ultrasonically treated at a power of 400 W for 5 min, and then extruded through a 200 nm polycarbonate membrane to obtain a tranexamic acid liposome dispersion.

[0038] The preparation process of the cross-linked hyaluronic acid microgel dispersion is as follows: Sodium hyaluronate with a molecular weight of 100 kDa was dissolved in deionized water to obtain a solution with a mass concentration of 0.08%; 8% of 1,4-butanediol glycidyl ether based on the mass of hyaluronic acid was added and reacted at 25℃ for 4 h; after the reaction was completed, dialysis was performed, and the cross-linked product was precipitated with ethanol; the precipitate was spray dried to obtain a microgel powder; the powder was redispersed in deionized water to prepare a dispersion with a mass concentration of 10% to obtain a cross-linked hyaluronic acid microgel dispersion.

[0039] Example 4: Compared with Example 3, the difference is that the molar ratio of nicotinamide to β-cyclodextrin-polyethylene glycol copolymer is 1:1.5.

[0040] Example 5: Compared with Example 3, the difference is that the molar ratio of nicotinamide to β-cyclodextrin-polyethylene glycol copolymer is 1:1.8.

[0041] Example 6: Compared with Example 3, the difference is that the volume ratio of the lipid phase solution to the aqueous tranexamic acid solution is 1:10.

[0042] Example 7: Compared with Example 3, the difference is that the volume ratio of the lipid phase solution to the aqueous tranexamic acid solution is 1:12.

[0043] Example 8: The difference between this example and Example 3 is that the amount of 1,4-butanediol glycidyl ether added accounts for 10% of the mass of hyaluronic acid.

[0044] Example 9: The difference between this example and Example 3 is that the amount of 1,4-butanediol glycidyl ether added accounts for 12% of the mass of hyaluronic acid.

[0045] Comparative Example 1: The difference between this comparative example and Example 3 is that nicotinamide was added directly.

[0046] Comparative Example 2: The difference between this comparative example and Example 3 is that an aqueous solution of tranexamic acid was directly added.

[0047] Comparative Example 3: The difference between this comparative example and Example 3 is that hyaluronic acid solution was added directly.

[0048] Determination of nicotinic acid growth rate: Prepare nicotinamide and nicotinic acid standard solutions (0.5-100 μg / mL) separately and establish a column line on the HPLC system; take 1.0 g of the mask essence and dilute to 50 mL (ultrasound for 3-5 min if necessary to ensure homogenization), filter through a 0.22 μm microporous membrane to remove particulates; determine the flow rate at 1.0 mL / min, column temperature at 30℃, and inject 10 μL; record the retention time and peak area; calculate the concentrations (mg / mL) of nicotinamide and nicotinic acid according to the standard curve and convert them to the content in the sample (%w / w); calculate the nicotinic acid growth rate (%) = (C t -C0) / C0×100%; where C t C0 represents the nicotinic acid content at time t (mg / g), and C0 represents the nicotinic acid content at time t0.

[0049] Determination of cumulative penetration of nicotinamide and tranexamic acid over 24 hours: In a skin model, hair-free, degreased skin samples of uniform thickness (500-800 μm) were equilibrated in PBS for 30 minutes; receptor solution was added to the receptor chamber and kept at a constant temperature of 32℃ to ensure no air bubbles were present; a mask essence or a sheet soaked in the mask (with consistent dosage per unit area) was placed on the surface of the donor chamber and sealed to prevent evaporation; sampling was conducted at 0.5, 1, 2, 4, 6, 8, 12, and 24 hours, with 0.5 mL of receptor solution taken each time and immediately replenished with an equal volume of fresh receptor solution; the concentrations of nicotinamide and tranexamic acid were determined by HPLC; the cumulative penetration was calculated using the following formula: ,in For the first Sample concentration (mg / mL) The sampling volume is (mL). The total volume of the receptor, Effective diffusion area (cm) 2 ).

[0050] Moisture retention rate determination: 18-30 subjects, male and female; 30 min before test, keep in a room with 22±2℃ and 45-55% relative humidity; clean the test area (forearm / cheek) and stop using skin care products for at least 12 h; designate test points (3 points on each side, avoiding blood vessels / scars), record 3 readings and take the average as C0; apply the mask (or apply the essence on the forearm at a standard dose of 2 mg / cm 2 ), remove it after the specified time (10-20 min), and gently wipe off the unabsorbed liquid; immediately after removing the mask (T0), 2 h, 4 h, and 8 h, read the moisture content (3 times for each point and take the average); calculate: moisture retention rate (%) = (C t −C0) / C0×100.

[0051] Irritation rate determination: at least 30 subjects are required, and the back should be free of skin lesions; each subject is applied with 2-4 samples (including the present application, comparative examples, and control groups), and 20-30 μL of each sample is applied; after application, close for 48 h, and avoid water washing and vigorous exercise during this period; after 48 h, remove the application, and observe and score at 0 h and 24 h, respectively; the scoring criteria are as follows (0-4 points): 0 = no reaction; 1 = mild erythema; 2 = erythema + mild edema / papules; 3 = obvious redness; 4 = blisters / erosions; irritation rate (%) = (number of people with ≥1 grade reaction) / (total number of subjects) × 100.

[0052] The nicotinamide whitening and repairing masks prepared in the above Examples 1-9 and Comparative Examples 1-3 are as follows, wherein the performance data of the nicotinamide whitening and repairing masks are shown in Table 1: Table 1 Performance data of nicotinamide whitening and repairing masks of Examples 1-9 and Comparative Examples 1-3

[0053] As can be seen from Table 1, the nicotinic acid growth rate is the lowest in Example 4 (4.0%), followed by Example 3 (4.2%), and the highest in Example 5 (4.5%); the cumulative penetration amount of nicotinamide is the highest in Example 3 (435 mg / cm 2 ), slightly lower in Example 4 (428 mg / cm 2 ), and significantly reduced in Example 5 (405 mg / cm 2); the moisture retention rate and the irritation rate have little difference among the three; the main reason is that the β-cyclodextrin (β-CD) molecule has a hydrophobic inner cavity and a hydrophilic outer surface, and its inclusion mainly depends on hydrophobic interaction, van der Waals force and size matching; when the molar ratio is 1:1.2 (Example 3) and 1:1.5 (Example 4), there are sufficient β-CD molecules in the system to ensure that most of the nicotinamide is effectively included to form stable inclusion compounds; this inclusion behavior is like a protective effect for unstable nicotinamide molecules, which isolates them from water and the environment, thereby greatly inhibiting the process of hydrolysis to form nicotinic acid, so the growth rate of nicotinic acid is low; the introduction of polyethylene glycol (PEG) segments enhances the water solubility and spreading and penetrating ability of the entire inclusion compound on the skin surface, promoting the transdermal delivery of nicotinamide, thereby increasing the permeation amount; however, when the molar ratio increases to 1:1.8 (Example 5), the excess β-CD-PEG copolymer will cause a steric hindrance effect, and too many β-CD molecules do not participate in effective inclusion, but form larger aggregates in the system, increase the diffusion resistance, make it more difficult for the inclusion compound to penetrate the stratum corneum, and result in a decrease in the permeation amount of nicotinamide. At the same time, this irregular and loose aggregate may bind some water molecules inside the aggregate, increasing the local water activity, thereby causing a slight increase in the hydrolysis rate of a small amount of poorly included or surface-bound nicotinamide, resulting in a slight rebound in the growth rate of nicotinic acid.

[0054] It can be further seen that in Example 6 and Example 7, compared with Example 3, the cumulative permeation amount of tranexamic acid is significantly reduced, and the irritation rate also increases; the volume ratio of lipid phase to water phase is a key parameter for determining the encapsulation rate, particle size and stability of liposomes; at the ratio of 1:8 in Example 3, when the lipid solution is injected into the water phase, liposomes with high encapsulation rate, uniform particle size and stable structure can be formed; these liposomes, due to their high similarity to cell membranes, can effectively fuse with the stratum corneum, and through the intercellular lipid pathway or deformation penetration, the encapsulated tranexamic acid is efficiently delivered to the deep layer of the skin, so the permeation amount is the highest; when the water phase ratio increases to 1:10 (Example 6) and 1:12 (Example 7), it means that in the preparation process, the unit volume of lipid needs to encapsulate a larger volume of water phase, which will cause part of the tranexamic acid to be unable to be effectively encapsulated in the inner water phase of the liposome, but to exist in the dispersed phase in a free form, forming larger, multi-chamber or non-uniform vesicles, or even causing the precipitation of phospholipids, which will greatly reduce the stability and penetration efficiency, resulting in a decrease in the effective delivery amount (permeation amount) of tranexamic acid; more importantly, the free tranexamic acid directly contacts the skin, and its irritation is much higher than that of the liposome-encapsulated state, which directly leads to an increase in the irritation rate of the product.

[0055] It can be further seen from Table 1 that the moisturizing performance of Examples 8 and 9 shows a trend of first increasing and then decreasing compared with Example 3; the moisturizing rate of Example 8 is the highest (+47.8%), while that of Example 9 falls back to +45.0%, even lower than that of the benchmark Example 3 (+46.5%); the crosslinking agent 1,4-butanediol glycidyl ether forms stable ether bonds by reacting with the hydroxyl groups of the hyaluronic acid molecular chain, thereby constructing a three-dimensional network structure; at the crosslinking agent dosage of Example 3 (8%), the network structure formed has moderate crosslinking degree, which can effectively absorb and lock water, providing excellent moisturizing effect; when the crosslinking agent dosage increases to Example 8 (10%), the network structure is more compact, and the water absorption capacity and mechanical strength reach the best state, and the moisturizing performance is significantly improved; however, when the crosslinking agent dosage further increases to Example 9 (12%), the network structure is excessively crosslinked, the crosslinking density significantly increases, resulting in reduced pores in the network, decreased water absorption capacity, and difficulty in releasing water, thereby leading to decreased moisturizing performance.

[0056] The nicotinic acid growth rate of Comparative Example 1 (28.5%) is extremely high, the irritability (10%) is significantly high, and the nicotinamide penetration amount (265 mg / cm 2 ) is much lower than that of Example 3; nicotinamide is extremely easy to hydrolyze in an aqueous formulation to generate nicotinic acid, and nicotinic acid has strong irritability to the skin, which is the main reason for product intolerance; Comparative Example 1 directly adds ordinary nicotinamide without protection measures, which is exposed to the formulation environment, resulting in severe hydrolysis, extremely high nicotinic acid growth rate, and thus high irritability rate; on the other hand, untreated nicotinamide is a hydrophilic small molecule, and its transdermal absorption mainly depends on passive diffusion, which is difficult to effectively penetrate the lipid barrier of the stratum corneum of the skin, and thus has low bioavailability and poor penetration amount; while the inclusion complex technology in Example 3 hides the nicotinamide molecules by the inclusion effect of β-CD, fundamentally cutting off the hydrolysis path of nicotinamide, greatly improving the stability and significantly reducing the irritability; at the same time, the introduction of the PEG chain and the nanosize effect of the inclusion complex improve the lipophilicity of nicotinamide, providing a new transdermal pathway, thereby greatly improving the penetration amount and efficacy of nicotinamide.

[0057] The tranexamic acid penetration amount of Comparative Example 2 (9.8 mg / cm 2 ) is extremely low, less than that of Example 3 (38.7 mg / cm 2) is a quarter; tranexamic acid is a highly hydrophilic molecule, difficult to pass through the skin keratinocytes in the main intercellular pathway of lipid; its simple aqueous solution form in proportion 2, its transdermal ability is extremely limited, most of the active substances can only stay on the skin surface and then be washed away, the transdermal rate is extremely low; and the liposome in example 3 has a high degree of similarity and compatibility with the lipid of the skin keratin layer, which can be absorbed, fused, and lipid exchanged to efficiently encapsulate the tranexamic acid inside the skin barrier and directly reach the target site, thereby achieving a magnitude of penetration and greatly enhancing its whitening effect.

[0058] The moisture retention rate of comparative example 3 (+28.0%) is much lower than that of example 3 (+46.5%), although there is little difference in stability and irritation between the two; ordinary sodium hyaluronate (comparative example 3) is a linear macromolecule, and its moisturizing effect depends on the hydrogen bond formed by the hydrophilic groups such as carboxyl on the molecular chain and water molecules; however, this combination is relatively weak, and water is easily evaporated in a dry environment, so the moisturizing effect is not long-lasting, and it performs well in short-term moisturizing but lacks long-term moisturizing ability; the cross-linked hyaluronic acid microgel (example 3) forms a three-dimensional network through chemical cross-linking; this network not only can bind water through hydrogen bonds, but also can physically lock a large amount of water through its porous structure to form a water reservoir; on the skin surface, this gel film can slowly and continuously release water to the keratin layer, providing long-term and strong moisturizing effect.

[0059] The above shows and describes the basic principles, main features and advantages of the present application. Those skilled in the art should understand that the present application is not limited to the above examples, and the above examples and descriptions in the specification are only preferred examples of the present application and are not intended to limit the present application. Without departing from the spirit and scope of the present application, various changes and improvements can be made to the present application, and these changes and improvements all fall within the scope of the claimed present application. The scope of protection of the present application is defined by the appended claims and their equivalents.

Claims

1. A preparation process of a niacinamide whitening repair mask, characterized in that, Includes the following steps: S1.1 Weigh the following raw materials separately: deionized water, glycerin, 1,3-propanediol, Centella asiatica extract, disodium EDTA, nicotinamide-β-cyclodextrin-polyethylene glycol inclusion complex, tranexamic acid liposome dispersion, cross-linked hyaluronic acid microgel dispersion, panthenol, α-arbutin, purslane extract and octoxyglycerol; S1.2 Dissolve glycerol and 1,3-propanediol in deionized water, heat to 30-35℃, then add disodium ethylenediaminetetraacetate, Centella asiatica extract and Portulaca oleracea extract, stir at 300-500 rpm for 10-15 min, adjust the pH to 5.6-6.0 with 0.05 mol / L sodium hydroxide to obtain phase A; S1.3 Add nicotinamide-β-cyclodextrin-polyethylene glycol inclusion complex, cross-linked hyaluronic acid microgel dispersion, tranexamic acid liposome dispersion, α-arbutin and panthenol to phase A, stir at 200-400 rpm for 15-30 min, adjust pH to 5.6-6.0 with 0.05 mol / L sodium hydroxide to obtain the essence; S1.4 When the essence is cooled to 30℃, add octyloxyglycerin and stir at 200-400rpm for 5-10min to obtain a mixed essence; filter the mixed essence through a 0.45μm microporous membrane and impregnate the mask cloth to obtain a niacinamide whitening and repairing mask.

2. The process for preparing the niacinamide whitening and repairing mask according to claim 1, characterized in that, In step S1.1, the following raw materials are weighed in parts by weight: 30-50 parts by weight of deionized water, 3.0-8.0 parts by weight of glycerin, 2.0-5.0 parts by weight of 1,3-propanediol, 0.1-0.5 parts by weight of Centella asiatica extract, 0.01-0.1 parts by weight of disodium ethylenediaminetetraacetate, 3.0-6.0 parts by weight of nicotinamide-β-cyclodextrin-polyethylene glycol inclusion complex, 2.0-5.0 parts by weight of tranexamic acid liposome dispersion, 0.5-2.0 parts by weight of cross-linked hyaluronic acid microgel dispersion, 0.5-2.0 parts by weight of panthenol, 0.2-0.5 parts by weight of α-arbutin, 0.1-0.5 parts by weight of purslane extract, and 0.1-0.5 parts by weight of octoxyglycerol.

3. The process for preparing the niacinamide whitening and repairing mask according to claim 2, characterized in that, The preparation process of the nicotinamide-β-cyclodextrin-polyethylene glycol inclusion complex is as follows: The β-cyclodextrin-polyethylene glycol copolymer was dissolved in deionized water to obtain a β-cyclodextrin-polyethylene glycol solution with a mass concentration of 5-10%. Nicotinamide was added to the β-cyclodextrin-polyethylene glycol solution by molar ratio, and the mixture was stirred at 300-400 rpm for 2 hours at room temperature, followed by refrigeration at 4°C for 12 hours. Finally, the mixture was subjected to vacuum spray drying at a pressure of 5-20 kPa, an inlet air temperature of 60-80°C, and an outlet air temperature of 40-50°C to obtain the nicotinamide-β-cyclodextrin-polyethylene glycol inclusion complex.

4. The process for preparing the niacinamide whitening and repairing mask according to claim 3, characterized in that, The molar ratio of nicotinamide and β-cyclodextrin-polyethylene glycol copolymer is 1:1-1.

5.

5. The process for preparing the niacinamide whitening and repairing mask according to claim 2, characterized in that, The preparation process of the tranexamic acid liposome dispersion is as follows: The lipid phase solution was injected into the tranexamic acid aqueous solution at a volume ratio of 1:5-10 and stirred at 1000 rpm for 10-20 min to obtain a mixture. The mixture was then ultrasonically treated with a power of 200-400W for 3-5 min and then extruded through a 200nm polycarbonate membrane to obtain a tranexamic acid liposome dispersion.

6. The process for preparing the niacinamide whitening and repairing mask according to claim 5, characterized in that, The lipid phase solution is prepared by dissolving soybean phospholipids and cholesterol in ethanol at a mass ratio of 8:2 to obtain a lipid phase solution with a mass concentration of 0.5-1%. Tranexamic acid aqueous solution is prepared by dissolving tranexamic acid in deionized water and adjusting the pH to 6.0 with 0.05 mol / L sodium hydroxide to obtain a tranexamic acid aqueous solution with a mass concentration of 1-3%.

7. The preparation process of the niacinamide whitening and repairing mask according to claim 2, characterized in that, The preparation process of the cross-linked hyaluronic acid microgel dispersion is as follows: Sodium hyaluronate with a molecular weight of 80-150 kDa was dissolved in deionized water to obtain a solution with a mass concentration of 0.05-0.1%; 1,4-butanediol glycidyl ether was added, and the mixture was reacted at 10-25℃ for 2-4 hours; after the reaction was completed, the mixture was dialyzed, and the cross-linked product was precipitated with ethanol; the precipitate was spray-dried to obtain a microgel powder; the powder was redispersed in deionized water to prepare a dispersion with a mass concentration of 8-10%, thus obtaining a cross-linked hyaluronic acid microgel dispersion.

8. The preparation process of the niacinamide whitening and repairing mask according to claim 7, characterized in that, The amount of 1,4-butanediol glycidyl ether added accounts for 5-10% of the mass of hyaluronic acid.

9. The preparation process of the niacinamide whitening and repairing facial mask according to claim 1, characterized in that, In step S1.4, the soaking method is as follows: the mask base fabric is laid flat in the tray, 18-22g of essence is injected into each mask using a metering pump, and the mask is left to soak for 2-5 minutes.

10. The preparation process of the niacinamide whitening and repairing facial mask according to claim 9, characterized in that, The mask base fabric is any one of Tencel fiber, silk, or bio-cellulose material.

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