Preparation process of a niacinamide whitening repair mask

Abstract

This invention relates to the field of whitening and repairing technology, specifically to a preparation process for a niacinamide whitening and repairing facial mask, comprising the following steps: dissolving glycerin and 1,3-propanediol in deionized water, adding disodium ethylenediaminetetraacetate, Centella asiatica extract, and Portulaca oleracea extract, stirring evenly and adjusting the pH to obtain phase A; adding niacinamide-β-cyclodextrin-polyethylene glycol inclusion complex, cross-linked hyaluronic acid microgel dispersion, tranexamic acid liposome dispersion, α-arbutin, and panthenol, stirring and adjusting the pH to obtain an essence; finally, after cooling, adding octoxyglycerol, stirring evenly, filtering, and impregnating the essence into a mask sheet to prepare a niacinamide whitening and repairing facial mask. The niacinamide-β-cyclodextrin-polyethylene glycol inclusion complex utilizes molecular inclusion technology to effectively improve the stability of niacinamide, avoiding the irritation risk caused by its hydrolysis to produce nicotinic acid, while simultaneously enhancing the transdermal absorption rate of niacinamide through the penetration-enhancing effect of polyethylene glycol.

Description

Technical Field

[0001] This invention relates to the field of whitening and repairing technology, and more specifically, to a niacinamide whitening and repairing facial mask preparation process. Background Technology

[0002] Facial masks, as an important carrier for skin care, are highly favored by consumers due to their high permeability and efficacy. Among the many skin care effects, whitening and repair are among the most in-demand areas. Niacinamide, a derivative of vitamin B3, is a classic whitening ingredient with clinically proven efficacy. Its mechanism mainly involves inhibiting the transport of melanin to keratinocytes, accelerating keratin renewal, and improving the skin barrier. In addition, ingredients such as tranexamic acid and alpha-arbutin enhance the whitening effect by inhibiting tyrosinase activity. To improve the skin feel and repair performance, modern facial mask formulas often combine moisturizers such as glycerin and panthenol, as well as soothing plant extracts such as centella asiatica and purslane. Current technology typically involves simply mixing the above active ingredients with deionized water, thickeners, preservatives, etc., and then loading them onto a mask sheet to prepare a basic whitening facial mask.

[0003] However, the traditional preparation process mentioned above still has obvious limitations; the core active ingredient niacinamide is very easy to hydrolyze into nicotinic acid during production and storage, causing skin redness, stinging and other irritating reactions, resulting in a decrease in the product's mildness and poor efficacy stability, which affects the final whitening effect. In view of this, we propose a preparation process for niacinamide whitening and repairing masks. Summary of the Invention

[0004] The purpose of this invention is to provide a preparation process for a niacinamide whitening and repairing facial mask, in order to solve the problem mentioned in the background art that the core active ingredient niacinamide is easily hydrolyzed to generate nicotinic acid during production and storage, causing skin redness, stinging and other irritating reactions, resulting in a decrease in the product's mildness and poor efficacy stability, thus affecting the final whitening effect.

[0005] This invention provides a process for preparing a niacinamide whitening and repairing facial mask, comprising the following steps:

[0006] 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;

[0007] 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;

[0008] 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;

[0009] 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.

[0010] Preferably, in step S1.1, the following raw materials are weighed in parts by weight: 30-50 parts deionized water, 3.0-8.0 parts glycerol, 2.0-5.0 parts 1,3-propanediol, 0.1-0.5 parts Centella asiatica extract, 0.01-0.1 parts disodium EDTA, 3.0-6.0 parts nicotinamide-β-cyclodextrin-polyethylene glycol inclusion complex, 2.0-5.0 parts tranexamic acid liposome dispersion, 0.5-2.0 parts cross-linked hyaluronic acid microgel dispersion, 0.5-2.0 parts panthenol, 0.2-0.5 parts α-arbutin, 0.1-0.5 parts purslane extract, and 0.1-0.5 parts octoxyglycerol.

[0011] Preferably, the preparation process of the nicotinamide-β-cyclodextrin-polyethylene glycol inclusion complex is as follows:

[0012] 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.

[0013] Preferably, the molar ratio of nicotinamide to β-cyclodextrin-polyethylene glycol copolymer is 1:1-1.5.

[0014] Preferably, the preparation process of the tranexamic acid liposome dispersion is as follows:

[0015] 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.

[0016] Preferably, the lipid phase solution is prepared by dissolving soybean lecithin 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%.

[0017] 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%.

[0018] Preferably, the preparation process of the cross-linked hyaluronic acid microgel dispersion is as follows:

[0019] 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.

[0020] Preferably, the amount of 1,4-butanediol glycidyl ether added accounts for 5-10% of the mass of hyaluronic acid.

[0021] Preferably, in step S1.4, the impregnation method is as follows: the mask base fabric is laid flat in a 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.

[0022] Preferably, the mask base fabric is any one of Tencel fiber, silk or bio-cellulose material.

[0023] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0024] In the preparation process of the niacinamide whitening and repairing mask of this invention, the niacinamide-β-cyclodextrin-polyethylene glycol inclusion complex utilizes molecular inclusion technology to effectively improve the stability of niacinamide and avoid the irritation risk caused by its hydrolysis to produce nicotinic acid. At the same time, the permeation-enhancing effect of polyethylene glycol enhances the transdermal absorption rate of niacinamide. The tranexamic acid liposome dispersion uses a phospholipid bilayer as a carrier to efficiently encapsulate water-soluble tranexamic acid, significantly improving its transdermal ability and targeting, making it easier for whitening ingredients to reach the skin base and exert their effects, while reducing the degradation of active ingredients. The cross-linked hyaluronic acid microgel dispersion forms a three-dimensional moisturizing network on the skin surface, not only providing long-lasting hydration but also extending the action time of active ingredients through a sustained-release mechanism, maintaining the stability of the formulation system. Detailed Implementation

[0025] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0026] Centella asiatica extract, CAS: 84696-21-9, purchased from Shaanxi Xintianyu Biotechnology Co., Ltd.

[0027] The active ingredients of Centella asiatica extract mainly include triterpenoids (asiaticoside, hydroxyasiaticoside, asiaticoside, hydroxyasiaticoside, etc.), as well as flavonoids (such as quercetin and kaempferol), volatile oils, polysaccharides, amino acids, etc.

[0028] Disodium ethylenediaminetetraacetate (EDTA): CAS 139-33-3, purchased from Hefei Tanrun Biotechnology Co., Ltd.

[0029] Purslane extract (CAS: 90083-07-1) was purchased from Fufeng Sinote Biotechnology Co., Ltd.

[0030] The active ingredients in purslane extract mainly include: flavonoids (such as quercetin), organic acids, polysaccharides, alkaloids, vitamin E, polyphenols, saponins, etc.

[0031] Octoxyglycerol (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 Alpha-Arbutin (CAS: 84380-01-8) were all purchased from Shanghai Yuanye Biotechnology Co., Ltd.

[0032] Preparation process of β-cyclodextrin-polyethylene glycol: Under nitrogen protection and ice bath conditions, polyethylene glycol is dissolved in toluene, p-toluenesulfonyl chloride and pyridine are slowly added, and the reaction is carried out at low temperature. After the reaction is completed, the polyethylene glycol is obtained by precipitation, filtration, washing and vacuum drying. The p-toluenesulfonyl activated polyethylene glycol is then dissolved together with β-cyclodextrin in dimethyl sulfoxide at a molar ratio of 1:1. Sodium hydroxide is added, and the mixture is stirred and reacted in an oil bath at 60-80℃ for 24-48 h under nitrogen protection. After the reaction is completed, the mixture is cooled to room temperature, dialyzed through ultrapure water, and freeze-dried to obtain the β-cyclodextrin-polyethylene glycol copolymer.

[0033] β-Cyclodextrin (CAS: 7585-39-9) and polyethylene glycol (CAS: 25322-68-3, molecular weight 2000-6000) were purchased from Shanghai Yuanye Biotechnology Co., Ltd.

[0034] Soybean phospholipids CAS: 69279-91-0, purchased from Hanzhong Hansuyuan Biotechnology Co., Ltd.

[0035] The mask base fabric is any one of Tencel fiber, silk or bio-cellulose material, preferably bio-cellulose.

[0036] Example 1: A preparation process for a niacinamide whitening and repairing facial mask, comprising the following steps:

[0037] S1.1 Weigh the following raw materials separately: 30 parts by weight of deionized water, 3.0 parts by weight of glycerin, 2.0 parts by weight of 1,3-propanediol, 0.1 parts by weight of Centella asiatica extract, 0.01 parts by weight of disodium ethylenediaminetetraacetate, 3.0 parts by weight of nicotinamide-β-cyclodextrin-polyethylene glycol inclusion complex, 2.0 parts by weight of tranexamic acid liposome dispersion, 0.5 parts by weight of cross-linked hyaluronic acid microgel dispersion, 0.5 parts by weight of panthenol, 0.2 parts by weight of α-arbutin, 0.1 parts by weight of purslane extract, and 0.1 parts by weight of octoxyglycerol;

[0038] 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;

[0039] 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.

[0040] 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.

[0041] The preparation process of nicotinamide-β-cyclodextrin-polyethylene glycol inclusion complex is as follows:

[0042] The β-cyclodextrin-polyethylene glycol copolymer was dissolved in deionized water to obtain a 5% (w / w) β-cyclodextrin-polyethylene glycol solution. Nicotinamide was added to the β-cyclodextrin-polyethylene glycol solution at a molar ratio of 1:1, and the mixture was stirred at 400 rpm for 2 h at room temperature, followed by refrigeration at 4 °C for 12 h. Finally, the mixture was subjected to vacuum spray drying at a pressure of 15 kPa, an inlet air temperature of 60 °C, and an outlet air temperature of 40 °C to obtain the nicotinamide-β-cyclodextrin-polyethylene glycol inclusion complex.

[0043] The preparation process of tranexamic acid liposome dispersion is as follows:

[0044] The lipid phase solution is prepared by dissolving soybean lecithin and cholesterol in ethanol at a mass ratio of 8:2, resulting in a lipid phase solution with a mass concentration of 0.5%.

[0045] 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 1% (w / w) tranexamic acid aqueous solution.

[0046] The lipid phase solution was injected into the tranexamic acid aqueous solution at a volume ratio of 1:5 and stirred at 1000 rpm for 20 min to obtain a mixture. The mixture was then sonicated at 400 W for 5 min and then extruded through a 200 nm polycarbonate membrane to obtain a tranexamic acid liposome dispersion.

[0047] The preparation process of cross-linked hyaluronic acid microgel dispersion is as follows:

[0048] 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%. 1,4-Butanediol glycidyl ether, accounting for 5% 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 dispersion with a mass concentration of 8%, thus obtaining a cross-linked hyaluronic acid microgel dispersion.

[0049] Example 2: A preparation process for a niacinamide whitening and repairing facial mask, comprising the following steps:

[0050] S1.1 Weigh the following raw materials separately: 50 parts by weight of deionized water, 8.0 parts by weight of glycerin, 5.0 parts by weight of 1,3-propanediol, 0.5 parts by weight of Centella asiatica extract, 0.1 parts by weight of disodium ethylenediaminetetraacetate, 6.0 parts by weight of nicotinamide-β-cyclodextrin-polyethylene glycol inclusion complex, 5.0 parts by weight of tranexamic acid liposome dispersion, 2.0 parts by weight of cross-linked hyaluronic acid microgel dispersion, 2.0 parts by weight of panthenol, 0.5 parts by weight of α-arbutin, 0.5 parts by weight of purslane extract, and 0.5 parts by weight of octoxyglycerol;

[0051] 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;

[0052] 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.

[0053] 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.

[0054] The preparation process of nicotinamide-β-cyclodextrin-polyethylene glycol inclusion complex is as follows:

[0055] The β-cyclodextrin-polyethylene glycol copolymer was dissolved in deionized water to obtain a 10% (w / w) β-cyclodextrin-polyethylene glycol solution. Nicotinamide was added to the β-cyclodextrin-polyethylene glycol solution at a molar ratio of 1:1.5, and the mixture was stirred at 400 rpm for 2 h at room temperature, followed by refrigeration at 4 °C for 12 h. Finally, the mixture was vacuum spray dried at a pressure of 15 kPa, an inlet air temperature of 60 °C, and an outlet air temperature of 40 °C to obtain the nicotinamide-β-cyclodextrin-polyethylene glycol inclusion complex.

[0056] The preparation process of tranexamic acid liposome dispersion is as follows:

[0057] The lipid phase solution is prepared by dissolving soybean lecithin and cholesterol in ethanol at a mass ratio of 8:2, resulting in a lipid phase solution with a mass concentration of 1%.

[0058] 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 3% (w / w) tranexamic acid aqueous solution.

[0059] The lipid phase solution was injected into the tranexamic acid aqueous solution at a volume ratio of 1:10 and stirred at 1000 rpm for 20 min to obtain a mixture. The mixture was then sonicated at 400 W for 5 min and then extruded through a 200 nm polycarbonate membrane to obtain a tranexamic acid liposome dispersion.

[0060] The preparation process of cross-linked hyaluronic acid microgel dispersion is as follows:

[0061] 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.

[0062] Example 3: A preparation process for a niacinamide whitening and repairing facial mask, comprising the following steps:

[0063] 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;

[0064] 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;

[0065] 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.

[0066] 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.

[0067] The preparation process of nicotinamide-β-cyclodextrin-polyethylene glycol inclusion complex is as follows:

[0068] The β-cyclodextrin-polyethylene glycol copolymer was dissolved in deionized water to obtain an 8% (w / w) β-cyclodextrin-polyethylene glycol solution. Nicotinamide was added to the β-cyclodextrin-polyethylene glycol solution at a molar ratio of 1:1.2, and the mixture was stirred at 400 rpm for 2 h at room temperature, followed by refrigeration at 4 °C for 12 h. Finally, the mixture was vacuum spray dried at a pressure of 15 kPa, an inlet air temperature of 60 °C, and an outlet air temperature of 40 °C to obtain the nicotinamide-β-cyclodextrin-polyethylene glycol inclusion complex.

[0069] The preparation process of tranexamic acid liposome dispersion is as follows:

[0070] The lipid phase solution is prepared by dissolving soybean lecithin and cholesterol in ethanol at a mass ratio of 8:2, resulting in a lipid phase solution with a mass concentration of 0.6%.

[0071] 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 2% (w / w) tranexamic acid aqueous solution.

[0072] The lipid phase solution was injected into the tranexamic acid aqueous solution at a volume ratio of 1:8 and stirred at 1000 rpm for 20 min to obtain a mixture. The mixture was then sonicated at 400 W for 5 min and then extruded through a 200 nm polycarbonate membrane to obtain a tranexamic acid liposome dispersion.

[0073] The preparation process of cross-linked hyaluronic acid microgel dispersion is as follows:

[0074] 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%. 1,4-Butanediol glycidyl ether, accounting for 8% 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 dispersion with a mass concentration of 10%, thus obtaining a cross-linked hyaluronic acid microgel dispersion.

[0075] Example 4: The difference between this example and Example 3 is that the molar ratio of nicotinamide and β-cyclodextrin-polyethylene glycol copolymer is 1:1.5.

[0076] Example 5: The difference between this example and Example 3 is that the molar ratio of nicotinamide and β-cyclodextrin-polyethylene glycol copolymer is 1:1.8.

[0077] Example 6: The difference between this example and Example 3 is that the volume ratio of the lipid phase solution to the tranexamic acid aqueous solution is 1:10.

[0078] Example 7: The difference between this example and Example 3 is that the volume ratio of the lipid phase solution to the tranexamic acid aqueous solution is 1:12.

[0079] 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.

[0080] 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.

[0081] Comparative Example 1: The difference between this comparative example and Example 3 is that nicotinamide was added directly.

[0082] Comparative Example 2: The difference between this comparative example and Example 3 is that an aqueous solution of tranexamic acid was directly added.

[0083] Comparative Example 3: The difference between this comparative example and Example 3 is that hyaluronic acid solution was added directly.

[0084] 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.

[0085] 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 ).

[0086] Determination of moisturizing rate: 18–30 subjects, both male and female; 30 minutes before the test, the subject should be placed in a room at 22±2℃ and relative humidity of 45–55%; the test area (forearm / cheek) should be cleaned and skincare products should be discontinued for at least 12 hours; designated test points (3 points per side, avoiding blood vessels / scars) should be used, and the average of 3 readings should be taken as C0; a face mask should be applied (or a standard dose of 2 mg / cm² should be applied to the forearm). 2 Apply the essence, remove it according to the instructions (10-20 minutes), and gently wipe away any unabsorbed liquid; read the moisture content immediately after removing the mask (T0), at 2 hours, 4 hours, and 8 hours (average of 3 readings per point); calculate: Moisturizing rate (%) = (C t −C0) / C0×100.

[0087] Determination of stimulation rate: The experiment requires at least 30 subjects with no skin lesions on their backs; each subject is given 2-4 samples (including the present invention, comparative examples, and control groups), with 20-30 μL of sample applied per patch; the patch is closed for 48 hours after application, during which time washing and strenuous exercise should be avoided; the patch is removed after 48 hours, and observations and scores are taken at 0h and 24h respectively; the scoring criteria are as follows (0-4 points): 0 = no reaction; 1 = mild erythema; 2 = erythema + mild edema / papules; 3 = significant redness and swelling; 4 = vesicles / erosion; stimulation rate (%) = (number of people with ≥ grade 1 reaction) / (total number of subjects) × 100.

[0088] The niacinamide whitening and repairing masks prepared in Examples 1-9 and Comparative Examples 1-3 are shown in Table 1.

[0089] Table 1 Performance data of Niacinamide Whitening and Repairing Masks in Examples 1-9 and Comparative Examples 1-3

[0090]

[0091] As shown in Table 1, the nicotinic acid growth rate was lowest in Example 4 (4.0%), followed by Example 3 (4.2%), and highest in Example 5 (4.5%); the cumulative permeation of nicotinamide was highest in Example 3 (435 mg / cm³). 2 Example 4 was slightly lower (428 mg / cm³). 2 Example 5 showed a significant reduction (405 mg / cm³). 2 The moisturizing rate and irritation were not significantly different among the three. The main difference lies in the fact that β-cyclodextrin (β-CD) molecules have a hydrophobic inner cavity and a hydrophilic outer surface. Their inclusion effect primarily relies on hydrophobic interactions, van der Waals forces, and size matching. When the molar ratio was 1:1.2 (Example 3) and 1:1.5 (Example 4), sufficient β-CD molecules were present in the system, ensuring that the vast majority of nicotinamide was effectively included, forming a stable inclusion complex. This inclusion behavior acts as a protective barrier for unstable nicotinamide molecules, isolating them from external moisture and the environment, thereby greatly inhibiting... The process of hydrolysis to niacin is obstructed, resulting in a low niacin growth rate. The introduction of polyethylene glycol (PEG) segments enhances the water solubility and spreading penetration ability of the entire inclusion complex on the skin surface, promoting transdermal delivery of niacinamide and thus increasing the penetration amount. However, when the molar ratio increases to 1:1.8 (Example 5), the excess β-CD-PEG copolymer leads to steric hindrance. Too many β-CD molecules do not participate in effective inclusion but instead form larger aggregates in the system, increasing diffusion resistance and making it more difficult for the inclusion complex to penetrate the stratum corneum, resulting in a decrease in niacinamide penetration. At the same time, these irregular and loose aggregates may actually bind some water molecules inside the aggregates, increasing local water activity, thus causing a slight rebound in the hydrolysis rate of a small amount of poorly included niacinamide or niacinamide on the surface of the aggregates, manifested as a slight rebound in the niacin growth rate.

[0092] Furthermore, in Examples 6 and 7, compared to Example 3, the cumulative permeation of tranexamic acid was significantly reduced, while the irritation rate also increased. The volume ratio of the lipid phase to the aqueous phase is a key parameter determining the encapsulation efficiency, particle size, and stability of liposomes. At the ratio of 1:8 in Example 3, when the lipid solution is injected into the aqueous phase, liposomes with high encapsulation efficiency, uniform particle size, and stable structure are formed. Because their structure is highly similar to that of the cell membrane, these liposomes can effectively fuse with the stratum corneum of the skin and efficiently deliver the encapsulated tranexamic acid to the deep layers of the skin through the intercellular lipid pathway or deformation penetration, thus achieving the highest permeation. When the aqueous phase ratio increases to 1... When the ratios are 1:10 (Example 6) and 1:12 (Example 7), it means that during the preparation process, the volume of aqueous phase that needs to be encapsulated by a unit volume of lipid is too large. This excessive volume of aqueous phase means that some tranexamic acid cannot be effectively encapsulated in the aqueous phase of the liposomes, but exists in the dispersed phase in a free form, forming larger, multi-chambered or uneven vesicles, and even phospholipid precipitation. Its stability and penetration efficiency will be greatly reduced, resulting in a decrease in the effective delivery amount (penetration) of tranexamic acid. More importantly, free tranexamic acid directly contacts the skin, and its irritation is much higher than that of the state encapsulated by liposomes, which directly leads to an increase in the product irritation rate.

[0093] As can be seen from Table 1, compared with Example 3, the moisturizing performance of Examples 8 and 9 showed a trend of first increasing and then decreasing; Example 8 had the highest moisturizing rate (+47.8%), while Example 9 dropped to +45.0%, even lower than the baseline Example 3 (+46.5%); the crosslinking agent 1,4-butanediol glycidyl ether reacts with the hydroxyl groups of the hyaluronic acid molecular chain to form stable ether bonds, thereby constructing a three-dimensional network structure; at the crosslinking agent dosage of Example 3 (8%), the network structure formed has a moderate degree of crosslinking, which can effectively absorb and lock in moisture, providing excellent moisturizing effect; when the crosslinking agent dosage is increased to Example 8 (10%), the network structure is more compact, the water absorption capacity and mechanical strength reach the best state, and the moisturizing performance is significantly improved; however, when the crosslinking agent dosage is further increased to Example 9 (12%), the network structure is over-crosslinked, the crosslinking density increases significantly, resulting in a reduction in the pores in the network, a decrease in the water absorption capacity, and difficulty in releasing moisture, thereby leading to a decrease in moisturizing performance.

[0094] The growth rate of nicotinic acid in Comparative Example 1 (28.5%) was extremely high, the irritation was significant (10%), and the nicotinamide penetration (265 mg / cm³) was also low. 2The results were significantly lower than in Example 3. Niacinamide is readily hydrolyzed in aqueous formulations to produce nicotinic acid, which is highly irritating to the skin and is the main cause of product intolerance. In Comparative Example 1, ordinary nicotinamide was added directly without protective measures and exposed to the formulation environment, resulting in severe hydrolysis and a very high nicotinic acid growth rate, leading to a high irritation rate. On the other hand, untreated nicotinamide is a hydrophilic small molecule, and its transdermal absorption mainly relies on passive diffusion, making it difficult to effectively penetrate the lipid barrier of the stratum corneum. Therefore, its bioavailability is low and its penetration is poor. In contrast, the inclusion complex technology in Example 3, through the inclusion effect of β-CD, hides the nicotinamide molecules, fundamentally cutting off its hydrolysis pathway, greatly improving stability and significantly reducing irritation. At the same time, the introduction of PEG chains and the nano-size effect of the inclusion complex improve its lipophilicity, providing a new transdermal pathway, thereby significantly improving its penetration and efficacy.

[0095] The tranexamic acid permeability of Comparative Example 2 was 9.8 mg / cm³. 2 Extremely low, less than Example 3 (38.7 mg / cm³). 2 One-quarter of the total; Tranexamic acid is a highly hydrophilic molecule, making it difficult to pass through the lipid-based intercellular pathway in the stratum corneum of the skin; in the simple aqueous solution form of Example 2, its transdermal ability is extremely limited, with most of the active ingredients only remaining on the skin surface before being washed away, resulting in a very low transdermal rate; while the liposomes in Example 3 have a phospholipid bilayer structure that is highly similar to and compatible with the lipids of the stratum corneum of the skin, and can efficiently deliver the encapsulated tranexamic acid through the skin barrier to the target site through mechanisms such as adsorption, fusion, and lipid exchange, thereby achieving an order-of-magnitude increase in penetration and greatly enhancing its whitening effect.

[0096] The moisturizing rate of Comparative Example 3 (+28.0%) was much lower than that of Example 3 (+46.5%), although the two were not significantly different in terms of stability and irritation. Ordinary sodium hyaluronate (Comparative Example 3) is a linear macromolecule, and its moisturizing effect depends on the hydrogen bonds formed between hydrophilic groups such as carboxyl groups on the molecular chain and water molecules. However, this binding is relatively weak, and water is easily evaporated in dry environments, resulting in a short-term moisturizing effect that is adequate but lacks long-term moisturizing ability. Cross-linked hyaluronic acid microgel (Example 3) forms a three-dimensional network through chemical cross-linking. This network can not only bind water through hydrogen bonds, but also physically lock in a large amount of water through its porous structure, forming a reservoir. On the skin surface, this gel film can slowly and continuously release water into the stratum corneum, providing a long-lasting and powerful moisturizing effect.

[0097] The foregoing has shown and described the basic principles, main features, and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments. The embodiments and descriptions in the specification are merely preferred examples and are not intended to limit the invention. Various changes and modifications can be made to the invention without departing from its spirit and scope, and all such changes and modifications fall within the scope of the present invention as claimed. The scope of protection of the present invention 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 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; 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. The preparation process of the nicotinamide-β-cyclodextrin-polyethylene glycol inclusion complex 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 of nicotinamide to β-cyclodextrin-polyethylene glycol copolymer of 1:1-1.5, and stirred at 300-400 rpm for 2 hours at room temperature, followed by refrigeration at 4℃ for 12 hours; finally, it is subjected to vacuum spray drying at 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 complex.

2. The preparation process of the niacinamide whitening and repairing facial mask according to claim 1, 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.

3. The process for preparing the niacinamide whitening and repairing mask according to claim 2, 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%.

4. The process for preparing the niacinamide whitening and protective mask according to claim 1, 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.

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

6. The process for preparing the niacinamide whitening and protective 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.

7. The process for preparing the niacinamide whitening and repairing mask according to claim 6, characterized in that, The mask base fabric is any one of Tencel fiber, silk, or bio-cellulose material.

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