An antioxidant electrospun face mask cloth and a preparation method thereof

Abstract

The application discloses an antioxidant electrostatic spinning mask cloth and a preparation method thereof, and belongs to the technical field of electrostatic spinning nanofiber membrane materials. The method comprises the following steps: (1) washing cuttle ink sacs, collecting cuttle ink, adding deionized water, mixing and stirring for 4-8 hours, centrifugally collecting melanin precipitates, and then freezing and drying after washing to obtain cuttle melanin particles, wherein the average particle size of the cuttle melanin particles is 100-200 nm; (2) dissolving collagen peptide, the cuttle melanin particles prepared in step (1) and polyvinyl alcohol in an acetic acid solution, ultrasonically homogenizing to obtain a spinning liquid, and then performing electrostatic spinning on the spinning liquid, and finally vacuum drying to obtain the antioxidant electrostatic spinning mask cloth. The method is simple in process, and the prepared product, the mask cloth, is excellent in mechanical properties, and good in moisturizing and antioxidant effects.

Description

Technical Field

[0001] This invention belongs to the field of electrospun nanofiber membrane material technology, specifically relating to an antioxidant electrospun facial mask fabric and its preparation method. Background Technology

[0002] Facial masks are a widely used personal care product. Currently, the most common type on the market is still the traditional sheet mask, whose mask sheet is often a simple carrier material without functional properties, such as non-woven fabric, natural cellulose fibers, or pectin fibers. Electrospinning technology can be used to produce fiber mask products. Electrospinned nanofiber membranes have excellent adsorption and breathability, a large specific surface area, and high porosity, allowing active ingredients to be introduced into the mask. They also have excellent fit and biocompatibility. Existing nanofiber masks include slow-release nanofiber masks and quick-dissolving nanofiber masks. Slow-release nanofiber masks gradually release their active ingredients upon contact with moist skin, while the nanofibers in quick-dissolving nanofiber masks completely dissolve in the skin.

[0003] Chinese patent document CN116077350A discloses an electrospun composite nanofiber membrane with a sandwich structure, including an adhesive layer, a functional layer, and a flexible breathable layer. The adhesive layer is a biocompatible electrospun polyvinyl alcohol / sodium hyaluronate nanofiber membrane, the functional layer is a nanofiber membrane containing chitosan, hyaluronic acid salts and their derivatives, and collagen peptides, and the flexible breathable layer is an ultrathin thermoplastic polyurethane nanofiber membrane. This membrane is no longer just a carrier, but can dissolve on its own to act as an essence, successfully integrating the mask sheet and essence. However, its preparation method is relatively complicated and has high requirements for the process.

[0004] Chinese patent document CN112587443A discloses a method for preparing a moisturizing nanofiber facial mask. The invention involves slowly adding polyvinyl alcohol and hyaluronic acid to a certain volume of water under stirring, heating and stirring until completely dissolved, then stopping stirring to obtain a spinning solution. At least one active substance with moisturizing properties is added to the spinning solution, and the mixture is stirred evenly to obtain a mixed spinning solution. This spinning solution is then electrospun and collected using a collection device to obtain a moisturizing nanofiber facial mask. The moisturizing active substance is selected from niacinamide, vitamin B5, polylysine, etc. The nanofibers in this facial mask dissolve in water and can form a nutrient-rich liquid sol film on the surface of the mask paper. However, this invention does not investigate the strength of the bonding force between the mask paper and the electrospun nanofibers.

[0005] Cuttlefish ink, a traditional Chinese medicine, is a suspension stored in the ink sac of cuttlefish. It contains various active substances, among which cuttlefish melanin granules have been found to possess anti-inflammatory, antibacterial, and anti-radiation pharmacological effects, giving it high medicinal value. However, the uneven size and poor solubility of the cuttlefish ink melanin granules affect its further use. Current research reports on cuttlefish ink melanin extraction processes mainly include high-speed centrifugation and water washing, concentrated hydrochloric acid washing, and enzymatic hydrolysis. In existing technologies, there are few reports of incorporating cuttlefish ink into functional facial mask sheets. Summary of the Invention

[0006] This invention provides a method for preparing an antioxidant electrospun facial mask fabric. The process is simple, and the resulting facial mask fabric has excellent mechanical properties, as well as good moisturizing and antioxidant effects.

[0007] The specific technical solution adopted is as follows:

[0008] A method for preparing an antioxidant electrospun facial mask fabric includes the following steps:

[0009] (1) Wash the squid ink sac, collect the squid ink, add deionized water and mix for 4-8 hours, centrifuge to collect the melanin precipitate, wash and freeze dry to obtain squid melanin particles, the average particle size of the squid melanin particles is 100-200nm.

[0010] (2) Collagen peptides, cuttlefish melanin particles obtained in step (1) and polyvinyl alcohol are dissolved in acetic acid solution, and ultrasonically homogenized to obtain spinning solution. After electrospinning using spinning solution, vacuum drying is performed to obtain the antioxidant electrospun mask cloth.

[0011] The method for extracting squid melanin particles in this invention is easy to operate and has a simple process. The obtained squid melanin particles have a relatively uniform particle size and contain a large number of active hydroxyl and amino groups on their surface. When introduced into a specific acetic acid solution system, they are combined with collagen peptides and polyvinyl alcohol to prepare an antioxidant electrospun facial mask fabric through electrospinning. First, the spinning solution has good dispersibility and uniformity, which facilitates the electrospinning operation. Second, the squid melanin particles and collagen peptides work together to have a synergistic effect, which can improve the mechanical properties of the facial mask fabric and further achieve the dual effects of moisturizing and anti-oxidation.

[0012] Preferably, in step (1), the centrifugation parameters are 8000-10000 rpm and 15-20 min. Under these parameters, the uniformity and dispersion of the squid melanin particles obtained are better.

[0013] Preferably, in step (1), the cleaning process involves ultrasonic cleaning with an ethanol aqueous solution for 3-5 times, followed by cleaning with deionized water; more preferably, the ultrasonic power is 200-400W and the ultrasonic time is 10-30min.

[0014] Preferably, the collagen peptides have a number average molecular weight of 1000-2000. Collagen peptides with corresponding molecular weights are generally obtained by enzymatic hydrolysis of collagen, have excellent water retention capacity, and can increase cell activity.

[0015] Preferably, in the spinning solution, the mass fraction of collagen peptides is 10-40 wt%, the mass fraction of squid melanin particles is 0.5-2 wt%, and the mass fraction of polyvinyl alcohol is 5-30 wt%.

[0016] More preferably, in the spinning solution, the mass fraction of collagen peptides is 30-35 wt%, the mass fraction of squid melanin particles is 1-1.2 wt%, and the mass fraction of polyvinyl alcohol is 5-15 wt%. Experiments have shown that under the above parameters, the resulting antioxidant electrospun facial mask fabric has an elastic modulus > 40 MPa, tensile strength > 0.5 MPa, elongation at break > 5%, and exhibits excellent antioxidant and moisturizing properties.

[0017] Preferably, the parameters for the electrospinning process are: voltage of 15-30kV; needle size of 16-22G; distance between the needle and the receiving platform of 5-15cm; and propulsion rate of the pusher of 1-5mL / h.

[0018] Preferably, in step (2), the parameters for ultrasonic homogenization are: ultrasonic power of 50-200W and time of 5-15min.

[0019] This invention also provides an antioxidant electrospun facial mask fabric prepared by the aforementioned method. When this antioxidant electrospun facial mask fabric comes into contact with moist skin, the nanofibers gradually dissolve, providing a moisturizing effect, further increasing skin elasticity, and achieving an antioxidant effect.

[0020] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0021] (1) The present invention uses a specific extraction method to obtain squid melanin particles with uniform particle size and a large number of active hydroxyl and amino groups on the surface. These particles are introduced into a specific acetic acid solution system and electrospun with collagen peptides and polyvinyl alcohol to prepare an antioxidant electrospun mask cloth. The squid melanin particles have good binding force with collagen peptides and polyvinyl alcohol, and the squid melanin particles and collagen peptides work together to have a synergistic effect, which can improve the mechanical properties of the mask cloth and further achieve the dual effects of moisturizing and anti-oxidation.

[0022] (2) The preparation route of the antioxidant electrospun mask cloth provided by the present invention is simple, does not use any additives, the raw materials are easy to obtain, and it is easy to industrialize. Attached Figure Description

[0023] Figure 1 This is a TEM image of the squid melanin particles obtained in Example 1. Detailed Implementation

[0024] The technical solution of the present invention will be further illustrated below through specific embodiments. Those skilled in the art should understand that the embodiments described are merely illustrative of the present invention and should not be construed as limiting the invention in any way.

[0025] Unless otherwise specified in the following examples and comparative examples, all techniques or conditions described in the literature in this field, or in accordance with the product instructions, shall be performed. Reagents or instruments whose manufacturers are not specified are all conventional products that can be purchased through legitimate channels or prepared using existing techniques.

[0026] The collagen peptides used in the examples and comparative examples were purchased from the German company, Galida Group, with a number average molecular weight of 1000-2000. Cuttlefish ink sacs were purchased from Dalian Ximei Food Trading Co., Ltd.

[0027] Example 1

[0028] The squid ink sac was washed clean, the squid ink was collected, deionized water was added and mixed and stirred for 6 hours, centrifuged at 10,000 rpm for 15 minutes to collect the melanin precipitate, 30% ethanol aqueous solution was added, ultrasonic cleaning was performed at 300W for 10 minutes, and repeated 3 times. Finally, deionized water was used for cleaning, and the cleaned solution was freeze-dried under vacuum to obtain squid melanin particles.

[0029] Prepare a 20% (v / v) acetic acid aqueous solution. First, add polyvinyl alcohol to dissolve it to obtain a polyvinyl alcohol acetic acid solution. Then, add collagen peptides and the cuttlefish melanin granules obtained in the above steps. Homogenize by ultrasound to obtain a spinning solution (ultrasound power 100W, homogenization time 10min). In the spinning solution, the mass fraction of polyvinyl alcohol is 10wt%, the mass fraction of collagen peptides is 30wt%, and the mass fraction of cuttlefish melanin granules is 1wt%.

[0030] Electrospinning was performed using the spinning solution. The electrospinning parameters were set as follows: voltage of 20kV, needle size of 18G, distance between needle and platform receiving device of 10cm, and propulsion rate of propeller of 3mL / h, to obtain antioxidant electrospinned mask fabric.

[0031] Example 2

[0032] The squid ink sac was washed clean, the squid ink was collected, deionized water was added and mixed and stirred for 6 hours, centrifuged at 10,000 rpm for 15 minutes to collect the melanin precipitate, 30% ethanol aqueous solution was added, ultrasonic cleaning was performed at 300W for 10 minutes, and repeated 3 times. Finally, deionized water was used for cleaning, and the cleaned solution was freeze-dried under vacuum to obtain squid melanin particles.

[0033] Prepare a 20% (v / v) acetic acid aqueous solution. First, add polyvinyl alcohol to dissolve it to obtain a polyvinyl alcohol acetic acid solution. Then, add collagen peptides and the cuttlefish melanin granules obtained in the above steps. Homogenize by ultrasonication to obtain a spinning solution (ultrasonic power 100W, homogenization time 10min). In the spinning solution, the mass fraction of polyvinyl alcohol is 10wt%, the mass fraction of collagen peptides is 20wt%, and the mass fraction of cuttlefish melanin granules is 1wt%.

[0034] Electrospinning was performed using the spinning solution. The electrospinning parameters were set as follows: voltage of 20kV, needle size of 18G, distance between needle and platform receiving device of 10cm, and propulsion rate of propeller of 3mL / h, to obtain antioxidant electrospinned mask fabric.

[0035] Example 3

[0036] The squid ink sac was washed clean, the squid ink was collected, deionized water was added and mixed and stirred for 6 hours, centrifuged at 10,000 rpm for 15 minutes to collect the melanin precipitate, 30% ethanol aqueous solution was added, ultrasonic cleaning was performed at 300W for 10 minutes, and repeated 3 times. Finally, deionized water was used for cleaning, and the cleaned solution was freeze-dried under vacuum to obtain squid melanin particles.

[0037] Prepare a 20% (v / v) acetic acid aqueous solution. First, add polyvinyl alcohol and dissolve it to obtain a polyvinyl alcohol acetic acid solution. Then, add collagen peptides and the cuttlefish melanin granules obtained in the above steps. Homogenize by ultrasound to obtain a spinning solution (ultrasound power 100W, homogenization time 10min). In the spinning solution, the mass fraction of polyvinyl alcohol is 10wt%, the mass fraction of collagen peptides is 10wt%, and the mass fraction of cuttlefish melanin granules is 1wt%.

[0038] Electrospinning was performed using the spinning solution. The electrospinning parameters were set as follows: voltage of 20kV, needle size of 18G, distance between needle and platform receiving device of 10cm, and propulsion rate of propeller of 3mL / h, to obtain antioxidant electrospinned mask fabric.

[0039] Example 4

[0040] The squid ink sac was washed clean, the squid ink was collected, deionized water was added and mixed and stirred for 6 hours, centrifuged at 10,000 rpm for 15 minutes to collect the melanin precipitate, 30% ethanol aqueous solution was added, ultrasonic cleaning was performed at 300W for 10 minutes, and repeated 3 times. Finally, deionized water was used for cleaning, and the cleaned solution was freeze-dried under vacuum to obtain squid melanin particles.

[0041] Prepare a 20% (v / v) acetic acid aqueous solution. First, add polyvinyl alcohol to dissolve it to obtain a polyvinyl alcohol acetic acid solution. Then, add collagen peptides and the cuttlefish melanin granules obtained in the above steps. Homogenize by ultrasound to obtain a spinning solution (ultrasound power 100W, homogenization time 10min). In the spinning solution, the mass fraction of polyvinyl alcohol is 10wt%, the mass fraction of collagen peptides is 30wt%, and the mass fraction of cuttlefish melanin granules is 0.5wt%.

[0042] Electrospinning was performed using the spinning solution. The electrospinning parameters were set as follows: voltage of 20kV, needle size of 18G, distance between needle and platform receiving device of 10cm, and propulsion rate of propeller of 3mL / h, to obtain antioxidant electrospinned mask fabric.

[0043] Comparative Example 1

[0044] Prepare a 20% acetic acid aqueous solution. First, add polyvinyl alcohol to dissolve it to obtain a polyvinyl alcohol acetic acid solution. Then, add collagen peptides and homogenize by ultrasonication to obtain a spinning solution (ultrasonic power 100W, homogenization time 10min). In the spinning solution, the mass fraction of polyvinyl alcohol is 10wt% and the mass fraction of collagen peptides is 30wt%.

[0045] Electrospinning was performed using the spinning solution. The electrospinning parameters were set as follows: voltage of 20kV, needle size of 18G, distance between needle and platform receiving device of 10cm, and propulsion rate of pusher of 3mL / h, to obtain electrospinned mask fabric.

[0046] Sample Analysis

[0047] (1) Transmission electron microscopy test:

[0048] The squid melanin particles obtained in Example 1 were subjected to TEM testing, and the results are as follows: Figure 1 As shown, the squid melanin particles are uniform in size and well dispersed, with an average particle size of 100-200 nm.

[0049] (2) Mechanical property testing:

[0050] The mechanical properties of the electrospun facial mask fabrics prepared in Examples 1-4 and Comparative Example 1 were tested using a universal testing machine. The results are shown in Table 1.

[0051] Table 1. Mechanical property test results of the electrospun facial mask fabrics prepared in Examples 1-4 and Comparative Example 1.

[0052]

[0053] As shown in Table 1, the higher the content of collagen peptides, the higher the elastic modulus of the spun film and the less likely it is to deform. The addition of squid melanin particles will increase the elastic modulus of the material to a certain extent, but it can still make the material maintain good flexibility while having a certain strength.

[0054] (3) Moisturizing performance test:

[0055] The antioxidant electrospun facial mask fabrics prepared in Examples 1-3 were cut into 5cm*5cm sheets. The initial weight of each sheet was measured using a balance and recorded as G0. The sheets were then immersed in deionized water at 25°C for 10 minutes to absorb water. After absorbing water, the sheets were removed and weighed, and the weight was recorded as G1. The sheets were then placed in a constant temperature incubator at 37°C for 1 hour, and the weight was recorded as G2. Finally, the water retention rate (%) of the sheets was calculated as follows: Water retention rate (%) = (G2-G0) / (G1-G0).

[0056] Table 2. Moisturizing performance test results of the antioxidant electrospun facial masks prepared in Examples 1-3.

[0057]

[0058] As can be seen from Table 2, the antioxidant electrospun facial mask fabric has excellent moisturizing performance, with a water retention rate of up to 95.8%, and the moisturizing performance of the mask increases with the increase of collagen peptide content.

[0059] (4) Antioxidant performance test:

[0060] The electrospun facial mask fabrics prepared in Examples 1, 4, and Comparative Example 1 were subjected to an iodine-based antioxidant test. The films all turned white when exposed to iodine, with Example 1 showing the fastest whitening rate, followed by Example 4. The whitening rate of the film in Comparative Example 1 was much slower than that of the other two groups, indicating that the addition of squid melanin particles can improve the antioxidant performance of the films.

[0061] The embodiments described above provide a detailed explanation of the technical solutions of the present invention. It should be understood that the above descriptions are merely specific embodiments of the present invention and are not intended to limit the present invention. Any modifications, additions, or similar substitutions made within the scope of the principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A method for preparing an antioxidant electrospun facial mask fabric, characterized in that, Includes the following steps: The squid ink sac was washed clean, the squid ink was collected, deionized water was added and mixed and stirred for 6 h, centrifuged at 10000 rpm for 15 min to collect the melanin precipitate, 30% ethanol aqueous solution was added, ultrasonic cleaning was performed at 300 W for 10 min, and repeated 3 times. Finally, deionized water was used for cleaning, and the cleaned solution was freeze-dried under vacuum to obtain squid melanin particles. A 20% (v / v) acetic acid aqueous solution was prepared. Polyvinyl alcohol was added first to dissolve it, resulting in a polyvinyl alcohol acetic acid solution. Then, collagen peptides and the cuttlefish melanin granules prepared in the previous step were added. The solution was homogenized by ultrasonication to obtain a spinning solution. The ultrasonic power was 100W, and the homogenization time was 10 min. In the spinning solution, the mass fraction of polyvinyl alcohol was 10 wt%, the mass fraction of collagen peptides was 30 wt%, and the mass fraction of cuttlefish melanin granules was 1 wt%. Electrospinning was performed using the spinning solution. The electrospinning parameters were set as follows: voltage of 20 kV, needle size of 18 G, distance between needle and platform receiving device of 10 cm, and propulsion rate of propeller of 3 mL / h, to obtain antioxidant electrospinned mask fabric. The number-average molecular weight of the collagen peptides is 1000-2000; The antioxidant electrospun mask fabric has an elastic modulus > 40 MPa, tensile strength > 0.5 MPa, and elongation at break > 5%.

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