CN115778827A - high-VC-loading core/shell type nanofiber mask and preparation method and application thereof - Google Patents
high-VC-loading core/shell type nanofiber mask and preparation method and application thereof Download PDFInfo
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- CN115778827A CN115778827A CN202310051685.1A CN202310051685A CN115778827A CN 115778827 A CN115778827 A CN 115778827A CN 202310051685 A CN202310051685 A CN 202310051685A CN 115778827 A CN115778827 A CN 115778827A
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- 238000011068 loading method Methods 0.000 title description 8
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- 238000009987 spinning Methods 0.000 claims abstract description 60
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims abstract description 48
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- 230000014759 maintenance of location Effects 0.000 description 20
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 16
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- MKJXYGKVIBWPFZ-UHFFFAOYSA-L calcium lactate Chemical compound [Ca+2].CC(O)C([O-])=O.CC(O)C([O-])=O MKJXYGKVIBWPFZ-UHFFFAOYSA-L 0.000 description 8
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W90/00—Enabling technologies or technologies with a potential or indirect contribution to greenhouse gas [GHG] emissions mitigation
- Y02W90/10—Bio-packaging, e.g. packing containers made from renewable resources or bio-plastics
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Abstract
The invention provides a high-VC-loading-capacity core/shell type nanofiber mask as well as a preparation method and application thereof, and relates to the technical field of skin care products, wherein the preparation method of the nanofiber mask comprises the following steps: (1) Preparing a polyvinylpyrrolidone solution, a polyethylene oxide solution, a sodium alginate solution and an acylation modified chitosan solution; (2) Uniformly mixing a polyvinylpyrrolidone solution, a polyethylene oxide solution and a sodium alginate solution to obtain a spinning solution A; uniformly mixing a polyvinylpyrrolidone solution, a polyethylene oxide solution and an acylated modified chitosan solution, adding VC, and uniformly stirring to obtain a spinning solution B; (3) And (3) performing electrostatic spinning by using the spinning solution A as a shell layer solution and the spinning solution B as a core layer solution, obtaining a fiber membrane after the electrostatic spinning is finished, and drying the fiber membrane to obtain the facial mask. The mask is green and environment-friendly, has good biocompatibility, antibacterial property, degradability and stability, and can realize multi-scene application.
Description
Technical Field
The invention relates to the technical field of skin care products, in particular to a high-VC-loading-capacity core/shell type nanofiber mask and a preparation method and application thereof.
Background
The mask mainly sold in the current market uses non-woven fabrics as base materials and is matched with nutrient solution for use. This conventional combination of fibrous substrate and nutrient solution has many problems in use, such as many active substances in the nutrient solution (e.g. ascorbic acid: VC) are easily deteriorated and lost in solution. The nano-fiber facial mask is developed very quickly, and by utilizing the electrostatic spinning process, nano-fiber facial mask materials made of various materials, particularly natural materials, can be processed very well, and the cost is lower.
Chitosan and sodium alginate are two very common natural polysaccharide raw materials applied to the field of cosmetics, but the chitosan and sodium alginate are mostly used independently, and related reports on coaxial electrostatic spinning of chitosan and sodium alginate are few, and meanwhile, the spinnability of the chitosan and sodium alginate is poor, and coaxial electrostatic spinning is still difficult.
Ascorbic acid (VC) has been widely used in cosmetic and dermatological products, to promote collagen synthesis, to inhibit skin pigmentation and to reduce the photoaging phenomenon; VC is chemically active, especially in aqueous solutionsThe medium-polarity volatile electrons are removed to form dehydroascorbic acid, and then the dehydroascorbic acid is further hydrolyzed into diketone gulonic acid to lose biological activity, so that the unstable property of the VC aqueous solution makes the VC aqueous solution difficult to apply to a cosmetic formula, and the exertion of the powerful efficacy of the VC aqueous solution is limited. Furthermore, VC is very susceptible to external environment, such as transition metal ion Cu 2+ 、Fe 3+ Light, pH, temperature, high concentration oxygen, etc. These environmental factors deteriorate VC, causing it to lose its original efficacy. Most of the traditional beauty masks in the market are pre-moistened cotton masks, and the pre-moistened aqueous phase solution can increase the degradation speed of unstable components such as VC and the like, so that the storage and the use of the facial masks are influenced.
At present, there are two main measures for improving the stability of VC and prolonging its service life: firstly, chemically modifying VC to change the VC into a stable chemical structure without changing the efficacy; secondly, the structure of the VC is not changed, and the VC is positioned in a relatively closed environment by adopting an embedding (or microcapsule) technology, so that the VC is prevented from being contacted with the external environment. However, there are only reports on the research work of improving the stability of VC by using the coaxial electrospinning technology.
CN201611186875 discloses a core-shell structure nanofiber membrane, the main materials of the shell layer are sodium alginate, polyethylene oxide and poloxamer F127, and the core layer is loaded with nanoparticles embedding active substances to realize colon-targeted controlled release drug delivery. The disclosed core-shell nanofiber membrane has no good water solubility, active ingredients cannot be rapidly released, the active ingredients are dispersed in a core layer in a nanoparticle form, the loading capacity of the active ingredients is low, and the core-shell nanofiber membrane is not suitable for mask products.
Disclosure of Invention
The invention provides a high-VC-loading core/shell type nanofiber mask as well as a preparation method and application thereof, aiming at the problems in the prior art.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the invention provides a preparation method of a facial mask, which comprises the following steps:
(1) Preparing a polyvinylpyrrolidone solution, a polyethylene oxide solution, a sodium alginate solution and an acylation modified chitosan solution;
(2) Uniformly mixing a polyvinylpyrrolidone solution, a polyethylene oxide solution and a sodium alginate solution to obtain a spinning solution A; uniformly mixing a polyvinylpyrrolidone solution, a polyethylene oxide solution and an acylated modified chitosan solution, adding VC, and uniformly stirring to obtain a spinning solution B;
(3) And (3) performing electrostatic spinning by using the spinning solution A as a shell solution and the spinning solution B as a core solution, obtaining a fiber membrane after the electrostatic spinning is finished, and drying the fiber membrane to obtain the composite material.
Further, the concentration of the polyvinylpyrrolidone solution in the step (1) is 6-15% w/v, the concentration of the polyethylene oxide solution is 2-6%w/v, the concentration of the sodium alginate solution is 0.5-4%w/v, and the concentration of the acylation modified chitosan solution is 0.5-4%w/v.
Preferably, the concentration of the polyvinylpyrrolidone solution in step (1) is 15% w/v, the concentration of the polyethylene oxide solution is 4%w/v, the concentration of the sodium alginate solution is 4%w/v, and the concentration of the acylated modified chitosan solution is 2%w/v.
Further, the volume ratio of the polyvinylpyrrolidone solution, the polyoxyethylene solution and the sodium alginate solution in the step (2) is (2-5): (0.5-2): (0.5-2.5), and the volume ratio of the polyvinylpyrrolidone solution, the polyoxyethylene solution and the acylation modified chitosan solution is (2-5): (0.5-2): (0.5-2.5).
Preferably, the volume ratio of the polyvinylpyrrolidone solution, the polyoxyethylene solution and the sodium alginate solution in the step (2) is (4-9): (1-2): 1, and the volume ratio of the polyvinylpyrrolidone solution, the polyoxyethylene solution and the acylation modified chitosan solution is (4-9): (1-2): 1.
Further preferably, in the step (2), the volume ratio of the polyvinylpyrrolidone solution, the polyethylene oxide solution and the sodium alginate solution is 4.
Further, the VC in the step (2) is added in an amount of 5 to 20% by weight based on the total weight of solutes in the spinning solution A and the spinning solution B.
Preferably, the VC is added in step (2) in an amount of 10% by weight based on the total weight of solutes in dope a and dope B.
Further, in the electrostatic spinning process in the step (3), the advancing speed of the shell layer solution is 0.6-1.2mL/h, and the advancing speed of the core layer solution is 0.1-0.6mL/h.
Preferably, the advancing speed of the shell layer solution is 0.8mL/h, and the advancing speed of the core layer solution is 0.2mL/h.
In some embodiments, the method for preparing the mask comprises the following steps: preparing 6 to 15% w/v of polyvinylpyrrolidone solution, 2 to 6% w/v of polyethylene oxide solution, 0.5 to 4% w/v of sodium alginate solution and 0.5 to 4% w/v of acylation modified chitosan solution. Uniformly mixing a polyvinylpyrrolidone solution, a polyoxyethylene solution and a sodium alginate solution according to a certain metering ratio to obtain a spinning solution A; uniformly mixing a polyvinylpyrrolidone solution, a polyethylene oxide solution and an acylated modified chitosan solution according to a certain metering ratio, adding 5-20% (mass ratio to the total polymer) of VC, and uniformly stirring to obtain a spinning solution B; then adding the two prepared precursor solutions into two 15mL injectors respectively, taking the spinning solution A as a shell solution and the spinning solution B as a core solution, connecting the injectors to coaxial needles of which the spinning nozzles are respectively composed of two metal needles with different diameters, wherein the specification of the outer-layer needle is 1.48mm in outer diameter and 1.12mm in inner diameter; the specification of the inner layer needle is 0.71mm of outer diameter and 0.41mm of inner diameter. The coaxial needle is connected with a high-voltage positive electrode, the voltage is adjusted to be 10 to 30kV, the temperature is controlled to be 25 to 50 ℃, and the humidity is controlled to be 10 to 50%; the micro-injection pump adjusts the injection speeds of the shell layer solution and the core layer solution, the shell layer advancing speed is 0.6-1.2mL/h, and the core layer advancing speed is 0.1-0.6mL/h. Collecting the fibers to a grounded receiving aluminum foil, and adjusting the distance between the receiving aluminum foil and the needle head to be 10-20cm. And after the electrostatic spinning process is finished, putting the collected fiber membrane in a normal-temperature vacuum drying box for 24 to 36h, and volatilizing the residual solvent to obtain SA @ NCS-VC.
In some preferred embodiments, the method for preparing the mask comprises the following steps: preparation 15% w/v of a polyvinylpyrrolidone solution, 4%w/v of a polyethylene oxide solution, 2%w/v of a sodium alginate solution, 2%w/v of an acylated modified chitosan solution. Mixing a polyvinylpyrrolidone solution, a polyethylene oxide solution and a sodium alginate solution according to the ratio of 4:1:1 to obtain spinning solution A; mixing a polyvinylpyrrolidone solution, a polyethylene oxide solution and an acylation modified chitosan solution according to the ratio of 4:1:1, adding 10% (by mass of the total polymer) of VC, and uniformly stirring to obtain a spinning solution B; then adding the two prepared precursor solutions into two 15m L injectors respectively, taking the spinning solution A as a shell layer solution and the spinning solution B as a core layer solution, and connecting the injectors to coaxial needles of which spinning nozzles are composed of two metal needles with different diameters respectively, wherein the specification of the outer-layer needle is 1.48mm in outer diameter and 1.12mm in inner diameter; the specification of the inner layer needle is 0.71mm of outer diameter and 0.41mm of inner diameter. The coaxial needle is connected with a high-voltage anode, and the voltage is adjusted to be 25kV; controlling the temperature to be 40 ℃ and the humidity to be 20 percent; the micro-injection pump adjusts the injection speeds of the shell layer solution and the core layer solution, the shell layer injection speed is 0.8mL/h, and the core layer injection speed is 0.2mL/h; the fibers were collected into a grounded receiving aluminum foil, and the distance between the receiving aluminum foil and the needle was adjusted to 15cm. And after the electrostatic spinning process is finished, placing the collected fiber membrane in a normal-temperature vacuum drying box 48h, and volatilizing the residual solvent to obtain SA @ NCS-VC.
Further, the invention also provides the facial mask prepared by the preparation method.
Further, the preparation method of the modified chitosan is disclosed in published invention patents CN114853921a;
further, the mask disclosed by the invention can be used together with essence, and specifically comprises the following steps: after the facial mask is flatly attached to the hand, essence is sprayed and the facial mask is touched by the hand.
Further, the serum comprises calcium lactate and/or lactic acid.
It should be noted that, in the present invention, the related materials and their corresponding abbreviations are as shown in the following table:
TABLE 1 materials and corresponding abbreviations in the present invention
| For short | Material |
| VC | Ascorbic acid |
| SA | Sodium alginate |
| NCS | Acylation modified chitosan |
The technical effects obtained by the invention are as follows:
1. the preparation method comprises the following steps of taking acylation modified chitosan, sodium alginate, polyvinylpyrrolidone, polyethylene oxide, VC and the like as raw materials, taking polyvinylpyrrolidone and polyethylene oxide as spinning aids, carrying out acylation modification on chitosan, and blending in a proper proportion to enable the chitosan and the sodium alginate which are originally difficult to coaxially spin to be successfully spun so as to obtain SA @ NCS-VC with a core-shell structure;
and 2, carrying out coaxial spinning on chitosan and sodium alginate by using SA @ NCS-VC, wherein the obtained fiber membrane has good biocompatibility, antibacterial property and degradability. The method can be used for developing green and environment-friendly mask products, and can reduce the problem of bacterial breeding in the mask storage process;
3. VC is added into the fiber membrane core layer, the stability of VC can be improved, and the VC retention rate can still reach more than 50% after the fiber membrane core layer is placed in an environment of 55 ℃ for 120 hours. Can be developed into specific facial mask product for prolonging shelf life of unstable active substance;
4. since SA @ NCS-VC can greatly improve the stability of VC, the VC with higher concentration can be carried, the carrying amount of VC can reach more than 10 percent of the mass of the whole polymer, and the carrying amount of VC in most of mask products containing VC in the market is 2-5 percent;
SA @ NCS-VC can control the dissolving speed and the dissolving degree of the dissolving solvent by changing the dissolving solvent, thereby realizing multi-scene application. After the essence is sprayed, the contained active substances can be completely released within 10min, so that the rapid skin care experience is realized; in addition, the components such as calcium lactate and lactic acid are added into the essence, so that the mask becomes gel after being sprayed with the essence, has a certain lifting effect, and can achieve the purpose of tightening the skin.
Drawings
FIG. 1 is a form view of a mask according to the present invention;
FIG. 2 is a scanning electron micrograph of SA @ NCS-VC;
FIG. 3 is a scanning electron microscope of NCS @ SA-VC;
FIG. 4 is a VC release rate curve for SA @ NCS-VC;
FIG. 5 is a curve of the retention rate of SA @ NCS-VC, VC aqueous solutions to VC;
FIG. 6 shows the state of SA @ NCS-VC before and after spraying the self-made essence, wherein a is before spraying the self-made essence, and b is after spraying the self-made essence;
FIG. 7 shows the SA @ NCS-VC status before and after spraying the self-made essence (containing 0.5% lactic acid), wherein a is before spraying the self-made essence, and b is after spraying the self-made essence;
FIG. 8 shows SA @ NCS-VC status before and after spraying the self-made essence (containing 1% calcium lactate), wherein a is before spraying the self-made essence, and b is after spraying the self-made essence;
FIG. 9 shows SA @ NCS-VC status before and after spraying the self-made essence (containing 0.5% lactic acid and 0.75% calcium lactate), wherein a is before spraying the self-made essence, and b is after spraying the self-made essence;
FIG. 10 shows SA @ NCS-VC status before and after spraying the self-made essence (containing 0.5% lactic acid and 1% calcium lactate), wherein a is before spraying the self-made essence, and b is after spraying the self-made essence.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
Before the present embodiments are further described, it is to be understood that the scope of the invention is not to be limited to the specific embodiments described below; it is also to be understood that the terminology used in the examples is for the purpose of describing particular embodiments only, and is not intended to limit the scope of the present invention.
When numerical ranges are given in the examples, it is understood that both endpoints of each of the numerical ranges and any value therebetween can be selected unless the invention otherwise indicated. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It should be noted that the raw materials used in the present invention are all common commercial products, and thus the sources thereof are not particularly limited.
The mask pattern of the present invention is specifically shown in fig. 1.
Example 1:
Example 2:
2% preparation of a polyvinyl pyrrolidone solution 20mL,4% w/v of a polyethylene oxide solution 10mL,2% w/v of a sodium alginate solution 10mL,2% w/v of an acylation-modified chitosan solution 10mL. Uniformly mixing 9mL of polyvinylpyrrolidone solution, 2mL of polyethylene oxide solution and 1mL of sodium alginate solution to obtain spinning solution A; uniformly mixing 9mL of polyvinylpyrrolidone solution, 2mL of polyethylene oxide solution and 1mL of acylated modified chitosan solution, adding 0.5gVC, and uniformly stirring to obtain spinning solution B; and then adding the two prepared precursor solutions into two 15m L injectors respectively, taking the spinning solution A as a shell solution and the spinning solution B as a core solution, and connecting the injectors to coaxial needles, wherein the spinning nozzles of the coaxial needles are formed by two metal needles with different diameters respectively. The coaxial needle is connected with a high-voltage anode, and the voltage is adjusted to be 20kV; controlling the temperature to be 40 ℃ and the humidity to be 20 percent; the injection speeds of the shell layer solution and the core layer solution are adjusted by a micro-injection pump, the shell layer advancing speed is 0.6mL/h, and the core layer advancing speed is 0.4mL/h; the fibers were collected into a grounded receiving aluminum foil, and the distance between the receiving aluminum foil and the needle was adjusted to 15cm. And after the electrostatic spinning process is finished, placing the collected fiber membrane in a normal-temperature vacuum drying box 48h, and volatilizing the residual solvent to obtain SA @ NCS-VC. The scanning electron micrograph of the prepared nanofiber facial mask is similar to that of figure 2.
Example 3:
2% preparation of a polyvinyl pyrrolidone solution 20mL,4% w/v of a polyethylene oxide solution 10mL,2% w/v of a sodium alginate solution 10mL,2% w/v of an acylation-modified chitosan solution 10mL. Uniformly mixing 8mL of polyvinylpyrrolidone solution, 2mL of polyethylene oxide solution and 2mL of acylated modified chitosan solution to obtain spinning solution A; uniformly mixing 8mL of polyvinylpyrrolidone solution, 2mL of polyethylene oxide solution and 2mL of sodium alginate solution, adding 0.5g of VC, and uniformly stirring to obtain spinning solution B; and then adding the two prepared precursor solutions into two 15m L injectors respectively, taking the spinning solution A as a shell solution and the spinning solution B as a core solution, and connecting the injectors to coaxial needles of which spinning nozzles are respectively composed of two metal needles with different diameters. The coaxial needle is connected with a high-voltage anode, and the voltage is adjusted to be 25kV; controlling the temperature to be 40 ℃ and the humidity to be 20 percent; the injection speeds of the shell layer solution and the core layer solution are adjusted by a micro-injection pump, the shell layer advancing speed is 0.8mL/h, and the core layer advancing speed is 0.2mL/h; the fibers were collected into a grounded receiving aluminum foil, and the distance between the receiving aluminum foil and the needle was adjusted to 15cm. After the electrostatic spinning process is finished, the collected fiber membrane is placed in a normal-temperature vacuum drying box 48h, and residual solvent is volatilized to obtain NCS @ SA-VC. The scanning electron microscope image of the prepared nanofiber facial mask is shown in fig. 3.
Example 4:
2% preparation of a polyvinyl pyrrolidone solution 20mL,4% w/v of a polyethylene oxide solution 10mL,2% w/v of a sodium alginate solution 10mL,2% w/v of an acylation-modified chitosan solution 10mL. Uniformly mixing 9mL of polyvinylpyrrolidone solution, 2mL of polyethylene oxide solution and 1mL of acylated modified chitosan solution to obtain spinning solution A; uniformly mixing 9mL of polyvinylpyrrolidone solution, 2mL of polyethylene oxide solution and 1mL of sodium alginate solution, adding 0.5g of VC, and uniformly stirring to obtain spinning solution B; and then adding the two prepared precursor solutions into two 15m L injectors respectively, taking the spinning solution A as a shell solution and the spinning solution B as a core solution, and connecting the injectors to coaxial needles of which spinning nozzles are respectively composed of two metal needles with different diameters. The coaxial needle is connected with a high-voltage anode, and the voltage is adjusted to be 25kV; controlling the temperature to be 40 ℃ and the humidity to be 20 percent; the injection speeds of the shell layer solution and the core layer solution are adjusted by a micro-injection pump, the shell layer advancing speed is 0.6mL/h, and the core layer advancing speed is 0.4mL/h; the fibers were collected into a grounded receiving aluminum foil, and the distance between the receiving aluminum foil and the needle was adjusted to 15cm. After the electrostatic spinning process is finished, placing the collected fiber membrane in a normal-temperature vacuum drying oven 48h, and volatilizing the residual solvent to obtain NCS @ SA-VC. The scanning electron micrograph of the prepared nanofiber facial mask is similar to that of figure 3.
Example 5:
a10 mg sample of SA @ NCS-VC (prepared in example 1) was taken, placed in 10mL of deionized water, and the absorbance thereof was measured at 243nm every 2min using an ultraviolet spectrophotometer, and the VC concentration therein was calculated according to a standard curve and recorded. The resulting VC release rate profile is shown in fig. 4. Meanwhile, the VC loading amount is calculated according to the measured VC concentration in the sample, and the VC loading amount in the SA @ NCS-VC prepared in example 1 is 11.23 percent
Example 6:
a sample of 10mg NCS @ SA-VC (prepared in example 3) was taken, placed in 10mL of deionized water, and the absorbance thereof was measured at 243nm every 2min using an ultraviolet spectrophotometer, and the VC concentration therein was calculated according to a standard curve and recorded. The resulting VC release rate profile is similar to figure 4. Meanwhile, the VC loading amount is calculated according to the measured VC concentration in the sample, and the VC loading amount in the NCS @ SA-VC prepared in the example 3 is 10.42 percent
Example 7:
a sample of 10mg SA @ NCS-VC (prepared in example 1) was taken, dissolved in 10mL of deionized water, and the absorbance thereof was measured at 243nm using an ultraviolet spectrophotometer, and the VC concentration therein was calculated according to a standard curve and recorded. Then, the SA @ NCS-VC sample is placed in an incubator, the temperature is adjusted to 55 ℃, 10mg of SA @ NCS-VC sample is taken at intervals of 24h and dissolved in 10mL deionized water, the absorbance of the sample is measured at 243nm by using an ultraviolet spectrophotometer, the VC concentration is calculated according to a standard curve, and then the VC retention rate is calculated. The resulting SA @ NCS-VC vs. VC retention curve is shown in FIG. 5.
Example 8:
a sample of 5mg SA @ NCS-VC (prepared in example 1) was taken, dissolved in 10mL deionized water, and the absorbance thereof was measured at 243nm using an ultraviolet spectrophotometer, and the VC concentration therein was calculated according to a standard curve and recorded. Then, the SA @ NCS-VC sample is placed in a thermostat, the temperature is adjusted to 55 ℃, 5mg of the SA @ NCS-VC sample is taken at intervals of 24h, the SA @ NCS-VC sample is dissolved in 10mL deionized water, the absorbance of the SA @ NCS-VC sample is measured at 243nm by using an ultraviolet spectrophotometer, the VC concentration is calculated according to a standard curve, and then the VC retention rate is calculated. The resulting SA @ NCS-VC vs. VC retention curve is similar to that of example 7.
Example 9:
a sample of 10mg NCS @ SA-VC (prepared in example 3) was taken, dissolved in 10mL of deionized water, and the absorbance thereof was measured at 243nm using an ultraviolet spectrophotometer, and the VC concentration therein was calculated according to a standard curve and recorded. Then, placing the NCS @ SA-VC sample in a thermostat, adjusting the temperature to 55 ℃, taking 10mg of the NCS @ SA-VC sample at intervals of 24h, dissolving the sample in 10mL deionized water, measuring the absorbance of the sample at 243nm by using an ultraviolet spectrophotometer, calculating the VC concentration according to a standard curve, and calculating the VC retention rate. The resulting NCS @ SA-VC vs. VC retention curve is similar to example 7.
Example 10:
a sample of 5mg NCS @ SA-VC (prepared in example 3) was taken, dissolved in 10mL of deionized water, and the absorbance thereof was measured at 243nm using an ultraviolet spectrophotometer, and the VC concentration therein was calculated according to a standard curve and recorded. Then, placing the NCS @ SA-VC sample in a thermostat, adjusting the temperature to 55 ℃, taking 5mg of the NCS @ SA-VC sample at intervals of 24h, dissolving the sample in 10mL deionized water, measuring the absorbance of the sample at 243nm by using an ultraviolet spectrophotometer, calculating the VC concentration according to a standard curve, and calculating the VC retention rate. The resulting NCS @ SA-VC vs. VC retention rate curve is similar to example 7.
Example 11:
a2 cm x 4 cm SA @ NCS-VC sample (prepared in example 1) is cut, the sample is flatly attached to the hand, the self-made essence is sprayed, the color and the state of the fiber film are not changed after 6s, the state of the fiber film is shown in figure 6, the fiber film is completely dissolved by touching with the hand, and the fiber shape is completely lost.
Example 12:
a2 cm x 4 cm SA @ NCS-VC sample (prepared in example 1) is cut and attached to the hand flatly, self-made essence (containing 0.5% of lactic acid) is sprayed, the color and the state of the fiber film are not changed after 10 seconds, the state of the fiber film is shown in figure 7, the fiber film is touched by hand, most of the fiber film is dissolved, and a small part of the fiber form is kept.
Example 13:
a2 cm x 4 cm SA @ NCS-VC sample (prepared in example 1) is cut, the sample is flatly attached to the hand, a self-made essence (containing 1% calcium lactate) is sprayed, the color and the state of the fiber film are not changed after 16s, the state of the fiber film is shown in figure 8, the fiber film is touched by a hand, the fiber film is partially dissolved, most of the fiber shape is kept, and the fiber film can be partially lifted.
Example 14:
a2 cm x 4 cm SA @ NCS-VC sample (prepared in example 1) is cut, the sample is flatly attached to the hand, a self-made essence (containing 0.5% of lactic acid and 0.75% of calcium lactate) is sprayed, the color and the state of the fiber film are not changed after 20s, the fiber film is in the state shown in figure 9, the fiber film is partially dissolved by touching with a hand, most of the fiber shape is kept, and the fiber film can be partially lifted.
Example 15:
a2 cm x 4 cm SA @ NCS-VC sample (prepared in example 1) is cut, the sample is flatly attached to the hand, self-made essence (containing 0.5% of lactic acid and 1% of calcium lactate) is sprayed, the color and the state of a fiber film are not changed after 20 seconds, the state of the fiber film is shown in figure 10, the fiber film is slightly dissolved by touching with hands, the fiber shape is kept, and the fiber film can be completely torn off.
Comparative example 1:
2mL of polyvinylpyrrolidone solution prepared at 15% w/v, 4% w/v of polyethylene oxide solution prepared at 10mL,2% w/v of acylation-modified chitosan solution prepared at 10mL. Uniformly mixing 8mL of polyvinylpyrrolidone solution, 2mL of polyethylene oxide solution and 2mL of acylation modified chitosan solution, adding 0.5g of VC, and uniformly stirring. Then the precursor solution prepared above is added into a 15m L injector for electrostatic spinning. Regulating voltage to 25kV, controlling temperature to 40 ℃ and controlling humidity to 20%; the injection speed is adjusted to be 0.8mL/h by a micro-injection pump; the fibers were collected into a grounded receiving aluminum foil, and the distance between the receiving aluminum foil and the needle was adjusted to 15cm. And after the electrostatic spinning process is finished, placing the collected fiber membrane in a normal-temperature vacuum drying oven 48h, and volatilizing the residual solvent to obtain the NCS-VC. Taking 10mg NCS-VC sample, dissolving in 10mL deionized water, measuring the absorbance at 243nm by using an ultraviolet spectrophotometer, calculating the VC concentration according to a standard curve, and recording. Then, placing the NCS-VC sample in a thermostat, adjusting the temperature to 55 ℃, taking 10mg of NCS-VC sample at intervals of 24h, dissolving the NCS-VC sample in 10mL deionized water, measuring the absorbance of the NCS-VC sample at 243nm by using an ultraviolet spectrophotometer, calculating the VC concentration according to a standard curve, and calculating the VC retention rate. The resulting NCS-VC vs VC retention rate curve is shown in fig. 5.
Comparative example 2:
Comparative example 3:
dissolving 30mg of VC in 1L of deionized water, placing in a thermostat, adjusting the temperature to 55 ℃, taking part of samples at intervals of 24 hours, measuring the absorbance at 243nm by using an ultraviolet spectrophotometer, calculating the concentration of VC in the sample according to a standard curve, and calculating the VC retention rate. The resulting VC aqueous solution versus VC retention curve is shown in fig. 5.
By comparing the VC retention rate curves (as shown in FIG. 5) obtained in example 7, comparative example 1 and comparative example 3, it can be seen that the SA @ NCS-VC fiber membrane has the highest VC retention rate, the NCS-VC has the second retention rate, and the VC aqueous solution has the lowest VC retention rate. Therefore, the VC stabilizer has obvious advantages compared with other products in the aspect of improving the stability of VC.
Comparative example 4:
2mL of a polyvinyl alcohol solution at 8%w/v, 2% 10mL of a sodium alginate solution at w/v, and 10mL of an acylation-modified chitosan solution at 2 w/v. Uniformly mixing 8mL of polyvinyl alcohol solution and 2mL of sodium alginate solution to obtain a spinning solution A; uniformly mixing 8mL of polyvinyl alcohol solution and 2mL of acylated modified chitosan solution, adding 0.5g of VC, and uniformly stirring to obtain spinning solution B; and then adding the two prepared precursor solutions into two 15m L injectors respectively, taking the spinning solution A as a shell solution and the spinning solution B as a core solution, and connecting the injectors to coaxial needles, wherein the spinning nozzles of the coaxial needles are formed by two metal needles with different diameters respectively. The coaxial needle is connected with a high-voltage anode, and the voltage is adjusted to be 25kV; controlling the temperature to be 40 ℃ and the humidity to be 20 percent; the injection speeds of the shell layer solution and the core layer solution are adjusted by a micro-injection pump, the shell layer advancing speed is 0.8mL/h, and the core layer advancing speed is 0.2mL/h; the fibers were collected into a grounded receiving aluminum foil, and the distance between the receiving aluminum foil and the needle was adjusted to 15cm. And after the electrostatic spinning process is finished, placing the collected fiber membrane in a normal-temperature vacuum drying oven for 48 hours, and volatilizing the residual solvent to obtain the sample. The self-made essence is sprayed, and the fact that the fiber membrane is high in viscosity after being dissolved (or formed into gel) and can be adhered to the skin, the skin feeling is poor, the fiber membrane is difficult to wash, and the fiber membrane is not suitable for manufacturing a mask product. The sample of the example 1 is sprayed with the self-made essence, and after the fiber membrane is dissolved (or becomes gel), the viscosity is moderate, the skin feel is good, the fiber membrane is easy to wash off, and the fiber membrane is suitable for preparing a mask product.
Comparative example 5:
2% preparation of a polyvinylpyrrolidone solution (2 mL, 2%) by w/v, 10mL of a sodium alginate solution (2%) by w/v, and 10mL of an acylation-modified chitosan solution (2%) by w/v. Uniformly mixing 4mL of polyvinylpyrrolidone solution, 5mL of polyethylene oxide solution and 3mL of sodium alginate solution to obtain spinning solution A; uniformly mixing 4mL of polyvinylpyrrolidone solution, 5mL of polyethylene oxide solution and 3mL of acylated modified chitosan solution, adding 0.5g of VC, and uniformly stirring to obtain spinning solution B; and then adding the two prepared precursor solutions into two 15mL injectors respectively, wherein the spinning solution A is taken as a shell layer solution, the spinning solution B is taken as a core layer solution, and the injectors are connected to coaxial needles of which the spinning nozzles are respectively composed of two metal needles with different diameters. The coaxial needle is connected with a high-voltage anode, and the voltage is adjusted to be 25kV; controlling the temperature to be 40 ℃ and the humidity to be 20 percent; the injection speeds of the shell layer solution and the core layer solution are adjusted by a micro-injection pump, the shell layer advancing speed is 0.8mL/h, and the core layer advancing speed is 0.2mL/h; the fibers were collected into a grounded receiving aluminum foil, and the distance between the receiving aluminum foil and the needle was adjusted to 15cm. And after the electrostatic spinning process is finished, placing the collected fiber membrane in a normal-temperature vacuum drying box 48h, and volatilizing residual solvent to obtain the sample. The maximum tensile strength is less than 0.8Mpa, the fiber membrane is easy to break, and the viscosity is still high after the fiber membrane is dissolved (or becomes gel), the fiber membrane can be adhered to the skin and has poor skin feel, and the fiber membrane is difficult to wash off and is not suitable for preparing a mask product. The samples in the embodiment 1 are taken, the maximum tensile strength is greater than 3Mpa through measurement, the samples are not easy to break, and the samples can be used for manufacturing mask products.
Finally, it should be noted that the above-mentioned contents are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, and that the simple modifications or equivalent substitutions of the technical solutions of the present invention by those of ordinary skill in the art can be made without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. A preparation method of the facial mask is characterized by comprising the following steps: the method comprises the following steps:
(1) Preparing a polyvinylpyrrolidone solution, a polyethylene oxide solution, a sodium alginate solution and an acylation modified chitosan solution;
(2) Uniformly mixing a polyvinylpyrrolidone solution, a polyethylene oxide solution and a sodium alginate solution to obtain a spinning solution A; uniformly mixing a polyvinylpyrrolidone solution, a polyethylene oxide solution and an acylated modified chitosan solution, adding VC, and uniformly stirring to obtain a spinning solution B;
(3) And (3) performing electrostatic spinning by using the spinning solution A as a shell solution and the spinning solution B as a core solution, obtaining a fiber membrane after the electrostatic spinning is finished, and drying the fiber membrane to obtain the composite material.
2. The method of claim 1, wherein: the concentration of the polyvinylpyrrolidone solution in step (1) is 6-15% w/v, the concentration of the polyoxyethylene solution is 2-6%w/v, the concentration of the sodium alginate solution is 0.5-4%w/v, and the concentration of the acylated modified chitosan solution is 0.5-4%w/v.
3. The method of claim 2, wherein: the concentration of the polyvinylpyrrolidone solution in step (1) was 15% w/v, the concentration of the polyoxyethylene solution was 4%w/v, the concentration of the sodium alginate solution was 4%w/v, and the concentration of the acylation modified chitosan solution was 2%w/v.
4. The method of claim 1, wherein: in the step (2), the volume ratio of the polyvinylpyrrolidone solution, the polyoxyethylene solution and the sodium alginate solution is (2-5): (0.5-2): (0.5-2.5), and the volume ratio of the polyvinylpyrrolidone solution, the polyoxyethylene solution and the acylated modified chitosan solution is (2-5): (0.5-2): (0.5-2.5).
5. The method of claim 4, wherein: in the step (2), the volume ratio of the polyvinylpyrrolidone solution to the polyoxyethylene solution to the sodium alginate solution is 4.
6. The method of claim 1, wherein: and (3) in the step (2), the addition weight of the VC accounts for 5-20% of the total weight of solutes in the spinning solution A and the spinning solution B.
7. The method of claim 6, wherein: the addition weight of VC in the step (2) accounts for 10% of the total weight of solutes in the spinning solution A and the spinning solution B.
8. The method of claim 1, wherein: in the electrostatic spinning process in the step (3), the advancing speed of the shell layer solution is 0.6-1.2mL/h, and the advancing speed of the core layer solution is 0.1-0.6mL/h.
9. The method of claim 1, wherein: the advancing speed of the shell layer solution is 0.8mL/h, and the advancing speed of the core layer solution is 0.2mL/h.
10. The mask pack produced by the production method according to any one of claims 1 to 9.
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