Carboxymethyl chitosan-maltodextrin dry instant facial mask and its preparation method

Abstract

This invention discloses a dry, quick-dissolving facial mask using carboxymethyl chitosan and maltodextrin as main raw materials, comprising a non-woven fabric substrate layer and a nanofiber layer. The nanofiber layer is formed on the non-woven fabric substrate layer using a spinning solution with pure water as a solvent and an electrospinning method. It comprises: 5-25 parts by weight of carboxymethyl chitosan, 30-70 parts by weight of dextrin, 2.5-10 parts by weight of high-molecular-weight polyethylene glycol, and 0.5-5 parts by weight of budding stalk polysaccharide. The average molecular weight of the carboxymethyl chitosan used is between 3 kDa and 30 kDa; the DE value of the maltodextrin used is between 1 and 10; the average molecular weight of the polyethylene glycol used is between 100 kDa and 500 kDa; and the average molecular weight of the budding stalk polysaccharide used is between 1 and 2 MDa. Tests show that the dry, quick-dissolving facial mask of this invention has excellent moisturizing, anti-inflammatory, redness-reducing, anti-aging, and firming effects, making it suitable not only for the general population but also for people with sensitive skin.

Description

Technical Field

[0001] This invention relates to a dry, quick-dissolving facial mask and its preparation method. More specifically, this invention relates to a cosmetic-grade dry, quick-dissolving facial mask with excellent skincare effects, made primarily from carboxymethyl chitosan and maltodextrin using electrospinning technology, and its preparation method. Background Technology

[0002] In the cosmetics market, facial masks occupy a large market share, primarily in the form of sheet masks combined with serums. However, as consumers' demands for skincare efficacy increase, new types of functional masks are constantly being developed. Instant-dissolving masks prepared using electrospinning technology not only provide an immediate firming experience, but long-term anti-wrinkle efficacy experiments have also shown that masks made with this technology offer higher skincare benefits than ordinary non-woven sheet masks, making them highly popular in the current cosmetics market.

[0003] Many materials can be electrospun, but the raw materials available for making cosmetic masks are very limited, mainly due to safety concerns. Most instant masks use natural or fermented polymers as the main material. Chinese patent application 201910053466.0 discloses a nano-instantaneous mask with a budding short-stalk enzyme polysaccharide as the framework and its preparation method, and Chinese patent application 201910052945.0 discloses a collagen nano-instantaneous mask with hyaluronic acid as the framework and its preparation method; both use natural fermented polysaccharides as the main material.

[0004] Chitosan, also known as deacetylated chitin or polyglucosamine, is a linear aminopolysaccharide composed of 2-glucosamine linked by β-1,4-glycosidic bonds. Due to its biodegradability, biocompatibility, non-toxicity, antibacterial properties, anticancer effects, lipid-lowering effects, and immune-enhancing properties, it is widely used in the biomedical field. The structure of chitosan makes it essentially insoluble in pure water, but soluble in various acids.

[0005] Dextrin is an intermediate product of starch decomposition, and its chemical formula is the same as that of starch, both being (C6H4O). 10 O5)n, but the degree of polymerization is between that of soluble starch and maltose.

[0006] Cyclodextrin (CD) is a general term for cyclic oligosaccharides composed of 6-12 D-glucan units, produced from linear starch by cyclodextrin glucosyltransferase (CGT) produced by Bacillus. The most common natural cyclodextrins are α-cyclodextrin, β-cyclodextrin, and γ-cyclodextrin, which have poor water solubility. However, the main drawback of poor water solubility of β-cyclodextrin can be overcome by introducing hydroxypropyl derivatives such as hydroxypropyl-β-cyclodextrin (HP-β-CD).

[0007] Maltodextrin (MD) is a low-conversion product between starch and starch sugars. It is a starch derivative that does not contain free starch, produced by low-degree enzymatic hydrolysis, refining, and spray drying. The physical properties of maltodextrin are directly related to its DE value (reducing sugar equivalent) of hydrolysis. Therefore, the DE value not only indicates the degree of hydrolysis but is also an important indicator for understanding product characteristics. When the DE value of maltodextrin is between 4 and 6, its sugar composition consists entirely of larger molecules of tetrasaccharides or more; when the DE value is between 9 and 12, its sugar composition contains more high-molecular-weight sugars and less low-molecular-weight sugars.

[0008] In the prior art, Chinese patent application 202010207765.8 discloses a protective wound dressing, which is obtained by electrospinning a spinning solution containing a composition of a mixture of β-cyclodextrin and Morinda officinalis alcohol extract. The β-cyclodextrin mixture includes chitosan and hydroxypropyl-β-cyclodextrin, and the chitosan is dissolved in a sufficient amount of 0.2 to 0.5 mol / L hydrochloric acid solution.

[0009] Chinese patent application 202211240194.3 discloses an antibacterial electrospun micro / nanofiber dressing, which includes polycaprolactone, chitosan, hydroxypropyl-β-cyclodextrin, formic acid, acetic acid, N,N-dimethylformamide, and dichloromethane; wherein, during electrospinning, the chitosan is dissolved in anhydrous formic acid and glacial acetic acid in a 7:3 ratio.

[0010] Chinese patent application 202011603562.7 discloses a method for preparing a composite nanofiber membrane, which includes the step of dissolving β-cyclodextrin, chitosan and gelatin in a first solvent; the first solvent is at least selected from isopropanol, glacial acetic acid with a mass concentration of 1%-3%, acetic acid and dilute hydrochloric acid with a mass concentration of 1%-5%.

[0011] Chinese patent application 201811135456.3 discloses a method for preparing a nanofiber membrane for simultaneously removing trace heavy metal ions and organic pollutants from water. The spinning solution of the nanofiber is prepared by dissolving polyvinyl alcohol, chitosan and cyclodextrin in a certain mass ratio in a 2% aqueous acetic acid solution.

[0012] Chitosan, dextrin, and other natural raw materials appear to be potential natural polysaccharides for use in cosmetic face masks. However, their application in the cosmetic field requires addressing at least the following practical technical problems or challenges:

[0013] (1) Solvent problem of spinning solution: Pure water must be used as solvent because if there are acidic substances or organic solvents in the mask, the delicate facial skin will be allergic to most people; general industrial electrospinning technology commonly uses organic solvents such as methanol, acetone, trifluoroacetic acid, and tetrahydrofuran. These solvents are not suitable for cosmetic use. Even if they evaporate during the manufacturing process, their residual amount can still cause certain toxic effects on human skin. Such solvents are basically prohibited in cosmetics. The safest and most suitable solvent for cosmetic use is pure water.

[0014] (2) Industrial mass production issues of spinning: The amount of yarn produced during electrospinning must reach a speed acceptable for industrial production, and this issue cannot be considered only from a laboratory perspective; if the spinning speed is too slow, it is not suitable for industrial production.

[0015] (3) User issues related to face masks: First, the dry fibers in the face mask should dissolve quickly during rehydration to achieve the skin-care effect; second, the dry fibers should have a certain degree of moisture resistance in high-humidity environments, otherwise, if the fibers in the face mask dissolve too quickly, it will affect the storage and transportation stability of the product and also affect the actual use by the user (such as making it difficult for the user to make necessary adjustments at the beginning of applying the face mask). In other words, the dry fibers in the face mask should be able to dissolve quickly, but it is also necessary to prevent them from dissolving too quickly. The optimal time should be controlled within 20-60 seconds.

[0016] Because chitosan, chitin, and cellulose have similar chemical structures—the only difference being that cellulose has a hydroxyl group at the C2 position, while chitin and chitosan have an acetylamino group and an amino group, respectively, at the C2 position—they are almost insoluble in water, or have very low solubility in water. Chitosan is similar; it requires acidic conditions to dissolve, such as acetic acid, hydrochloric acid, or trifluoroacetic acid.

[0017] Therefore, it is necessary to develop a formulation containing a water-soluble chitosan (chitosan) derivative, with pure water as the solvent, which has a high fiber output rate during industrial production. The resulting mask can dissolve quickly in water and has good moisture resistance in high humidity environments. Summary of the Invention

[0018] The purpose of this invention is to provide a dry, quick-dissolving facial mask for cosmetic use, made primarily from water-soluble chitosan and dextrin as spinning materials, and a method for preparing the same. The spinning solution of this dry, quick-dissolving facial mask uses a pure aqueous solution as the solvent, and the resulting product has no residual acidic substances or organic solvents.

[0019] To achieve the aforementioned objectives, this invention provides a dry, quick-dissolving facial mask using carboxymethyl chitosan and maltodextrin as main raw materials. The quick-dissolving facial mask comprises a non-woven fabric substrate layer and a nanofiber layer. The nanofiber layer is formed on the non-woven fabric substrate layer using a spinning solution with pure water as a solvent and an electrospinning method. The nanofiber layer comprises:

[0020] 5-25 parts by weight of carboxymethyl chitosan,

[0021] 30-70 parts by weight of maltodextrin

[0022] 2.5-10 parts by weight of high molecular weight polyethylene glycol,

[0023] 0.5-5 parts by weight of budding short stalk enzyme polysaccharide;

[0024] The average molecular weight of the carboxymethyl chitosan used is between 3 kDa and 30 kDa.

[0025] The maltodextrin used has a DE value of 1-10;

[0026] The average molecular weight of the polyethylene glycol used is between 100 kDa and 500 kDa;

[0027] The average molecular weight of the budding short stalk enzyme polysaccharide used is between 1 and 2 M Da, preferably between 1.5 and 2 M Da.

[0028] Chitosan is a product of the natural polysaccharide chitin, which has had some acetyl groups removed. It is insoluble or slightly soluble in pure water, but soluble in acids, while chitin itself is insoluble even under acidic conditions. The inventors of this invention discovered that adding a carboxyl group to chitosan improves its hydrophilicity, resulting in a chitosan derivative, carboxymethyl chitosan (or carboxymethyl deacetylated chitosan), which has significantly improved water solubility and can form spinning solutions soluble in pure water. Chitosan itself, however, is insoluble in water without the addition of acidic substances such as acetic acid.

[0029] Furthermore, the inventors of this invention discovered that carboxymethyl chitosan alone cannot form fibers; it must be combined with dextrin to achieve this. Moreover, the choice of dextrin is crucial, as not all dextrins are suitable for producing dry, instant facial masks via electrospinning. Under the same spinning conditions, the combination of carboxymethyl chitosan and hydroxypropyl cyclodextrin cannot be spun, while the combination with maltodextrin can. The specific reason may be related to the viscosity of the resulting spinning solution.

[0030] The inventors of this invention also surprisingly discovered that adding PEG with a high molecular weight, such as 100K Da-500K Da, not only enables the obtained spun fibers (nanofibers) to have good moisture resistance in high humidity environments, but also significantly increases the fiber yield (more than 10 times) under the same spinning conditions and with other components being the same.

[0031] The inventors of this invention also unexpectedly discovered that, under the same spinning conditions and with the same other components, adding budding short stalk enzyme polysaccharide with an average molecular weight between 1-2 M Da can further increase the amount of filament produced during spinning. However, adding too much budding short stalk enzyme polysaccharide will reduce its moisture resistance, such as shrinkage in high humidity environments.

[0032] The dry, quick-dissolving facial mask prepared according to the above-described technical solution of the present invention has excellent skin care effects. Compared with the patented products previously applied for by the applicant, it has improved the superior soft and moisturizing feel, reduced the stickiness, and provided consumers with a better experience. At the same time, it has anti-wrinkle, moisturizing, and repairing effects.

[0033] In the dry, instant facial mask of the present invention, the carboxymethyl chitosan used can be divided into medium molecular weight and low molecular weight carboxymethyl chitosans due to their different molecular weights. The average molecular weight of the medium molecular weight carboxymethyl chitosan is between 10 kDa and 30 kDa, preferably between 20 kDa and 25 kDa, while the average molecular weight of the low molecular weight carboxymethyl chitosan is between 1000 and 10000 Da, preferably between 3000 and 10000 Da. The carboxymethyl chitosan used in the present invention can be entirely medium molecular weight carboxymethyl chitosan, entirely low molecular weight carboxymethyl chitosan, or a mixture of medium and low molecular weight carboxymethyl chitosans. Preferably, medium molecular weight carboxymethyl chitosan and low molecular weight carboxymethyl chitosan are used in a mass ratio of 1:9 to 9:1, more preferably a mass ratio of 4:1 to 1:4, and most preferably a mass ratio of 2:1 to 1:2.

[0034] The inventors of this application have discovered that using two different molecular weights of carboxymethyl chitosan can provide optimal skin feel and user experience, preventing pilling and flaking when applied to the face. In this invention, K Da represents kilodaltons.

[0035] In the dry, quick-dissolving facial mask of the present invention, the nanofiber layer preferably contains 2-4 parts by weight of budding short-stem enzyme polysaccharide. In fact, the inventors of this application have discovered that although adding budding short-stem enzyme polysaccharide can further increase the amount of yarn produced during spinning, adding too much will reduce its moisture resistance. Experiments have shown that when the budding short-stem enzyme polysaccharide accounts for 2.5-5 wt% of the total weight of the nanofiber layer, the optimal effect is achieved in terms of a comprehensive consideration of production efficiency and product performance. Therefore, the content of budding short-stem enzyme polysaccharide in the formulation system of the present invention is strictly controlled.

[0036] In the dry instant facial mask of the present invention, the maltodextrin reducing sugar equivalent (DE value) used is 1-10, preferably between 1-5, and more preferably between 1-3.

[0037] In the dry instant facial mask of the present invention, the polyethylene glycol used is a high molecular weight polyethylene glycol with an average molecular weight between 100 kDa and 500 kDa, preferably between 200 kDa and 400 kDa, for example between 250 kDa and 350 kDa.

[0038] In the dry instant facial mask of the present invention, its nanofiber layer may further include 0.1-5 parts by weight, preferably 1-3 parts by weight, of medium-low molecular weight hyaluronic acid, wherein the average molecular weight of the sodium hyaluronate used is between 5 kDa and 1.5 MDa, preferably between 25 kDa and 50 kDa.

[0039] In the dry, quick-dissolving facial mask of the present invention, a certain amount of surfactant may also be added, for example, 0.5-2.5 parts by weight, preferably 1.0-1.5 parts by weight. The main function of the surfactant used is to reduce surface tension, facilitating the formation of Taylor cones at the spinneret, but not all surfactants are suitable for the present invention. The surfactant of the present invention should be water-soluble, have no adverse effects on skin care, and should not affect the formation of uniform fibers by electrospinning. That is, in the present invention, any water-soluble surfactant with certain skin care effects and conducive to electrospinning can be used. It should be noted that the amount of surfactant added is limited, because adding too much surfactant will accelerate the dissolution rate of the nanofiber layer.

[0040] Specifically, in the dry-state instant facial mask of the present invention, the surfactants used may be: polyoxyethylene sorbitan ester emulsifiers, such as polysorbate-20, polysorbate-60, polysorbate-80, etc.; sucrose ester emulsifiers, such as sucrose laurate, sucrose stearate; polyglycerol emulsifiers, such as polyglycerol-10 myristate, polyglycerol-6 caprylate, polyglycerol-6 stearate, etc.; glycoside emulsifiers, such as cocoa glucoside, lauryl glucoside, etc.; polyether or polyether ester emulsifiers, such as PEG-40 hydrogenated castor oil, PEG-20 methyl glucosesquistearate, etc.; and so on.

[0041] The electrospinning technology used in this invention refers to a construction technology in which a polymer solution overcomes surface tension under high voltage electrostatic action, forms a Taylor cone at the spinneret, and is ejected at high speed. After mechanical stretching and solvent evaporation, it solidifies to form a nanofiber structure.

[0042] The nanofiber layer in the dry-state instant facial mask of this invention is a layered structure formed by fibers with a diameter of only a few hundred nanometers, manufactured using water-soluble macromolecules such as water-soluble carboxymethyl chitosan and maltodextrin as a matrix and pure water as a solvent through electrospinning technology. It has the advantages of large specific surface area, good fiber continuity, small fiber membrane pore size, and high porosity. It has a good effect on the sustained release and protection of active ingredients, and can easily penetrate the stratum corneum of the skin to reach the deep layers of the skin, exerting functions such as moisturizing, whitening, and delaying aging.

[0043] As a specific embodiment of the present invention, the nanofiber layer of the dry-state instant facial mask of the present invention includes:

[0044] 15-20 parts by weight of carboxymethyl chitosan

[0045] 50-60 parts by weight of dextrin

[0046] 2.5-10 parts by weight of high molecular weight polyethylene glycol

[0047] 2-4 parts by weight of budding short stem enzyme polysaccharide.

[0048] In another specific embodiment of the present invention, the nanofiber layer of the dry-state instant facial mask of the present invention comprises:

[0049] 15-20 parts by weight of carboxymethyl chitosan

[0050] 50-60 parts by weight of dextrin

[0051] 5-10 parts by weight of high molecular weight polyethylene glycol

[0052] 2-4 parts by weight of sprouting short stem enzyme polysaccharide

[0053] 0.5-5 parts by weight of hyaluronic acid.

[0054] In another specific embodiment of the present invention, the nanofiber layer of the dry-state instant-dissolving facial mask of the present invention comprises:

[0055] 15-20 parts by weight of carboxymethyl chitosan

[0056] 50-60 parts by weight of dextrin

[0057] 5-10 parts by weight of high molecular weight polyethylene glycol

[0058] 2-4 parts by weight of sprouting short stem enzyme polysaccharide

[0059] 0.5-5 parts by weight of hyaluronic acid.

[0060] In another specific embodiment of the present invention, the nanofiber layer of the dry-state quick-dissolving facial mask of the present invention comprises:

[0061] 15-20 parts by weight of carboxymethyl chitosan

[0062] 50-60 parts by weight of dextrin

[0063] 2.5-10 parts by weight of high molecular weight polyethylene glycol

[0064] 2-4 parts by weight of sprouting short stem enzyme polysaccharide

[0065] 0.5-5 parts by weight of hyaluronic acid

[0066] 1.0-1.5 polyglycerol-10 myristate.

[0067] In another specific embodiment of the present invention, the nanofiber layer of the dry-state quick-dissolving facial mask of the present invention comprises:

[0068] 15-20 parts by weight of carboxymethyl chitosan

[0069] 50-60 parts by weight of dextrin

[0070] 2.5-10 parts by weight of high molecular weight polyethylene glycol

[0071] 2-4 parts by weight of sprouting short stem enzyme polysaccharide

[0072] 0.5-5 parts by weight of hyaluronic acid

[0073] 0.5-2.5 parts by weight of polyglycerol-10 myristate

[0074] 0.5-10 parts by weight of tranexamic acid

[0075] In another specific embodiment of the present invention, the nanofiber layer of the dry-state quick-dissolving facial mask of the present invention comprises:

[0076] 15-20 parts by weight of carboxymethyl chitosan

[0077] 50-60 parts by weight of dextrin

[0078] 2.5-10 parts by weight of high molecular weight polyethylene glycol

[0079] 2-4 parts by weight of sprouting short stem enzyme polysaccharide

[0080] 0.5-5 parts by weight of hyaluronic acid

[0081] 0.5-2.5 parts by weight of polyglycerol-10 myristate

[0082] 0.5-10 parts by weight of tranexamic acid

[0083] 0.1-1 parts by weight of polypeptides, such as nonapeptide-1, tripeptide-1, etc.

[0084] In the dry, quick-dissolving facial mask of this invention, a peelable protective layer may be further included on top of the nanofiber layer. In this product design, the final product has three layers: a non-woven fabric as a base layer, electrospun fibers spun on this base layer, and the fibers formed by electrospun fibers forming the middle layer (nanofiber layer); and an outer film, which can be a PE film, a BOPP film, or a non-woven fabric layer, but static electricity must be removed. This product does not require peeling off the fiber layer; simply peel off the outer film. The product may or may not include a nutrient solution; consumers simply spray pure water onto their face to use it.

[0085] Furthermore, in the dry instant facial mask of the present invention, the nanofiber layer may include 0.5-10 parts by weight of functional substances, such as polypeptides, proteins, vitamins, or other skin care agents.

[0086] On the other hand, to achieve the objective of this invention, this invention also provides a method for preparing the above-mentioned dry-state instant facial mask, wherein the method includes the following steps:

[0087] (1) Preparation of spinning solution: Using purified water as solvent, add carboxymethyl chitosan, maltodextrin, high molecular weight polyethylene glycol, and budding stalk enzyme polysaccharide, and stir to form a uniform spinning solution. This spinning solution contains 3-6 wt% carboxymethyl chitosan, 10-15 wt% maltodextrin, 0.5-2 wt% polyethylene glycol, and 0.5-1.0 wt% budding stalk enzyme polysaccharide.

[0088] (2) Electrospinning: The above-prepared spinning solution is added to the electrospinning equipment, and electrospinning is performed using non-woven fabric as the receiving substrate.

[0089] The average molecular weight of the carboxymethyl chitosan used is between 3 kDa and 30 kDa, the DE value of the maltodextrin used is between 1 and 10, the average molecular weight of the polyethylene glycol used is between 100 kDa and 500 kDa, and the average molecular weight of the budding stalk enzyme polysaccharide used is between 1 and 2 M Da.

[0090] In the preparation method of the present invention described above, the spinning solution in step (1) may further contain 0.1-1% sodium hyaluronate and / or 0.1-0.5% surfactant, wherein the molecular weight of the hyaluronic acid used is between 5K and 1.5M Da. Of course, the spinning solution in step (1) may also contain other functional substances. The humidity of the spinning environment can be controlled at 30%-50%, the spinning distance at 140mm-220mm, the spinning voltage at 40KV-85KV, and the spinning speed at 0.1-1.2 rpm.

[0091] The electrospinning equipment used in the above preparation process can be a roller-type needleless electrospinning equipment, which has the characteristics of large spinning volume, high production efficiency and uniform spinning.

[0092] Scanning electron microscopy experiments confirmed that the nanofiber layer of the mask of this invention is very uniform, without any defects such as clumps, knots, broken fibers, or voids, ensuring that the active substances are evenly distributed, have high utilization efficiency, and provide comprehensive skin care. In this way, the formed fiber structure is close to the arrangement of skin cells, which is more conducive to fully exerting the skin care effects.

[0093] The present invention will now be further described in conjunction with the accompanying drawings and specific embodiments. However, these specific embodiments are merely descriptions of certain specific implementations of the present invention and are not intended to limit the present invention. Attached Figure Description

[0094] Figure 1 The instant soothing effect of the dry-state quick-dissolving mask prepared in this invention was measured by VISIA-CR in human testing (comparison between modeling and 15 minutes after use).

[0095] Figure 2 The long-term soothing effect of the dry-state quick-dissolving facial mask prepared according to this invention was measured by VISIA-CR in human testing.

[0096] Figure 3 yes Figure 1 The changing trend of the Erythema Index (EI) value corresponding to the immediate relief;

[0097] Figure 4 yes Figure 2 The changing trend of the Erythema Index (EI) value of the skin corresponding to medium- and long-term relief. Detailed Implementation

[0098] In the specific embodiments of the present invention below, the manufacturers or distributors of the main raw materials used are as follows:

[0099] raw material Manufacturers Budding short stalk enzyme polysaccharide japan hayashibara Carboxymethyl chitosan Shanghai Chunlu polyethylene glycol Dow Chemicals Hyaluronic acid Tiansheng Bio / Huaxi Bio maltodextrin Guleite New Materials Polyglycerol-10 myristate SAKAMOTO

[0100] Comparative experiments of formulation systems

[0101] To investigate the feasibility of the formulation system, this invention conducted a series of experiments on the residual components in the nanofibers (presence or absence of acetic acid), the efficiency of electrospinning (g / h), the rehydration and solubility of the resulting spun film, and the moisture resistance of the resulting spun film (tested under high humidity conditions with RH of 75%). The results are shown in the table below. In all formulations, the same components were derived from the same batch of commercial products. For example, the average molecular weight of carboxymethyl chitosan was 10 kDa-30 kDa, the DE value of maltodextrin was 1-5, the average molecular weight of polyethylene glycol was 100 kDa-300 kDa, and the average molecular weight of pullulan was 1.5-2 M Da. The spinning solution was prepared at 25°C in each experiment, spinning was carried out on the same equipment, and the ambient temperature and humidity during spinning were 25°C and 35%-40% RH, respectively. The spinning distance was 175 cm, and the spinning voltage was 80 kV.

[0102]

[0103] Note 1: CMCS represents carboxymethyl chitosan, and HPCYD represents hydroxypropyl cyclodextrin.

[0104] 2. The fact that it easily absorbs moisture and becomes transparent means that it dissolves very easily. Having some moisture resistance means that it will not dissolve for 10-30 minutes in a high-humidity environment with an RH of 75%.

[0105] The experimental data in the table above show that:

[0106] (1) Formulas containing chitosan are insoluble in pure water and can only be dissolved in acetic acid aqueous solution;

[0107] (2) Carboxymethyl chitosan is soluble in pure water, and the spinning membrane prepared from this type of spinning solution has no acidic residue.

[0108] (3) The spinning membranes formed by acidic spinning solution of chitosan have good moisture resistance because they do not dissolve within the observation period (3 days) when rehydrated; while the spinning membranes formed by pure water spinning solution of carboxymethyl chitosan can dissolve in water within a few seconds when rehydrated.

[0109] (4) For acidic spinning solutions of chitosan, the difference in spinning effect between adding hydroxypropyl cyclodextrin and adding maltodextrin is not significant (see Formula 3 and Formula 4); however, for pure water spinning solutions of carboxymethyl chitosan, adding hydroxypropyl cyclodextrin will not result in spinning, while adding maltodextrin will result in spinning (see Formula 7 and Formula 8).

[0110] (5) Whether it is the acidic spinning solution of chitosan or the pure water spinning solution of carboxymethyl chitosan, the addition of polyethylene glycol can significantly improve the efficiency of electrospinning and increase the amount of yarn produced per unit time. Please compare formula 3 with formula 5 and formula 7 with formula 9.

[0111] (6) For pure water spinning solution of carboxymethyl chitosan, the spinning film formed without the addition of polyethylene glycol is very easy to dissolve and easily absorbs moisture and becomes transparent in a high humidity environment of 75%RH. The addition of polyethylene glycol can improve the moisture resistance of the spinning film, and it has a certain moisture resistance in a high humidity environment of 75%RH.

[0112] (7) For pure water spinning solution of carboxymethyl chitosan, the addition of budding short stem enzyme polysaccharide can significantly improve the efficiency of electrospinning and increase the amount of filament produced per unit time. See the comparison of formulas 9, 10 and 12.

[0113] (8) Further comparison of Formula 10 and Formula 12 shows that adding too much budding short stem enzyme polysaccharide will no longer improve the efficiency of electrospinning, but will instead affect the moisture-proof performance of the spinning film.

[0114] (9) Further comparison of Formula 10 and Formula 11 shows that the moisture-proof performance of the spinning film is significantly affected. Under a high humidity environment of 75% RH, the spinning film obtained by Formula 10 (with maltodextrin) only shrinks due to partial moisture absorption. After reducing the amount of pullulanose, this phenomenon is significantly improved (see Formula 12). The spinning film obtained by Formula 11 (with hydroxypropyl cyclodextrin) becomes transparent due to easy dissolution and moisture absorption.

[0115] The method for determining the amount of spun yarn in the above comparative experiment is as follows: the spun film is cut into 10CM*10CM sizes, the spun layer is peeled off, and the weight is measured on an electronic balance with a range of 100 grams and an accuracy of 0.0001. The measurement environment is 25℃ and 35%RH.

[0116] Example 1

[0117] The dry, quick-dissolving facial mask of the present invention is prepared according to the following steps:

[0118] (1) Preparation of spinning solution: Using pure water as solvent, add carboxymethyl chitosan, dextrin, and sodium hyaluronate. Stir in a constant temperature water bath at 20℃-50℃ for 2-6 hours until the solution is uniform and free of particles, to obtain a spinning solution containing the following components: 0.5wt% budding stalk polysaccharide, 12% maltodextrin, 4wt% carboxymethyl chitosan, 2wt% polyethylene glycol, and the remainder pure water. The average molecular weight of the budding stalk polysaccharide used is approximately 1.5-2 M Da, the DE value of the maltodextrin used is less than 5, the average molecular weight of the carboxymethyl chitosan used is 10 KDa-30 KDa, and the average molecular weight of the polyethylene glycol used is approximately 100 KDa-300 KDa.

[0119] (2) Electrospinning: Pour the above-prepared uniform solution into the feed tank of the electrospinning equipment, control the humidity of the spinning environment to be 30%-50%, the spinning distance to be 140mm-220mm, the spinning voltage to be 40KV-85KV, and the spinning speed to be 0.1-1.2 rpm, and perform electrospinning with non-woven fabric as the receiving substrate.

[0120] Example 2

[0121] A dry, instant facial mask was prepared using essentially the same steps and methods as in Example 1, but the spinning solution contained the following components: 0.6 wt% budding stalk polysaccharide, 10 wt% maltodextrin, 4 wt% carboxymethyl chitosan, 1 wt% polyethylene glycol, 0.1 wt% hyaluronic acid, and the balance being purified water. The average molecular weight of the budding stalk polysaccharide used was approximately 300 kDa, the DE value of the maltodextrin was less than 5, the average molecular weight of the carboxymethyl chitosan was 30 kDa, the average molecular weight of the polyethylene glycol was approximately 300 kDa, and the average molecular weight of the hyaluronic acid was between 25 kDa and 50 kDa.

[0122] Example 3

[0123] A dry, instant facial mask was prepared using essentially the same steps and methods as in Example 1, but the spinning solution contained the following components: 1.0 wt% budding stalk polysaccharide, 14 wt% dextrin, 5 wt% carboxymethyl chitosan, 1 wt% polyethylene glycol, 0.3 wt% polyglycerol-10 myristate, and the balance being purified water. The average molecular weight of the budding stalk polysaccharide used was approximately 200 kDa, the DE value of the maltodextrin used was less than 5, the average molecular weight of the carboxymethyl chitosan used was 30 kDa, and the average molecular weight of the polyethylene glycol used was approximately 300 kDa.

[0124] Example 4

[0125] A dry, instant facial mask was prepared using essentially the same steps and methods as in Example 1, but the spinning solution contained the following components: 0.8 wt% budding stalk polysaccharide, 10 wt% dextrin, 2 wt% polyethylene glycol, 6 wt% carboxymethyl chitosan, 0.5 wt% hyaluronic acid, 0.2 wt% sucrose laurate, and the balance being purified water. The average molecular weight of the budding stalk polysaccharide used was approximately 200 kDa, the DE value of the maltodextrin used was less than 5, the average molecular weight of the carboxymethyl chitosan used was 10 kDa, the average molecular weight of the polyethylene glycol used was approximately 300 kDa, and the average molecular weight of the hyaluronic acid used was between 25 kDa and 50 kDa.

[0126] Example 5

[0127] A dry, instant facial mask was prepared using essentially the same steps and methods as in Example 1, but the spinning solution contained the following components: 0.5 wt% budding stalk polysaccharide, 14 wt% dextrin, 1.5 wt% polyethylene glycol, 5 wt% carboxymethyl chitosan, 0.1 wt% hyaluronic acid, 0.3 wt% PEG-20 methyl glucosesquistearate, and the balance being purified water. The average molecular weight of the budding stalk polysaccharide used was approximately 200 kDa, the DE value of the maltodextrin used was less than 5, the average molecular weight of the carboxymethyl chitosan used was 20 kDa, and the average molecular weight of the polyethylene glycol used was approximately 300 kDa.

[0128] Example 6

[0129] The face mask was prepared using essentially the same steps and methods as in Example 1, but the spinning solution contained the following components: 0.5 wt% budding stalk polysaccharide, 12 wt% dextrin, 1.5 wt% polyethylene glycol, 5 wt% carboxymethyl chitosan, 0.1 wt% sodium hyaluronate, 0.3 wt% PEG-20 methyl glucoside sesquistearate, 2% nicotinamide, 2% tranexamic acid, and the balance being purified water. The average molecular weight of the budding stalk polysaccharide used was approximately 200 kDa, the DE value of the maltodextrin used was less than 5, the average molecular weight of the carboxymethyl chitosan used was 20 kDa, and the average molecular weight of the polyethylene glycol used was approximately 300 kDa.

[0130] Example 7

[0131] The dry, instant-dissolving face mask is prepared using the same steps and methods as in Example 1, but with the addition of a protective film layer over the spun layer (nanofiber layer) and the removal of static electricity. The final mask has three layers: a nonwoven fabric base, electrospun fibers spun on this base to form the middle layer (nanofiber layer), and an outer protective film. A product package can contain several masks and may include a nutrient solution container, such as a small sprayer.

[0132] Experimental test on the effect of the dry-state quick-dissolving facial mask of the present invention

[0133] The dry, quick-dissolving facial mask prepared in Example 1 was used to study its soothing and redness-reducing effects on the skin using skin tissue samples.

[0134] This experiment was conducted on human subjects at a CMA-accredited third-party testing institution. Thirty participants with a lactic acid stinging test score greater than 3 or who described themselves as having sensitive skin were recruited. The treatment lasted for 30 days, with the product used every other morning and evening. The erythema index on the skin was measured using VISIA-CR, and the hemoglobin value of the skin was tested using a Mexameter MX 18.

[0135] in, Figure 1 and Figure 3 This shows an experimental example of short-term soothing effects. The lower the Erythema Index (EI) value, the better the skin-soothing effect of the sample. At 15 minutes after use, the difference in EI values ​​between the experimental group and the control group was significantly lower (p<0.001), indicating that the experimental group had a skin-soothing effect, and the soothing effect was significantly better than that of the skin itself.

[0136] Figure 2 and Figure 4 The experiment shown is an example of long-term effects. After 14 days of use, compared with before use, the area of ​​facial erythema was significantly reduced by 4.87% (p<0.001), indicating that it has a significant effect in relieving redness after 14 days. After 28 days of use, compared with before use, the area of ​​facial erythema was significantly reduced by 8.19% (p<0.001), indicating that it has a significant effect in relieving redness after 28 days.

[0137] in, Figure 3 and Figure 4 The significance level is indicated by the following methods: "ns" indicates no statistical difference (p>0.05); "*" indicates a significant difference (p<0.05, 0.01); "**" indicates a significant difference (p<0.01, 0.001); and "***" indicates a significant difference (p<0.001).

Claims

1. A dry, instant-dissolving facial mask primarily composed of carboxymethyl chitosan and maltodextrin, comprising a non-woven fabric substrate layer and a nanofiber layer; wherein, The nanofiber layer is formed on the nonwoven fabric substrate layer using a spinning solution with pure water as a solvent and an electrospinning method. The nanofiber layer comprises: 5-25 parts by weight of carboxymethyl chitosan, 30-70 parts by weight of maltodextrin 2.5-10 parts by weight of high molecular weight polyethylene glycol, 0.5-5 parts by weight of budding short stalk enzyme polysaccharide; The average molecular weight of the carboxymethyl chitosan used is between 3 kDa and 30 kDa. The DE value of the maltodextrin used is between 1 and 10; The average molecular weight of the polyethylene glycol used is between 100 kDa and 500 kDa; The average molecular weight of the budding short stalk enzyme polysaccharide used is between 1 and 2 M Da; The budding short stalk enzyme polysaccharide accounts for 2.5-5% of the total weight of the nanofiber layer.

2. The dry-state instant-dissolving facial mask as described in claim 1, wherein, The carboxymethyl chitosan used contains medium molecular weight carboxymethyl chitosan with a molecular weight of 10 kDa-30 kDa and low molecular weight carboxymethyl chitosan with a molecular weight of 3000-10000 Da, and the mass ratio of medium molecular weight carboxymethyl chitosan to low molecular weight carboxymethyl chitosan is between 1:9 and 9:

1.

3. The dry-state instant-dissolving face mask as described in claim 2, wherein, The mass ratio of medium molecular weight carboxymethyl chitosan to low molecular weight carboxymethyl chitosan used is between 2:1 and 1:

2.

4. The dry-state instant-dissolving facial mask as described in any one of claims 1-3, wherein, The nanofiber layer further comprises 0.1-5 parts by weight of hyaluronic acid, wherein the average molecular weight of the hyaluronic acid is between 5 kDa and 1.5 MDa.

5. The dry-state instant-dissolving facial mask as described in any one of claims 1-3, wherein, The nanofiber layer further comprises 0.5-2.5 parts by weight of a surfactant, wherein the surfactant is at least one selected from the group consisting of: polysorbate-20, polysorbate-60, polysorbate-80, sucrose laurate, sucrose stearate, polyglycerol-10 myristate, polyglycerol-6 caprylate, polyglycerol-6 stearate, coco-glucoside, lauryl glucoside, PEG-40 hydrogenated castor oil, and PEG-20 methyl glucosesquistearate.

6. The dry-state instant-dissolving facial mask as described in any one of claims 1-3, wherein, The nanofiber layer further comprises 0.5-10 parts by weight of functional substances.

7. The dry-state instant-dissolving facial mask as described in any one of claims 1-3, wherein, The nanofiber layer comprises: 15-20 parts by weight of carboxymethyl chitosan 50-60 parts by weight of maltodextrin 2.5-10 parts by weight of high molecular weight polyethylene glycol 2-4 parts by weight of sprouting short stem enzyme polysaccharide 0.5-5 parts by weight of hyaluronic acid.

8. A method for preparing a dry, quick-dissolving facial mask as described in any one of claims 1-7, wherein, The method includes the following steps: (1) Preparation of spinning solution: Using purified water as solvent, add carboxymethyl chitosan, maltodextrin, high molecular weight polyethylene glycol, and budding stalk enzyme polysaccharide, and stir to form a uniform spinning solution. This spinning solution contains 3-6 wt% carboxymethyl chitosan, 10-15 wt% maltodextrin, 0.5-2 wt% polyethylene glycol, and 0.5-1.0 wt% budding stalk enzyme polysaccharide. (2) Electrospinning: The above-prepared spinning solution is added to the electrospinning equipment, and electrospinning is performed using non-woven fabric as the receiving substrate. The average molecular weight of the carboxymethyl chitosan used is between 3 kDa and 30 kDa, the DE value of the maltodextrin used is between 1 and 10, the average molecular weight of the polyethylene glycol used is between 100 kDa and 500 kDa, and the average molecular weight of the budding stalk enzyme polysaccharide used is between 1 and 2 MDa.

9. The method of claim 8, wherein, The spinning solution in step (1) also contains 0.1-1% sodium hyaluronate and / or 0.1-0.5% surfactant, wherein the molecular weight of the hyaluronic acid used is between 5K and 1.5M Da.

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