A nanofiber membrane material with temperature-sensitive controlled release, preparation and application thereof

Abstract

The application discloses a nanofiber membrane material with temperature-sensitive controlled release, and preparation and application thereof. In the application, the nanofiber membrane material comprises a shell layer and a core layer formed by using a coaxial electrospinning technology; the shell layer comprises a polymer material with temperature-sensitive response; the core layer is a skin function material for producing various effects on the skin in the shell layer; and the polymer material with temperature-sensitive response is dissolved or swelled at 35-40 DEG C to release the core layer. Through the special shell-core structure, the active factor can be completely wrapped in the oxygen-light shielding shell layer material before use; when used, the shell layer material is rapidly dissolved or swelled to release the active factor, and the effects of moisturizing, whitening, wrinkle removing and anti-allergy are achieved; and the problems of unstable active ingredient, preservative or stabilizer harmful to the skin in traditional masks can be effectively solved, so the application has a wide application prospect.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of biomaterials. More particularly, it relates to a nanofiber membrane with temperature-sensitive controlled release, preparation and application thereof. BACKGROUND

[0002] In recent years, people pay more and more attention to the field of beauty, especially facial care. Facial mask is a product for facial skin care and beautifying. It is widely recognized in the market due to its convenience and remarkable effect. The existing facial mask usually uses a mask base cloth to carry a beautifying liquid. By directly contacting with the face, the active ingredients in the mask are allowed to enter the stratum corneum of the skin surface, so as to achieve the purposes of moisturizing, whitening, wrinkle removal and anti-allergy. However, the traditional facial mask usually adds some preservatives or stabilizers to protect the stability of the active ingredients. However, the addition of some preservatives or stabilizers may irritate the facial skin and cause safety problems. If no preservatives or stabilizers are used, the active ingredients may be oxidized or degraded before use, thereby reducing their efficacy.

[0003] Later, researchers found that electrospinning technology can be applied to various cosmetics, such as facial mask, eye mask, deodorant, antiperspirant, etc. Their common feature is that they can be used in the form of fiber membrane. Moreover, the ease of incorporating active ingredients into electrospun fibers also makes electrospinning show excellent application prospect in cosmetic applications. Electrospinning can effectively capture them in fibers or their mesh, which can protect these active ingredients to some extent. However, the protection effect of the existing literature is limited. How to increase the stability of active ingredients, reduce their oxidation or degradation, and at the same time avoid the use of emulsifiers, stabilizers, preservatives and other chemicals is a problem to be solved for electrospun facial mask.

[0004] Therefore, there is an urgent need to develop a new type of nanofiber membrane with controlled release effect to effectively solve the problems of unstable active ingredients in facial mask and harm to the skin. SUMMARY

[0005] To solve the above problems, the first object of the present application is to provide a nanofiber membrane with temperature-sensitive controlled release. The nanofiber membrane comprises a shell-core two-layer prepared by coaxial spinning. The shell layer is a polymer material with light and oxygen barrier, and the core layer is a functional polymer material loaded with active factors. Before use, the shell layer completely covers the core layer, which can prevent the oxidation and degradation of the active factors. When used (at 35-40℃ close to human body temperature), the polymer material will dissolve or swell, thereby exposing the inner layer material and releasing the core layer. This reduces the oxidation and degradation of the active factors during the shelf life, thereby achieving the purpose of protecting the active ingredients. At the same time, the addition of preservatives or stabilizers and other safety problems is avoided.

[0006] A second object of the present application is to provide a method for preparing the nanofiber film material as described above.

[0007] A third object of the present application is to provide an application of the nanofiber film material as described above in the field of beauty makeup.

[0008] To achieve the first object described above, the present application adopts the following technical solution:

[0009] The present application discloses a nanofiber film material with temperature-sensitive controlled release, which comprises a shell layer and a core layer formed by using coaxial electrospinning technology.

[0010] The shell layer comprises a polymer material with temperature-sensitive response.

[0011] The core layer is a skin function material for producing various effects on the skin in the shell layer.

[0012] The polymer material with temperature-sensitive response dissolves or swells at 35-40℃, releasing the core layer.

[0013] In traditional masks, active factors for moisturizing, whitening, wrinkle removal, and anti-sensitivity are usually dispersed in mask gel, which is not conducive to the protection of active factors. The mask is prone to oxidation and degradation of active factors during the shelf life, affecting the use effect of the mask. Adding some antioxidant ingredients or preservatives, stabilizers, and other ingredients can protect the active factors to some extent, but also increases the risk of skin damage. In order to protect the active factors and improve the safety of the mask, the inventors designed a nanofiber film material with temperature-sensitive controlled release. The nanofiber film material is prepared by using coaxial electrospinning technology to form a shell and a core. The shell is a polymer material that can block light and oxygen, which can protect the active factors in the core during storage. Specifically, before use, the shell completely covers the core to prevent the active factors from being oxidized by oxygen and degraded by light. When used (at a temperature close to the human body temperature of 35-40℃), the polymer material dissolves or swells, releasing the core. After the release of the core, the active factors act on the skin, only contacting the external environment for a short time, greatly reducing the time of oxidation and degradation of the active factors, achieving the purpose of protecting the active ingredients. At the same time, the nanofiber film material does not contain preservatives or stabilizers and other substances that harm the facial skin, avoiding safety problems during use.

[0014] Further, the polymer material with temperature-sensitive response is a polymer formed by polymerization of acrylamide monomers. Each monomer is polymerized into a dense structure under the action of potassium persulfate or ammonium persulfate, which plays a role in blocking oxygen and shielding light, protecting the substances wrapped in the structure. Preferably, the molecular weight of the polymer is 10 5 -10 6, viscosity 25-250 mPa-s; preferably, the acrylamide monomer includes, but is not limited to, one or a combination of at least two of hydroxymethyl acrylamide, acrylamide, N-isopropyl acrylamide, N-methyl acrylamide, dimethylamino propyl acrylamide. Typical but non-limiting examples of the combination include: a combination of hydroxymethyl acrylamide and acrylamide, a combination of acrylamide and N-isopropyl acrylamide, a combination of acrylamide and N-methyl acrylamide, a combination of hydroxymethyl acrylamide and dimethylamino propyl acrylamide, a combination of hydroxymethyl acrylamide, acrylamide and N-isopropyl acrylamide, a combination of hydroxymethyl acrylamide, acrylamide and N-methyl acrylamide, and the like.

[0015] Further, the skin function material includes a functional polymer material and an active factor loaded on the functional polymer material.

[0016] Further, the functional polymer material is used to load and disperse the active factor, and the functional polymer material includes one or a combination of at least two of gelatin, chitosan, PVP, PVA. Typical but non-limiting examples of the combination include: a combination of gelatin and chitosan, a combination of chitosan and PVP, a combination of gelatin and PVP, a combination of chitosan and PVA, a combination of gelatin, chitosan and PVP, and the like.

[0017] Further, the active factor is used to provide different effects such as moisturizing, whitening, wrinkle removal, and anti-sensitivity, and a person skilled in the art can select the active factor with different effects according to needs. For example, the active factor with moisturizing effect includes, but is not limited to, one or more of xylitol, erythritol, sorbitol, mannitol, panthenol, polyglutamic acid, betaine, aloe extract, hydroxyethyl urea; the active factor with whitening effect includes, but is not limited to, one or more of arbutin, vitamin C, sodium ascorbyl phosphate, magnesium ascorbyl phosphate, ascorbyl glucoside, 3-O-ethoxy ascorbic acid, ascorbyl palmitate, ascorbyl tetraisopalmitate, kojic acid, kojic acid palmitate, fruit acid, malic acid, tartaric acid, citric acid; one or more of daisy extract, nicotinamide, tranexamic acid, ferulic acid hexyl acetate; the active factor with wrinkle removal effect includes, but is not limited to, one or more of vitamin E, sodium tocopheryl phosphate, ubiquinone, grape seed extract, tea extract, vitamin A, vitamin A acetate, ginkgo extract, resveratrol, ceramide, ginseng root extract, puerarin, soy isoflavones; the active factor with anti-sensitivity effect includes, but is not limited to, one or more of dipotassium glycyrrhizinate, allantoin, α-bisabolol, salvia miltiorrhiza root extract, matrine, spilanthes extract, vitamin B2, vitamin B6, vitamin B6 dipalmitate, azelaic acid, baicalin.

[0018] It should be pointed out that, through the research of the inventor, at least one unstable and easily oxidizable functional ingredient can be added in the nanofiber membrane without adding preservatives or stabilizers, and the structure and state of the functional ingredient can be maintained, avoiding oxidation and degradation, the unstable and easily oxidizable functional ingredient is selected from the four active factors of the above-mentioned four functions, including but not limited to one or more of vitamin C, vitamin B2, vitamin E, pyridoxine dipalmitate, kojic acid palmitate, sodium ascorbate phosphate, magnesium ascorbate phosphate, ascorbic acid glucoside, 3-O-ethoxy ascorbic acid, ascorbic acid palmitate, ascorbic acid tetraisopropyl palmitate, vitamin A, vitamin A acetate, ginkgo biloba extract, resveratrol, ceramide, ginseng root extract, puerarin, riboflavin, vitamin B6, vitamin B6 dipalmitate.

[0019] To achieve the above-mentioned second object, the application adopts the following technical scheme:

[0020] The application discloses a method for preparing the nanofiber membrane, comprising the following steps:

[0021] S1, preparing a shell layer spinning precursor solution:

[0022] Under the protection of nitrogen, the monomers of the polymer material and ultrapure water are added to a three-necked flask for mixing, then a persulfate solution is added for polymerization reaction, after the reaction is completed, dialysis is performed for 50-100h, the water is replaced every 10h, and the polymer material is obtained by freeze-drying, then the polymer material is added to N,N-dimethylformamide to prepare the shell layer spinning precursor solution;

[0023] S2, preparing a core layer spinning precursor solution:

[0024] The functional polymer material is added to ultrapure water, and then the active factor is added to prepare the core layer spinning precursor solution;

[0025] S3, preparing a nanofiber membrane with temperature-sensitive controlled release:

[0026] The shell layer spinning precursor solution of step S1 and the core layer spinning precursor solution of step S2 are subjected to coaxial electrospinning, then are cut into different specifications, are sterilized by electron beam irradiation, and are vacuum packaged to obtain the nanofiber membrane with a shell-core structure.

[0027] Further, in step S1, the mass-volume ratio of the monomers of the polymer material to ultrapure water is 1-2g:6-12ml.

[0028] Further, the persulfate salt is selected from potassium persulfate or ammonium persulfate, and the mass ratio of the monomer to the persulfate salt is 1:0.05-0.4; for example, the mass ratio of the monomer to the persulfate salt is 1:0.05, 1:0.1, 1:0.15, 1:0.2, 1:0.25, 1:0.30, 1:0.35, 1:0.4, and the like.

[0029] Further, in step S1, the polymer material in the shell layer spinning precursor solution accounts for 10-30% of the mass percentage; preferably, the polymer material in the shell layer spinning precursor solution accounts for 10-20% of the mass percentage.

[0030] Further, in step S1, the polymer material in the shell layer spinning precursor solution accounts for 10-30% of the mass percentage; preferably, the polymer material in the shell layer spinning precursor solution accounts for 10-20% of the mass percentage.

[0031] Further, in step S2, the functional polymer material in the core layer spinning precursor solution accounts for 10-40% of the mass percentage, the active factor accounts for 0.5-1% of the mass percentage, and the rest is ultrapure water; preferably, the functional polymer material in the core layer spinning precursor solution accounts for 10-20% of the mass percentage, the active factor accounts for 0.5-1% of the mass percentage, and the rest is ultrapure water.

[0032] Further, in the coaxial electrospinning, the temperature of the shell layer spinning precursor solution and the core layer spinning precursor solution is 45℃, the environmental temperature is 20-26℃, the environmental humidity is 20-40%, the spinning voltage is 20-100KV, the current is 0.2-1.5mA, the spinning distance is 40-120cm, and the spinning speed is 0.1-0.2RPM.

[0033] To achieve the third object, the application discloses an application of the nanofiber membrane material in the field of beauty care, which is used for preparing a facial mask, an eye mask, a neck mask, a marionette line mask, a cheek wrinkle mask, or a forehead line mask.

[0034] The application has the following advantages:

[0035] The application discloses a nanofiber membrane material with temperature-sensitive controlled release, and preparation and application thereof.

[0036] 1. The nanofiber membrane material with a shell-core structure is prepared by the coaxial electrospinning technology, and under the joint action of the temperature-sensitive polymer material, the active ingredients such as moisturizing, whitening, wrinkle removal, and anti-allergy are effectively protected from oxidation or degradation, and meanwhile, the safety problem caused by the introduction of preservatives or stabilizers and the like is solved, and the safety is obviously improved.

[0037] 2. The polymer material selected is an acrylamide polymer that can dissolve or swell at temperatures close to human body temperature. This polymer has excellent temperature responsiveness. It does not dissolve or swell at low temperatures, but it can dissolve at 35-40℃, allowing the core layer to be released and achieving controlled release of active factors.

[0038] 3. The raw materials used in this invention have low toxicity and high safety, and the various functional polymer materials and active factors work together to have a good regulatory effect on the skin.

[0039] 4. Due to the protection of the shell-core structure and polymer materials, the added active factors can be fully released with minimal loss, which is beneficial for achieving the purposes of moisturizing, whitening, wrinkle removal, and anti-allergy. Attached Figure Description

[0040] The specific embodiments of the present invention will be described in further detail below with reference to the accompanying drawings.

[0041] Figure 1 The microstructure of the sample prepared in Example 1 is shown in comparison at 25 and 37 °C.

[0042] Figure 2 The amount of vitamin B2 released over time from the sample prepared in Example 1 at 25 and 37°C is shown.

[0043] Figure 3 The release of kojic acid palmitate over time is shown for the sample prepared in Example 1 at 25 and 37°C.

[0044] Figure 4 The release amounts of vitamin B2 and kojic acid palmitate over time are shown for the sample prepared in Comparative Example 1 at 25°C. Detailed Implementation

[0045] To more clearly illustrate the present invention, the following description, in conjunction with preferred embodiments and accompanying drawings, further explains the invention. Similar components in the drawings are indicated by the same reference numerals. Those skilled in the art should understand that the specific description below is illustrative rather than restrictive and should not be construed as limiting the scope of protection of the present invention.

[0046] Example

[0047] The experimental steps are as follows:

[0048] S1, Shell spinning precursor solution:

[0049] 6 g of hydroxymethyl acrylamide, 2 g of acrylamide, and 2 g of N-isopropyl acrylamide were added into a three-necked flask, 60 ml of ultrapure water was added under the protection of nitrogen; then 1 g of potassium persulfate was dissolved in ultrapure water and added into the flask, and the reaction was carried out at 0℃ for 3 hours and at 35℃ for 8 hours. The reaction solution was dialyzed against ultrapure water for 72 hours, and the water was changed every 10 hours. The polymer material was obtained by freeze-drying for 3 days using a freeze dryer. The prepared polymer material was added into N,N-dimethylformamide to prepare a 15 wt% shell spinning precursor solution;

[0050] S2, core layer spinning precursor solution:

[0051] Gelatin and PVP were added into ultrapure water at a mass ratio of 1:2, and then active factors were added (the components and contents are shown in Table 1) to prepare a core layer spinning precursor solution, with the mass percentage of active factors being 1% and the mass percentage of functional polymer material being 20%;

[0052] S3, preparation of nanofiber membrane material with temperature-sensitive controlled release:

[0053] The shell spinning precursor solution of step S1 and the core layer spinning precursor solution of step S2 were subjected to coaxial electrospinning, with the temperature of the shell spinning precursor solution and the core layer spinning precursor solution being 45℃, the environmental temperature being 25℃, the environmental humidity being 35%, the voltage being 20KV, the current being 1.0 mA, the spinning distance being 120 cm, and the spinning speed being 0.2 RPM. After cutting, electron beam irradiation sterilization (irradiation dose being 15 KGy), and vacuum packaging, a nanofiber membrane material with a shell-core structure was prepared.

[0054] Comparative example

[0055] The experimental steps are as follows:

[0056] S1, spinning precursor solution:

[0057] Gelatin and PVP were added into ultrapure water at a mass ratio of 1:2, and then active factors were added (the components and contents are shown in Table 1) to prepare a core layer spinning precursor solution, with the mass percentage of active factors being 1% and the mass percentage of functional polymer material being 20%;

[0058] S2, preparation of nanofiber membrane material:

[0059] The spinning precursor solution of step S1 was subjected to coaxial electrospinning, with the temperature of the shell spinning precursor solution and the core layer spinning precursor solution being 45℃, the environmental temperature being 25℃, the environmental humidity being 35%, the voltage being 20KV, the current being 1.0 mA, the spinning distance being 120 cm, and the spinning speed being 0.2 RPM. After cutting, electron beam irradiation sterilization (irradiation dose being 15 KGy), and vacuum packaging, a nanofiber membrane material was prepared.

[0060] The types and contents of active ingredients in Examples 1-4 and Comparative Examples 1-4 are shown in Table 1:

[0061] Table 1. List of active ingredients in Examples 1-4 and Comparative Examples 1-4

[0062]

[0063]

[0064] Test case

[0065] 1. Drug release test

[0066] The nanofiber membranes prepared in Example 1 and Comparative Example 1 were selected as test samples. 1 g of each sample was accurately weighed and placed in a container containing 50 mL of PBS buffer (pH = 7.4, 0.02 M). The container was placed in a constant-temperature shaker at 25°C and 37°C, respectively, at a speed of 60 rpm. At 1 min, 3 min, 5 min, 7 min, 9 min, 11 min, 13 min, 15 min, 20 min, 25 min, and 30 min, 5 mL of the solution was accurately measured, centrifuged, and the supernatant was collected. The absorbance at 254 nm (characteristic UV absorption peak of kojic acid palmitate) and 475 nm (characteristic UV absorption peak of vitamin B2) was measured. Electron micrographs of the sample from Example 1 were obtained at 25°C and 37°C, and curves showing the relationship between drug release degree and time at 25°C and 37°C were plotted. The results are shown in [Figure 1]. Figures 1-4 .

[0067] from Figure 1 It can be seen that at 25℃, the fibers are smooth and flat, but when the temperature rises to 37℃, wrinkles appear on the fiber surface. From Figure 2 and Figure 3 As can be seen, the sample prepared in Example 1 showed almost no release behavior at room temperature (25°C), indicating that the active ingredient can be well protected by the shell during the shelf life. When the temperature was raised to 37°C, there was a significant slow-release behavior, indicating that the shell material has excellent temperature responsiveness. Furthermore, from... Figure 4 The test results of Comparative Example 1 show that without shell protection, the active ingredient will be released quickly at 25°C. This means that the active ingredient will be exposed to the external environment earlier during its shelf life, which will cause oxidation and degradation of the active ingredient.

[0068] 2.1 Whitening Effect Evaluation Experiment

[0069] Tyrosinase is the main rate-limiting enzyme in the process of melanin formation. The higher the inhibitory activity of tyrosinase, the better the skin whitening effect.

[0070] Reagent preparation:

[0071] Preparation of phosphate buffer solution (PBS): Take 50 ml of 0.1 mol / L potassium dihydrogen phosphate, add 29 ml of 0.1 mol / L potassium hydroxide solution, and add water to make the total volume of the mixed solution 100 ml to obtain a PBS solution with pH 7.0.

[0072] Preparation of tyrosinase solution: Take 5.2 mg of tyrosinase, and prepare a tyrosinase solution with a concentration of 250 u / mL using PBS (pH = 7.0).

[0073] Preparation of L-Dopa solution: Accurately take 100 mg of L-Dopa, and prepare an L-Dopa solution with a mass fraction of 0.1% by dissolving in PBS (pH = 7.0) to a volume of 100 mL.

[0074] Preparation of test group solution: Take 100 mg of the sample of Example 2 and Comparative Example 2, respectively, and prepare a solution by dissolving in PBS to a volume of 10 mL, mixing, filtering, and collecting the filtrate.

[0075] Measurement of tyrosinase activity: Take a 48-well enzyme-linked plate, add 50 μL of tyrosinase solution (12.5 u) to each well, then add 250 μL of test group solution, respectively, and incubate at 37°C for 10 min, add 500 μL of 0.1% DL-dopa, and continue to incubate at 37°C for 5 min, measure the absorbance at 490 nm, repeat the above operation three times, and take the average value. The inhibition rate of tyrosinase is calculated according to the following formula,

[0076] Tyrosinase inhibition rate = {[(A-B)-(C-D)] / (A-B)} x 100%,

[0077] wherein A: 250 μL of buffer and 50 μL of tyrosinase are added, B: only 300 μL of buffer is added, C: 250 μL of test group solution and 50 μL of tyrosinase are added, and D: 250 μL of test group solution and 50 μL of buffer are added. The results are shown in Table 2:

[0078] Table 2 Comparison of tyrosinase inhibition rate data of Example 2 and Comparative Example 2

[0079] Group Inhibition rate of tyrosinase / % Example 2 94％ Comparative Example 2 85％

[0080] The results show that the sample of Example 2 has higher inhibitory activity on tyrosinase than Comparative Example 2, and has better whitening effect on the skin.

[0081] 2.2 Evaluation test of whitening and moisturizing effect

[0082] Test subjects: 20 volunteers with different degrees of facial skin dryness, fine lines, and dull complexion, with an average age of 20-40 years old, were recruited and divided into two groups for parallel testing. Test group 1 used the facial mask prepared in Example 2, and test group 2 used the facial mask prepared in Comparative Example 2.

[0083] Test method: The use mode was once in the morning and once in the evening, and the continuous use was 30 days. The whitening and moisturizing conditions were evaluated on the 15th day and the 30th day, respectively.

[0084] Evaluation criteria: The subjects scored between 0 and 10, and the average score of 10 people in each group was taken. No change in skin condition was 0 points, and the skin was significantly whitened (whitening condition), the fine lines were significantly reduced, and the skin was significantly fine (moisturizing condition) were 10 points.

[0085] The test results are shown in Table 3:

[0086] Table 3: Whitening and moisturizing effect evaluation test summary table

[0087]

[0088] As can be seen from the above, the facial mask can quickly whiten the skin, achieve good whitening and moisturizing effects in 15 days, and achieve obvious penetration effects in 30 days, so that the skin is moisturized and whitened for a long time.

[0089] 3. Skin wrinkle removal effect evaluation

[0090] Test subjects: 20 volunteers with an average age of 20-40 years old were recruited and divided into two groups for parallel testing. Experimental group 1 used the facial mask prepared in Example 3, and experimental group 2 used the facial mask prepared in Comparative Example 3.

[0091] Test method: The use mode was once in the morning and once in the evening, and the continuous use was 30 days. Then, a model of silicon material was made, and the visibility tester of the image analyzer was used to determine the wrinkle state of the specified part. The results are shown in Table 4, and the numerical value of each parameter is the average of the parameter value after 30 days minus the parameter value before 30 days.

[0092] Evaluation criteria:

[0093] R1: The difference value between the maximum value and the minimum value of the wrinkle contour line;

[0094] R2: The wrinkle contour line is arbitrarily divided into 5 parts, and R1 is the average of the 5 parts;

[0095] R3: The highest value of R1 in every 5 parts;

[0096] R4: The average value of the peak top and valley bottom value is subtracted from the baseline of the wrinkle contour line;

[0097] R5: Average of the values obtained by subtracting the baseline of the wrinkle contour from each wrinkle profile;

[0098] Explanation: The more negative the result, the better the wrinkle improvement effect.

[0099] Table 4 Summary of Skin Wrinkle Removal Effect Evaluation

[0100] Group R1 R2 R3 R4 R5 Experimental Group 1 -0.24 -0.18 -0.09 -0.08 -0.06 Experimental Group 2 -0.18 -0.15 -0.06 -0.05 -0.04

[0101] The results show that Example 3 has a better wrinkle removal effect than Comparative Example 3.

[0102] 4.1 Anti-allergic efficacy evaluation test

[0103] When the body has an allergic disease or inflammation, histamine, a chemical transmitter substance in mast cells, plays an important role. By determining the concentration of histamine, the anti-allergic effect of the sample can be evaluated. Studies have shown that the higher the hyaluronidase activity, the higher the amount of histamine released, and there is a good correlation between the inhibition of hyaluronidase activity and the inhibition of mast cell release of histamine.

[0104] Solution preparation:

[0105] Acetic acid buffer solution: Prepare 5.0 ml of 0.2M aqueous acetic acid as A solution; prepare 50.0 mL of 0.3M as B solution; mix A and B solutions, and dilute to 100 mL.

[0106] Hyaluronidase solution: weigh 10 mg of hyaluronidase into a beaker, add 4 mL of acetic acid buffer solution.

[0107] Sodium hyaluronate solution: weigh 5 mg of sodium hyaluronate into a beaker, add 10 mL of acetic acid buffer solution.

[0108] Ehrlich's reagent: weigh 0.8 g of p-dimethylaminobenzaldehyde, dissolve in 15 mL of concentrated hydrochloric acid and 15 mL of anhydrous ethanol.

[0109] Acetylacetone solution: take 3.5 mL of acetylacetone, dissolve in 50 mL of 1.0 mol / L sodium carbonate solution.

[0110] The nanofiber membrane of 10 mg of Example 4 and Comparative Example 4 was weighed accurately and placed in a sample tube, 1 mL of ultrapure water was added to prepare a mask liquid sample. 0.1 mL of 0.25 mM CaCl2 solution was taken, 0.5 mL of hyaluronidase solution was added, and incubated at 37°C for 20 min. 0.5 mL of the mask liquid sample of Example 4 and Comparative Example 4 was added to the test tube, and incubated at 37°C for 20 min. Then 0.5 mL of sodium hyaluronate solution was added, and incubated at 37°C for 30 min. After standing at room temperature for 5 min, 0.1 mL of 0.4M NaOH solution and 0.5 mL of acetylacetone solution were added, and reacted at 100°C for 15 min, and then immediately added to an ice bath for 5 min. 1.0 mL of Ehrlich reagent was taken, and diluted with 3.0 mL of anhydrous ethanol, and color developed for 20 min, during which the wavelength was scanned in the range of 450-700 nm to determine the maximum absorption wavelength, and the absorbance value was measured at the maximum absorption wavelength by spectrophotometry.

[0111] Inhibition rate of hyaluronidase (%) = ((A-B)-(C-D)) / (A-B) x 100%;

[0112] Wherein, A: OD value measured by the control solution; B: OD value measured by the control blank solution; C: OD value measured by the test substance; D: OD value of the test sample blank, and the test results are shown in Table 5.

[0113] Table 5 Test results of anti-sensitivity efficacy evaluation test

[0114] Sample Hyaluronidase inhibition rate / % Example 4 94.3％ Comparative Example 4 80.4％

[0115] As can be seen from Table 5, the hyaluronidase inhibition rate of the temperature-sensitive controlled-release nanofiber membrane loaded with the anti-sensitivity active factor of the present application is more than 90%, indicating that the mask has a good inhibitory effect on hyaluronidase.

[0116] 4.2 Anti-sensitivity effect test

[0117] Test object: 20 volunteers with sensitive skin (visible sensitive symptoms on the face) with an average age of 20-40 years were recruited and divided into two groups for parallel testing. The experimental group 1 used the mask prepared in Example 4, and the experimental group 2 used the mask prepared in Comparative Example 4.

[0118] Test method: The skin of the subjects is measured before and after use, and a one-month product trial human efficacy evaluation test is conducted. Before use, wash the face, soak the prepared mask in warm water for 30 seconds, and then apply it to the face for 30 minutes. Once a day in the morning and evening. Before the test, the subjects need to use the Antera 3D instrument to measure and analyze the redness of the skin of the respondents' face (skin hemoglobin content), the water content of the skin stratum corneum, and the trans-epidermal water loss rate of the skin, and the results are shown in Table 6.

[0119] Explanation: The significant increase in the test value of the water content of the skin stratum corneum indicates that the water content of the skin stratum corneum of the subjects is significantly improved, and has a moisturizing effect; the significant decrease in the test value of the trans-epidermal water loss rate of the skin indicates that the water retention capacity of the skin of the subjects is significantly improved, and the skin barrier function is significantly improved, and has a repairing effect; the significant decrease in the test value of the skin hemoglobin content indicates that the hemoglobin content of the skin of the subjects is significantly reduced, and has a soothing effect.

[0120] Table 6 Skin change ratio test data before and after use

[0121] Group Skin hematin content Stratum corneum moisture content Trans-epidermal water loss rate Experimental Group 1 87％ 89％ 93％ Experimental Group 2 40％ 55％ 46％

[0122] The test results show that the change ratio of the skin hemoglobin content, the water content of the skin stratum corneum, and the trans-epidermal water loss rate of the skin of the subjects in the experimental group 1 is greater than that of the experimental group 2 before the sample trial, indicating that the mask loaded with the anti-allergic factor of the present application can improve the ability of transdermal absorption, quickly repair damaged skin, and thus better play a role in soothing and calming the skin.

[0123] Obviously, the above embodiments of the present application are only examples for clearly illustrating the present application, and are not a limitation on the embodiments of the present application. For those skilled in the art, other different forms of changes or variations can be made on the basis of the above description, and it is impossible to enumerate all the embodiments here. Any obvious changes or variations derived from the technical solutions of the present application still fall within the protection scope of the present application.

Claims

1. A nanofiber membrane material with temperature-sensitive controlled release, characterized in that, The nanofiber membrane material comprises a shell layer and a core layer formed by using a coaxial electrospinning technology; The shell layer comprises a polymer material with a temperature-sensitive response; The core layer is a skin function material in the shell layer for producing various effects on the skin; The polymer material with a temperature-sensitive response dissolves or swells at 35-40 DEG C to release the core layer; The polymer material with temperature-sensitive response is a polymer formed by polymerization of acrylamide monomers; the molecular weight of the polymer is 10 5 -10 6 , and the viscosity is 25-250 mPa·s; the acrylamide monomers include one or more of hydroxymethyl acrylamide, acrylamide, N-isopropyl acrylamide, N-methyl acrylamide, and dimethylamino propyl acrylamide. The nanofiber membrane material is prepared by the following method: S1, preparing a shell layer spinning precursor solution: Under nitrogen protection, monomers of a polymer material are mixed with ultrapure water, and then a persulfate solution is added for polymerization reaction, after which the reaction is dialyzed for 50-100 hours, and the polymer material is obtained by freeze-drying, and then the polymer material is added to N, N-dimethylformamide to prepare the shell layer spinning precursor solution; S2, preparing a core layer spinning precursor solution: A functional polymer material is added to ultrapure water, and then an active factor is added to prepare the core layer spinning precursor solution; S3, preparing a nanofiber membrane material with temperature-sensitive controlled release: The shell layer spinning precursor solution of step S1 and the core layer spinning precursor solution of step S2 are subjected to coaxial electrospinning, and then the nanofiber membrane material with a shell-core structure is prepared after cutting, irradiation sterilization, and vacuum packaging.

2. The nanofiber material of claim 1, wherein, The skin function material comprises a functional polymer material and an active factor loaded on the functional polymer material.

3. The nanofiber material of claim 2, wherein, The functional polymer material comprises one or more of gelatin, chitosan, PVP, and PVA.

4. The nanofiber material of claim 2, wherein, The active factor comprises at least one unstable and easily oxidized functional ingredient.

5. The nanofiber material of claim 4, wherein, The functional ingredient comprises one or more of vitamin C, vitamin B2, vitamin E, pyridoxine dipalmitate, kojic acid palmitate, sodium ascorbyl phosphate, magnesium ascorbyl phosphate, ascorbic acid glucoside, 3-O-ethoxy ascorbic acid, ascorbic acid palmitate, ascorbic acid tetraisopalmitate, vitamin A, vitamin A acetate, ginkgo extract, resveratrol, ceramide, ginseng root extract, puerarin, riboflavin, vitamin B6, and vitamin B6 dipalmitate.

6. A method of producing the nanofiber film material according to any one of claims 1 to 5, characterized by, The method comprises the following steps: S1, preparing a shell layer spinning precursor solution: Under nitrogen protection, monomers of a polymer material are mixed with ultrapure water, and then a persulfate solution is added for polymerization reaction, after which the reaction is dialyzed for 50-100 hours, and the polymer material is obtained by freeze-drying, and then the polymer material is added to N, N-dimethylformamide to prepare the shell layer spinning precursor solution; S2, preparing a core layer spinning precursor solution: A functional polymer material is added to ultrapure water, and then an active factor is added to prepare the core layer spinning precursor solution; S3, preparing a nanofiber membrane material with temperature-sensitive controlled release: The shell layer spinning precursor solution of step S1 and the core layer spinning precursor solution of step S2 are subjected to coaxial electrospinning, and then the nanofiber membrane material with a shell-core structure is prepared after cutting, irradiation sterilization, and vacuum packaging.

7. The production method according to claim 6, characterized by, In step S1, the mass-to-volume ratio of the monomers of the polymer material to ultrapure water is 1-2 g:6-12 ml.

8. The preparation method according to claim 6, characterized in that, The persulfate is selected from potassium persulfate or ammonium persulfate, and the mass ratio of the monomers to the persulfate is 1:0.05-0.

4.

9. The preparation method according to claim 6, characterized in that, In step S1, the polymerization reaction is first carried out at 0℃ for 1-5h, and then at 25-40℃ for 7-10h.

10. The method of claim 6, wherein, In step S1, the mass percentage of the polymer material in the shell spinning precursor solution is 10-30%.

11. The preparation method according to claim 6, characterized in that, The mass percentage of the polymer material in the shell spinning precursor solution is 10-20%.

12. The method of claim 6, wherein, In step S2, the mass percentage of the functional polymer material in the core spinning precursor solution is 10-40%, the mass percentage of the active factor is 0.5-1%, and the rest is ultrapure water.

13. The method of claim 6, wherein, The mass percentage of the functional polymer material in the core spinning precursor solution is 10-20%, the mass percentage of the active factor is 0.5-1%, and the rest is ultrapure water.

14. The method of claim 6, wherein, In the coaxial electrospinning, the temperature of the shell spinning precursor solution and the core spinning precursor solution is 45℃, the environmental temperature is 20-26℃, the environmental humidity is 20-40%, the spinning voltage is 20-100KV, the current is 0.2-1.5mA, the spinning distance is 40-120cm, and the spinning speed is 0.1-0.2RPM.

15. The method of claim 6, wherein the method further comprises, The irradiation dose is 10-15KGy.

16. Use of the nanofiber film material according to any one of claims 1 to 5 in the field of cosmetics, characterized in that, The nanofiber membrane material is used for preparing a facial mask, an eye mask, a neck mask, a marionette line mask, a cheek line mask, or a forehead line mask.

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