A plant active ingredient-based nanofiber mask, and a preparation method and application thereof
By using an all-natural plant nanofiber base and atomization anchoring technology, the problem of environmental friendliness and low active ingredient loading efficiency of face masks has been solved, achieving efficient preservation and stable release of whitening effects, and possessing excellent biodegradability and antioxidant efficacy.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- YUNNAN MINZU UNIV
- Filing Date
- 2026-03-26
- Publication Date
- 2026-06-19
AI Technical Summary
Existing mask base fabric synthetic materials are not environmentally friendly enough, have low loading efficiency for ethnic plant active ingredients, and the active ingredients are easily lost in traditional loading methods.
Using all-natural plant nanofibers as a base, a nanocellulose mask is prepared by combining low-temperature extraction with atomization anchoring technology. The active plant ingredients are loaded into the nanofiber network by ultrasonic atomization to form a three-dimensional porous structure, achieving efficient loading and stable release.
It achieves 100% biodegradability of the mask, improves the loading rate and preservation efficiency of active ingredients, has excellent antioxidant properties and whitening effects, and has good biocompatibility.
Smart Images
Figure CN122229693A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to a nanofiber facial mask based on plant active ingredients, its preparation method and application, belonging to the field of functional cosmetics technology. Background Technology
[0002] As an important category of skincare products, the choice of carrier materials and active ingredients in facial masks directly affects product performance and environmental friendliness. Currently, most commercially available facial masks use non-woven fabrics as the base material. While publicly available green, biodegradable plant fiber masks, made from pulp fibers and bio-based adhesives, offer some environmental benefits, the fiber diameter is in the micrometer range, limiting their ability to load active ingredients. Another common type of bio-based synthetic fiber antibacterial mask uses a blend of gramineous fibers and regenerated cellulose fibers to create the base fabric through a hydroentanglement process. Although possessing antibacterial properties, these masks still rely on essence soaking to load active ingredients, leading to potential ingredient loss.
[0003] Electrospinning technology provides an effective method for preparing nanofiber membranes. A related technology discloses a bio-based antibacterial face mask, which uses modified chitosan, hyaluronic acid, and gelatin to prepare a functional membrane via electrospinning, followed by a modified polyimide layer. While achieving antibacterial and unidirectional moisture-wicking functions, its matrix still partially relies on synthetic polymers (such as polyimide), and the direct mixing of active ingredients into the spinning solution can lead to activity loss due to the high-voltage electric field and organic solvents during the spinning process. Furthermore, this technology does not solve the problem of efficient loading of natural plant extracts.
[0004] Extracts from plants such as saffron, snow lotus, fireweed, sea buckthorn, wild chrysanthemum, aloe vera, Bletilla striata, Panax notoginseng, Artemisia argyi, and Portulaca oleracea are rich in heat-sensitive active ingredients (such as flavonoids and terpenes), and traditional extraction and loading methods struggle to preserve their activity. There is a lack of research on combining these unique plant extracts with all-natural nanofiber substrates and achieving efficient anchoring of active ingredients through innovative processes.
[0005] Therefore, developing a face mask with all-natural plant nanofibers as the base, loaded with active ingredients from plateau ethnic plants through a gentle process, and possessing excellent performance and environmental protection characteristics, has significant innovative significance and market value. Summary of the Invention
[0006] To address the shortcomings of related technologies, this invention provides a nanofiber facial mask based on plant active ingredients, its preparation method, and its application. The nanofiber facial mask prepared by this invention has excellent whitening effects: the tyrosinase inhibition rate of the transdermal permeable liquid is >40% after 2 hours and >65% after 24 hours, solving the problems of existing facial mask base fabric synthetic materials being not environmentally friendly and having low loading efficiency of ethnic plant active ingredients.
[0007] One objective of this invention is to provide a nanofiber facial mask containing plant-based active ingredients. The nanofiber mask is composed of a layer of plant-based active ingredients atomized, deposited, and anchored onto a nanofiber substrate layer. The plant-based active ingredient layer comprises, by weight percentage: 10-30% plant-based active extracts, 2-8% natural carriers, and the remainder being water. The nanofiber substrate layer comprises, by weight percentage: 50-80% natural plant nanofibers, 5-15% natural crosslinking agents, and 3-10% natural plasticizers. The loading of the plant-based active ingredient layer onto the nanofiber substrate layer is 50-200 mg / m³. 2 .
[0008] Preferably, the plant active extract is a combination of two or more of the following: saffron extract, snow lotus extract, fireweed extract, sea buckthorn fruit extract, wild chrysanthemum extract, aloe vera extract, Bletilla striata extract, Panax notoginseng extract, Artemisia argyi extract, and Portulaca oleracea extract; the natural plant nanofiber is a cellulose nanofiber obtained by mechanical nano-sizing of wood pulp fiber, cotton fiber, or bamboo fiber, with a diameter of 50-100 nm.
[0009] More preferably, the plant active extract is a combination of saffron extract and snow lotus extract; the natural plant nanofiber is cellulose nanofiber obtained by mechanical nano-sizing of wood pulp fiber, with a diameter of 50-100 nm.
[0010] Preferably, the atomization deposition employs ultrasonic atomization or high-pressure micro-mist technology, with atomized droplet particle size of 10-50 μm; the natural carrier is β-cyclodextrin; the natural crosslinking agent is either genipin or tannic acid; and the natural plasticizer is either glycerol or citrate.
[0011] More preferably, the atomization deposition employs ultrasonic atomization technology.
[0012] The second objective of this invention is to provide a method for preparing a nanofiber facial mask based on plant active ingredients, specifically including the following steps: (1) Preparation of plant active extracts: Plant powder is placed in a solvent and cold soaked to obtain a mixture. The mixture is then subjected to ultrasonication, filtration, evaporation and concentration, and freeze drying to obtain plant active extract powder.
[0013] (2) Preparation of natural plant nanofibers: Wood pulp fiber, cotton fiber or bamboo fiber is subjected to cyclic high-pressure homogenization under alkaline conditions (preferably pH 10-12) to obtain a natural plant nanofiber suspension.
[0014] (3) Preparation of nanofiber substrate: Natural crosslinking agent and natural plasticizer are placed in natural plant nanofiber suspension and dispersed (preferably dispersed using a high-speed shear emulsifier) to form a spinnable solution. The spinnable solution is electrospun (preferably electrospun using a porous nozzle electrospinning device) to make a nanofiber membrane.
[0015] (4) Post-treatment: The nanofiber membrane is vacuum dried and then cross-linked by ultraviolet irradiation to obtain the nanofiber substrate layer.
[0016] (5) Active ingredient atomization and anchoring: The active ingredient loading solution is atomized and deposited on the surface of the nanofiber substrate using atomization deposition technology, and then dried and cured to obtain a nanofiber mask based on plant active ingredients.
[0017] Preferably, in step (1), the solvent is prepared by mixing anhydrous ethanol and water in a volume ratio of 1:(3-5); the cold soaking conditions are: cold soaking at 4-8℃ for 24-48h; the amount of plant powder added to the mixture is 0.0667-0.125g / mL; the ultrasonic conditions are: ultrasonic treatment at a power of 300-500W and a temperature of 40-50℃ for 30-45min.
[0018] Preferably, the conditions for the cyclic high-pressure homogenization treatment in step (2) are: homogenization and cyclic treatment for 5-8 times under a pressure of 80-100MPa; the content of natural plant nanofibers in the natural plant nanofiber suspension is 3-5% by mass percentage.
[0019] Preferably, the dispersion conditions in step (3) are: dispersion for 20-30 minutes at a rotation speed of 10000-15000 rpm; the electrospinning conditions are: spinning for 8-12 hours at a voltage of 18-25 kV, a receiving distance of 12-18 cm, a spinning speed of 0.8-1.5 mL / h, an ambient temperature of 22-28 °C, and an ambient relative humidity (RH) of 40-50%.
[0020] Preferably, the vacuum drying conditions in step (4) are: vacuum drying at 40-45℃ for 6-8 hours; and the ultraviolet irradiation crosslinking time is 10-15 minutes.
[0021] More preferably, step (4) involves ultraviolet crosslinking using UVB (280-315nm).
[0022] Preferably, in step (5), when ultrasonic atomization is used for atomization deposition, the atomization rate is 0.5-2 mL / min; the drying and curing temperature is 25-30℃; and the active ingredient loading solution is an aqueous solution of plant active extract powder and natural carrier.
[0023] The third objective of this invention is to provide an application of the nanofiber facial mask based on plant active ingredients prepared in this invention in the field of medical aesthetics and cosmetics.
[0024] Mechanism of the invention: This invention solves the problems of poor environmental friendliness, low active ingredient loading rate, and easy deactivation of traditional face masks by combining an all-natural base with a gentle directional loading process.
[0025] (1) The all-natural nanofiber substrate provides a basis for environmental protection and high load-bearing capacity. Plant cellulose is mechanically nano-sized to obtain fibers with a diameter of 50-100 nm, which are then electrospun into a three-dimensional network with an ultra-high specific surface area. This biomimetic structure can not only closely adhere to the skin and promote the delivery of ingredients, but also achieve complete biodegradability because all its components (cellulose, natural cross-linking agents) can be recognized by microorganisms. Compared with synthetic material substrates (such as polyimide in Comparative Example 2), this is the fundamental reason why it has both high load-bearing capacity and excellent environmental friendliness.
[0026] (2) The low-temperature extraction-atomization anchoring process achieves efficient preservation and precise loading of active ingredients. Compared with traditional high-temperature extraction or simple soaking (Comparative Example 1), this invention uses low-temperature cold soaking and gentle ultrasonic extraction to maximize the protection of the initial activity of heat-sensitive active substances (such as crocin). Subsequently, the active liquid containing β-cyclodextrin (natural carrier) is converted into micron-sized droplets by ultrasonic atomization, allowing it to penetrate deep into the nanofiber network and be effectively encapsulated and fixed. Compared with soaking, this atomization anchoring method achieves uniform and high-capacity loading (50-200 mg / m³) of active ingredients in three-dimensional space. 2 It utilizes carrier encapsulation to delay release, ensuring long-lasting and stable antioxidant (high DPPH scavenging rate) and whitening (continuous inhibition of tyrosinase) effects.
[0027] The beneficial effects of this invention are: (1) All-natural and environmentally friendly base: This invention uses pure plant fibers (wood pulp, cotton, bamboo) that have been mechanically nano-processed as electrospinning matrix, avoiding the use of synthetic polyimide materials, and achieving 100% biodegradability of the mask base. The degradation rate (28 days of soil burial) is excellent and far higher than that of synthetic material masks (<20%).
[0028] (2) High-efficiency preservation and directional anchoring of active ingredients: Compared with the method of simply soaking and loading active ingredients to prepare masks, this invention uses low-temperature extraction combined with atomization anchoring technology to maximize the preservation of the efficacy of heat-sensitive active ingredients (such as crocin and yazolide); the micron-sized droplets formed by atomization deposition can penetrate into the nanofiber network and achieve high-efficiency loading (loading rate increased by 20-30%) through physical adsorption and carrier inclusion (such as β-cyclodextrin).
[0029] (3) Excellent antioxidant properties: The nanofibers have a huge specific surface area (>20m²). 2 The nanofiber mask product prepared by this invention has excellent DPPH free radical scavenging rate and long-lasting and stable antioxidant effect, thanks to its three-dimensional network structure and the DPPH free radical scavenging rate.
[0030] (4) Significant whitening effect: The transdermal permeate collected by the Franz diffusion cell shows that the mask of the present invention achieves efficient transdermal delivery and continuous release of whitening active ingredients, thereby achieving a rapid and long-lasting tyrosinase inhibition effect at the skin target site.
[0031] (5) Ethnic medical aesthetic features and safety: This invention selects ethnic plants with Yunnan plateau characteristics (such as saffron, snow lotus, fire grass, green prickly pear fruit, wild chrysanthemum, aloe vera, Bletilla striata, Panax notoginseng, Artemisia argyi, and purslane). The above plants have not been fully developed by modern cosmetics, and the all-natural ingredient system has excellent biocompatibility. Attached Figure Description
[0032] Figure 1 This is a SEM image of the nanofiber membrane prepared in Example 1 of the present invention.
[0033] Figure 2 The graphs show the DPPH free radical scavenging rates of the nanofiber mask samples prepared in Examples 1-3 and Comparative Examples 1-2 of this invention.
[0034] Figure 3 The graph shows the tyrosinase inhibition rate of the transdermal permeable liquid in nanofiber mask samples prepared in Examples 1-3 and Comparative Examples 1-2 of this invention.
[0035] Figure 4 The soil degradation rate diagrams are for the nanofiber mask samples prepared in Examples 1-3 and Comparative Examples 1-2 of this invention. Detailed Implementation
[0036] To better illustrate the purpose, technical solution, and advantages of this invention, the invention will be further described below with reference to specific embodiments. In the embodiments and comparative examples of this invention, unless otherwise specified, all chemical reagents used were commercially available analytical grade reagents.
[0037] Example 1 A method for preparing a nanofiber facial mask based on plant active ingredients specifically includes the following steps: (1) Preparation of plant active extracts: Dried saffron powder was placed in a solvent prepared by anhydrous ethanol and deionized water in a volume ratio of 1:4. Low-temperature cold maceration extraction combined with ultrasonic-assisted technology was used. The mixture was macerated at 6℃ for 36h to obtain a mixed solution. The amount of saffron powder added to the mixed solution was 0.1g / mL. The mixed solution was then ultrasonicated at 45℃ and 400W for 40min and filtered (the filter residue was discarded). The mixture was then concentrated by thin-film evaporation at 45℃ to 1 / 5 of the original volume of the mixed solution. Then, it was freeze-dried at -50℃ and vacuum degree <10Pa for 24h to obtain saffron extract powder with high activity content. Snow lotus extract powder was prepared by the same method.
[0038] (2) Preparation of natural plant nanofibers: Under pH 11, wood pulp fibers were subjected to 6 cycles of high-pressure homogenization at a pressure of 90 MPa using a high-pressure homogenizer. The temperature was controlled within the range of 25-35℃ using a circulating water cooling system during the entire homogenization process, resulting in a wood pulp nanofiber suspension with an average diameter of 80 nm. The content of wood pulp nanofibers in the suspension was 4% by mass.
[0039] (3) Preparation of nanofiber membrane: Genipin and glycerol were placed in the wood pulp nanofiber suspension obtained in step (2) and dispersed for 25 min at 12000 rpm using a high-speed shear emulsifier to form a uniform spinnable solution. The spinnable solution was electrospun for 10 h at a voltage of 22 kV, a receiving distance of 15 cm, a spinning speed of 1.2 mL / h, an ambient temperature of 25 °C, and a humidity of 45% RH to produce a nanofiber membrane with a thickness of 220 μm.
[0040] (4) Post-treatment: The nanofiber membrane was vacuum dried at 45°C for 7 hours, and then irradiated with low-intensity UVB (280-315nm) for 12 minutes to obtain a nanofiber substrate layer. The nanofiber substrate layer contained 80% wood pulp nanofiber by mass percentage, 13% genipin by mass percentage, and 7% glycerol by mass percentage.
[0041] (5) Active ingredient atomization and anchoring: Using an ultrasonic atomization device, under the conditions of atomization rate of 1 mL / min and droplet size of 20 μm, the active ingredient loading solution prepared by saffron extract, snow lotus extract and β-cyclodextrin was atomized and deposited on the surface of the nanofiber substrate. The loading amount of plant active ingredient layer on the nanofiber substrate was 120 mg / m 2The active ingredient loading solution comprises, by mass percentage: 15% saffron extract, 10% snow lotus extract, 5% β-cyclodextrin, and the balance being deionized water. It is then dried and cured at 30°C to obtain a nanofiber mask based on plant active ingredients.
[0042] The nanofiber mask prepared in this embodiment was subjected to SEM testing, and the test results are as follows: Figure 1 As shown, tests revealed that the fiber diameter distribution is uniform, with an average diameter of approximately 800 nm. The fibers interweave to form a three-dimensional porous network structure with uniform pore distribution and no obvious beading or defects. The DPPH free radical scavenging rate of the nanofiber mask prepared in this embodiment was tested, and the test structure is shown below. Figure 2 As shown, the DPPH free radical scavenging rate of the nanofiber mask in this embodiment was 88.3% as tested. The tyrosinase inhibition rate of the nanofiber mask prepared in this embodiment was tested using a transdermal permeation solution; the test structure is shown below. Figure 3 As shown in the figure, the tyrosinase inhibition rate of the transdermal solution of the nanofiber mask in this embodiment was 87%. The soil degradation rate of the nanofiber mask prepared in this embodiment was tested, and the results are as follows. Figure 4 As shown in the figure, the soil degradation rate of the nanofiber mask prepared in this embodiment was 85% after 28 days, according to the test results. This embodiment solves the problems of poor environmental performance, low active ingredient loading rate and easy inactivation of traditional masks through the synergistic effect of an all-natural base and a mild directional loading process. The low-temperature extraction-atomization anchoring process achieves efficient preservation and precise loading of active ingredients, resulting in a nanofiber mask product with excellent DPPH free radical scavenging rate, long-lasting and stable antioxidant effect, and excellent biodegradability.
[0043] Example 2 A method for preparing a nanofiber facial mask based on plant active ingredients specifically includes the following steps: (1) Preparation of plant active extracts: Dried saffron powder was placed in a solvent prepared by anhydrous ethanol and deionized water in a volume ratio of 1:4. Low-temperature cold maceration extraction combined with ultrasonic-assisted technology was used. The mixture was macerated at 6℃ for 36h to obtain a mixed solution. The amount of saffron powder added to the mixed solution was 0.1g / mL. The mixed solution was then ultrasonicated at 45℃ and 400W for 40min and filtered (the filter residue was discarded). The mixture was then concentrated by thin-film evaporation at 45℃ to 1 / 5 of the original volume of the mixed solution. Then, it was freeze-dried at -50℃ and vacuum degree <10Pa for 24h to obtain saffron extract powder with high activity content. Snow lotus extract powder was prepared by the same method.
[0044] (2) Preparation of natural plant nanofibers: Under pH 11, wood pulp fibers were subjected to 6 cycles of high-pressure homogenization at a pressure of 90 MPa using a high-pressure homogenizer. The temperature was controlled within the range of 25-35℃ using a circulating water cooling system during the entire homogenization process, resulting in a wood pulp nanofiber suspension with an average diameter of 50 nm. The content of wood pulp nanofibers in the suspension was 4% by mass.
[0045] (3) Preparation of nanofiber membrane: Tannic acid and citrate were placed in the wood pulp nanofiber suspension obtained in step (2) and dispersed for 20 min at 15000 rpm using a high-speed shear emulsifier to form a uniform spinnable solution. The spinnable solution was electrospun for 8 h at a voltage of 25 kV, a receiving distance of 12 cm, a spinning speed of 1.5 mL / h, an ambient temperature of 26 ℃, and a humidity of 40% RH to produce a nanofiber membrane with a thickness of 250 μm.
[0046] (4) Post-treatment: The nanofiber membrane was vacuum dried at 45°C for 7 hours, and then irradiated with low-intensity UVB (280-315nm) for 12 minutes to obtain a nanofiber substrate layer. The nanofiber substrate layer contained 79% wood pulp nanofiber by mass percentage, 15% tannic acid by mass percentage, and 6% citrate by mass percentage.
[0047] (5) Active ingredient atomization and anchoring: Using an ultrasonic atomization device, under the conditions of atomization rate of 1 mL / min and droplet size of 20 μm, the active ingredient loading solution prepared by saffron extract, snow lotus extract and β-cyclodextrin was atomized and deposited on the surface of the nanofiber substrate. The loading amount of plant active ingredient layer on the nanofiber substrate was 100 mg / m³. 2 The active ingredient loading solution comprises, by mass percentage: 12% saffron extract, 8% snow lotus extract, 6% β-cyclodextrin, and the balance being deionized water. It is then dried and cured at 30°C to obtain a nanofiber mask based on plant active ingredients.
[0048] The nanofiber mask prepared in this embodiment was subjected to SEM testing. The results showed that the fiber diameter was uniform, the fibers were interwoven to form a three-dimensional porous network structure, the pores were uniformly distributed, and there were no obvious beads or defects. The DPPH free radical scavenging rate of the nanofiber mask prepared in this embodiment was tested, and the test structure is shown below. Figure 2 As shown, tests revealed that the DPPH free radical scavenging rate of the nanofiber mask in this embodiment was 85%. The transdermal tyrosinase inhibition rate of the nanofiber mask prepared in this embodiment was tested, and the test structure is shown below. Figure 3As shown in the figure, the tyrosinase inhibition rate of the transdermal permeable solution of the nanofiber mask in this embodiment was 82%. The soil degradation rate of the nanofiber mask prepared in this embodiment was tested, and the results are as follows. Figure 4 As shown in the figure, the soil degradation rate of the nanofiber mask prepared in this embodiment was 83% after 28 days, according to the test results. This embodiment solves the problems of poor environmental performance, low active ingredient loading rate and easy inactivation of traditional masks through the synergistic effect of an all-natural base and a mild directional loading process. The low-temperature extraction-atomization anchoring process achieves efficient preservation and precise loading of active ingredients, resulting in a nanofiber mask product with excellent DPPH free radical scavenging rate, long-lasting and stable antioxidant effect, and excellent biodegradability.
[0049] Example 3 A method for preparing a nanofiber facial mask based on plant active ingredients specifically includes the following steps: (1) Preparation of plant active extracts: Dried saffron powder was placed in a solvent prepared by anhydrous ethanol and deionized water in a volume ratio of 1:4. Low-temperature cold maceration extraction combined with ultrasonic-assisted technology was used. The mixture was macerated at 6℃ for 36h to obtain a mixed solution. The amount of saffron powder added to the mixed solution was 0.1g / mL. The mixed solution was then ultrasonicated at 45℃ and 400W for 40min and filtered (the filter residue was discarded). The mixture was then concentrated by thin-film evaporation at 45℃ to 1 / 5 of the original volume of the mixed solution. Then, it was freeze-dried at -50℃ and vacuum degree <10Pa for 24h to obtain saffron extract powder with high activity content. Snow lotus extract powder was prepared by the same method.
[0050] (2) Preparation of natural plant nanofibers: Under pH 11, wood pulp fibers were subjected to 6 cycles of high-pressure homogenization at a pressure of 90 MPa using a high-pressure homogenizer. The temperature was controlled within the range of 25-35℃ using a circulating water cooling system during the entire homogenization process, resulting in a wood pulp nanofiber suspension with an average diameter of 100 nm. The content of wood pulp nanofibers in the suspension was 4% by mass.
[0051] (3) Preparation of nanofiber membrane: Genipin and glycerol were placed in the wood pulp nanofiber suspension obtained in step (2) and dispersed for 20 min at 15000 rpm using a high-speed shear emulsifier to form a uniform spinnable solution. The spinnable solution was electrospun for 12 h at a voltage of 18 kV, a receiving distance of 18 cm, a spinning speed of 0.8 mL / h, an ambient temperature of 24 ℃, and a humidity of 50% RH to produce a nanofiber membrane with a thickness of 190 μm.
[0052] (4) Post-treatment: The nanofiber membrane was vacuum dried at 45°C for 7 h, and then irradiated with low-intensity UVB (280-315 nm) for 12 min to obtain a nanofiber substrate layer. The nanofiber substrate layer contained 75% wood pulp nanofiber by mass percentage, 15% genipin by mass percentage, and 10% glycerol by mass percentage.
[0053] (5) Active ingredient atomization and anchoring: Using an ultrasonic atomization device, under the conditions of atomization rate of 0.5 mL / min and droplet size of 50 μm, the active ingredient loading solution prepared by saffron extract, snow lotus extract and β-cyclodextrin was atomized and deposited on the surface of the nanofiber substrate. The loading amount of plant active ingredient layer on the nanofiber substrate was 100 mg / m 2 The active ingredient loading solution comprises, by mass percentage: 20% saffron extract, 5% snow lotus extract, 3% β-cyclodextrin, and the balance being deionized water. It is then dried and cured at 25°C to obtain a nanofiber mask based on plant active ingredients.
[0054] The nanofiber mask prepared in this embodiment was subjected to SEM testing. The results showed that the fiber diameter was uniform, the fibers were interwoven to form a three-dimensional porous network structure, the pores were uniformly distributed, and there were no obvious beads or defects. The DPPH free radical scavenging rate of the nanofiber mask prepared in this embodiment was tested, and the test structure is shown below. Figure 2 As shown, tests revealed that the DPPH free radical scavenging rate of the nanofiber mask in this embodiment was 83%. The transdermal tyrosinase inhibition rate of the nanofiber mask prepared in this embodiment was tested, and the test structure is shown below. Figure 3 As shown in the figure, the test results showed that the tyrosinase inhibition rate of the transdermal permeable solution of the nanofiber mask in this embodiment was 80%. The soil degradation rate of the nanofiber mask prepared in this embodiment was tested, and the results are as follows. Figure 4 As shown in the figure, the soil degradation rate of the nanofiber mask prepared in this embodiment was 76% after 28 days, according to the test results. This embodiment solves the problems of poor environmental performance, low active ingredient loading rate and easy inactivation of traditional masks through the synergistic effect of an all-natural base and a mild directional loading process. The low-temperature extraction-atomization anchoring process achieves efficient preservation and precise loading of active ingredients, resulting in a nanofiber mask product with excellent DPPH free radical scavenging rate, long-lasting and stable antioxidant effect, and excellent biodegradability.
[0055] Example 4 A method for preparing a nanofiber facial mask based on plant active ingredients specifically includes the following steps: (1) Preparation of plant active extracts: Dried saffron powder was placed in a solvent prepared by anhydrous ethanol and deionized water in a volume ratio of 1:5. Low-temperature cold maceration extraction combined with ultrasonic-assisted technology was used. The mixture was macerated at 4℃ for 24h to obtain a mixed solution. The amount of saffron powder added to the mixed solution was 0.0667g / mL. The mixed solution was then ultrasonicated at 40℃ and 500W for 45min and filtered (the filter residue was discarded). The solution was then concentrated by thin-film evaporation at 45℃ to 1 / 5 of the original volume of the mixed solution. Finally, it was freeze-dried at -50℃ and vacuum degree <10Pa for 24h to obtain saffron extract powder with high activity content. Snow lotus extract powder was prepared by the same method.
[0056] (2) Preparation of natural plant nanofibers: Under the condition of pH 12, wood pulp fibers were subjected to 8 cycles of high-pressure homogenization at a pressure of 80 MPa using a high-pressure homogenizer. The temperature was controlled within the range of 25-35℃ by a circulating water cooling system during the entire homogenization process, resulting in a wood pulp nanofiber suspension with an average diameter of 100 nm. The content of wood pulp nanofibers in the suspension was 3% by mass.
[0057] (3) Preparation of nanofiber membrane: Genipin and glycerol were placed in the wood pulp nanofiber suspension obtained in step (2) and dispersed for 30 min at 10,000 rpm using a high-speed shear emulsifier to form a uniform spinnable solution. The spinnable solution was electrospun for 12 h at a voltage of 18 kV, a receiving distance of 18 cm, a spinning speed of 0.8 mL / h, an ambient temperature of 28 °C, and a humidity of 50% RH to produce a nanofiber membrane with a thickness of 190 μm.
[0058] (4) Post-treatment: The nanofiber membrane was vacuum dried at 42°C for 6 hours, and then irradiated with low-intensity UVB (280-315nm) for 15 minutes to obtain a nanofiber substrate layer. The nanofiber substrate layer contained 80% wood pulp nanofiber by mass percentage, 10% genipin by mass percentage, and 10% glycerol by mass percentage.
[0059] (5) Active ingredient atomization and anchoring: Using an ultrasonic atomization device, under the conditions of an atomization rate of 2 mL / min and a droplet size of 50 μm, the active ingredient loading solution prepared by snow lotus extract, saffron extract and β-cyclodextrin was atomized and deposited on the surface of the nanofiber substrate. The loading amount of the plant active ingredient layer on the nanofiber substrate was 50 mg / m³. 2The active ingredient loading solution comprises, by mass percentage: 15% saffron extract, 15% snow lotus extract, 2% β-cyclodextrin, and the balance being deionized water. It is then dried and cured at 25°C to obtain a nanofiber mask based on plant active ingredients.
[0060] SEM testing was performed on the nanofiber mask prepared in this embodiment. The results showed that the fiber diameter was uniform, the fibers were interwoven to form a three-dimensional porous network structure, the pores were uniformly distributed, and there were no obvious beads or defects. The DPPH free radical scavenging rate of the nanofiber mask prepared in this embodiment was tested, and the results showed that the DPPH free radical scavenging rate was 85%. The tyrosinase inhibition rate of the transdermal permeable solution of the nanofiber mask prepared in this embodiment was tested, and the results showed that the tyrosinase inhibition rate of the transdermal permeable solution of the nanofiber mask prepared in this embodiment was 80%. The soil degradation rate of the nanofiber mask prepared in this embodiment was tested, and the results showed that the soil degradation rate of the nanofiber mask prepared in this embodiment was 80% after 28 days. This embodiment solves the problems of poor environmental friendliness, low active ingredient loading rate and easy inactivation of traditional masks by synergistic effect of all-natural base and mild directional loading process. The low temperature extraction-atomization anchoring process realizes efficient preservation and precise loading of active ingredients, so that the prepared nanofiber mask product has excellent DPPH free radical scavenging rate, long-lasting and stable antioxidant effect and excellent biodegradability.
[0061] Example 5 A method for preparing a nanofiber facial mask based on plant active ingredients specifically includes the following steps: (1) Preparation of plant active extracts: Dried saffron powder was placed in a solvent prepared by anhydrous ethanol and deionized water in a volume ratio of 1:3. Low-temperature cold maceration extraction combined with ultrasonic-assisted technology was used. The mixture was macerated at 8°C for 48 h to obtain a mixed solution. The amount of saffron powder added to the mixed solution was 0.125 g / mL. The mixed solution was then ultrasonicated at 50°C and 300 W for 30 min and filtered (the filter residue was discarded). The solution was then concentrated by thin-film evaporation at 45°C to 1 / 5 of the original volume of the mixed solution. Finally, it was freeze-dried at -50°C and vacuum degree <10 Pa for 24 h to obtain saffron extract powder with high activity content. Snow lotus extract powder was prepared by the same method.
[0062] (2) Preparation of natural plant nanofibers: Under pH 10, wood pulp fibers were subjected to five cycles of high-pressure homogenization at a pressure of 100 MPa using a high-pressure homogenizer. The temperature was controlled within the range of 25-35℃ using a circulating water cooling system during the entire homogenization process, resulting in a wood pulp nanofiber suspension with an average diameter of 100 nm. The content of wood pulp nanofibers in the suspension was 5% by mass.
[0063] (3) Preparation of nanofiber membrane: Tannic acid and citrate were placed in the wood pulp nanofiber suspension obtained in step (2) and dispersed for 30 min at 10,000 rpm using a high-speed shear emulsifier to form a uniform spinnable solution. The spinnable solution was electrospun for 12 h at a voltage of 18 kV, a receiving distance of 18 cm, a spinning speed of 0.8 mL / h, an ambient temperature of 22 °C, and a humidity of 50% RH to produce a nanofiber membrane with a thickness of 190 μm.
[0064] (4) Post-treatment: The nanofiber membrane was vacuum dried at 40°C for 8 hours, and then irradiated with low-intensity UVB (280-315nm) for 10 minutes to obtain a nanofiber substrate layer. The nanofiber substrate layer contained 80% wood pulp nanofiber by mass percentage, 12% genipin by mass percentage, and 8% glycerol by mass percentage.
[0065] (5) Active ingredient atomization and anchoring: Using an ultrasonic atomization device, under the conditions of atomization rate of 2 mL / min and droplet size of 10 μm, the active ingredient loading solution prepared by saffron extract, snow lotus extract and β-cyclodextrin was atomized and deposited on the surface of the nanofiber substrate. The loading amount of plant active ingredient layer on the nanofiber substrate was 200 mg / m³. 2 The active ingredient loading solution comprises, by mass percentage: 5% saffron extract, 5% snow lotus extract, 8% β-cyclodextrin, and the balance being deionized water. It is then dried and cured at 28°C to obtain a nanofiber mask based on plant active ingredients.
[0066] SEM testing was performed on the nanofiber mask prepared in this embodiment. The results showed that the fiber diameter was uniformly distributed, the fibers were interwoven to form a three-dimensional porous network structure, the pores were uniformly distributed, and there were no obvious beads or defects. The DPPH free radical scavenging rate of the nanofiber mask prepared in this embodiment was tested, and the results showed that the DPPH free radical scavenging rate was 80%. The tyrosinase inhibition rate of the transdermal permeable solution of the nanofiber mask prepared in this embodiment was tested, and the results showed that the tyrosinase inhibition rate of the transdermal permeable solution of the nanofiber mask prepared in this embodiment was 75%. The soil degradation rate of the nanofiber mask prepared in this embodiment was tested, and the results showed that the soil degradation rate of the nanofiber mask prepared in this embodiment was 75% after 28 days. This embodiment solves the problems of poor environmental friendliness, low active ingredient loading rate and easy inactivation of traditional masks by synergistic effect of all-natural base and mild directional loading process. The low temperature extraction-atomization anchoring process realizes efficient preservation and precise loading of active ingredients, so that the prepared nanofiber mask product has excellent DPPH free radical scavenging rate, long-lasting and stable antioxidant effect and excellent biodegradability.
[0067] Comparative Example 1 A method for preparing a nanofiber facial mask based on plant active ingredients specifically includes the following steps: (1) Preparation of plant active extracts: Dried saffron powder was placed in a solvent prepared by anhydrous ethanol and deionized water in a volume ratio of 1:4. Low-temperature cold maceration extraction combined with ultrasonic-assisted technology was used. The mixture was macerated at 6℃ for 36h to obtain a mixed solution. The amount of saffron powder added to the mixed solution was 0.1g / mL. The mixed solution was then ultrasonicated at 45℃ and 400W for 40min and filtered (the filter residue was discarded). The mixture was then concentrated by thin-film evaporation at 45℃ to 1 / 5 of the original volume of the mixed solution. Then, it was freeze-dried at -50℃ and vacuum degree <10Pa for 24h to obtain saffron extract powder with high activity content. Snow lotus extract powder was prepared by the same method.
[0068] (2) Preparation of natural plant nanofibers: Under pH 11, wood pulp fibers were subjected to 6 cycles of high-pressure homogenization at a pressure of 90 MPa using a high-pressure homogenizer. The temperature was controlled within the range of 25-35℃ using a circulating water cooling system during the entire homogenization process, resulting in a wood pulp nanofiber suspension with an average diameter of 80 nm. The content of wood pulp nanofibers in the suspension was 4% by mass.
[0069] (3) Preparation of nanofiber membrane: Genipin and glycerol were placed in the wood pulp nanofiber suspension obtained in step (2) and dispersed for 25 min at 12000 rpm using a high-speed shear emulsifier to form a uniform spinnable solution. The spinnable solution was electrospun for 10 h at a voltage of 22 kV, a receiving distance of 15 cm, a spinning speed of 1.2 mL / h, an ambient temperature of 25 °C, and a humidity of 45% RH to produce a nanofiber membrane with a thickness of 220 μm.
[0070] (4) Post-treatment: The nanofiber membrane was vacuum dried at 45°C for 7 hours, and then irradiated with low-intensity UVB (280-315nm) for 12 minutes to obtain a nanofiber substrate layer. The nanofiber substrate layer contained 80% wood pulp nanofiber by mass percentage, 13% genipin by mass percentage, and 7% glycerol by mass percentage.
[0071] (5) Active ingredient immersion loading: The nanofiber substrate was immersed in an active ingredient loading solution prepared from saffron extract, snow lotus extract and β-cyclodextrin for 30 min. The loading amount of plant active ingredients on the nanofiber substrate was 40 mg / m³. 2 The active ingredient loading solution comprises, by mass percentage: 15% saffron extract, 10% snow lotus extract, 5% β-cyclodextrin, and the balance being deionized water. It is then dried and cured at 30°C to obtain a nanofiber mask based on plant active ingredients.
[0072] SEM analysis was performed on the nanofiber mask prepared in this comparative example. The results showed that the nanofiber mask had a uniform fiber diameter distribution, and the fibers were interwoven to form a three-dimensional porous network structure with uniform pore distribution. The DPPH free radical scavenging rate of the nanofiber mask prepared in this comparative example was tested, and the test structure is shown below. Figure 2 As shown in the figure, the DPPH free radical scavenging rate of the nanofiber mask in this comparative example was found to be 70%. The tyrosinase inhibition rate of the nanofiber mask prepared in this comparative example was tested using a transdermal permeation solution. The test structure is shown in the figure. Figure 3 As shown in the figure, the tyrosinase inhibition rate of the transdermal solution of the nanofiber mask in this comparative example was 74%. Soil degradation rate testing was conducted on the nanofiber mask prepared in this comparative example, and the results are as follows. Figure 4 As shown in the figure, the soil degradation rate of the nanofiber mask prepared in this comparative example was 73% after 28 days. This indicates that the degradation performance mainly depends on the substrate material, but the overall lag in its functional indicators proves that the soaking method has a fundamental defect in terms of efficient loading and retention of active ingredients.
[0073] Comparative Example 2 A method for preparing a nanofiber facial mask based on plant active ingredients specifically includes the following steps: (1) Preparation of plant active extracts: Dried saffron powder was placed in a solvent prepared by anhydrous ethanol and deionized water in a volume ratio of 1:4. Low-temperature cold maceration extraction combined with ultrasonic-assisted technology was used. The mixture was macerated at 6℃ for 36h to obtain a mixed solution. The amount of saffron powder added to the mixed solution was 0.1g / mL. The mixed solution was then ultrasonicated at 45℃ and 400W for 40min and filtered (the filter residue was discarded). The mixture was then concentrated by thin-film evaporation at 45℃ to 1 / 5 of the original volume of the mixed solution. Then, it was freeze-dried at -50℃ and vacuum degree <10Pa for 24h to obtain saffron extract powder with high activity content. Snow lotus extract powder was prepared by the same method.
[0074] (2) Preparation of nanofiber membrane: Polyimide was placed in N,N-dimethylacetamide and dispersed for 25 min at 12000 rpm using a high-speed shear emulsifier to form a uniform spinnable solution. The spinnable solution was electrospun for 10 h at a voltage of 22 kV, a receiving distance of 15 cm, a spinning speed of 1.2 mL / h, an ambient temperature of 25 °C, and a humidity of 45% RH to produce a nanofiber membrane with a thickness of 220 μm.
[0075] (3) Post-treatment: The nanofiber membrane was vacuum dried at 45°C for 7 hours, and then irradiated with low-intensity UVB (280-315nm) for 12 minutes to obtain a nanofiber substrate layer. The polyimide content in the nanofiber substrate layer was 100% by mass percentage.
[0076] (4) Active ingredient atomization and anchoring: Using an ultrasonic atomization device, under the conditions of atomization rate of 1 mL / min and droplet size of 20 μm, the active ingredient loading solution prepared by saffron extract, snow lotus extract and β-cyclodextrin was atomized and deposited on the surface of the nanofiber substrate. The loading amount of plant active ingredient layer on the nanofiber substrate was 120 mg / m 2 The active ingredient loading solution comprises, by mass percentage: 15% saffron extract, 10% snow lotus extract, 5% β-cyclodextrin, and the balance being deionized water. It is then dried and cured at 30°C to obtain a nanofiber mask based on plant active ingredients.
[0077] SEM analysis was performed on the nanofiber mask prepared in this comparative example. The results showed that the nanofiber mask prepared in this comparative example had a uniform fiber diameter distribution, and the fibers were interwoven to form a three-dimensional porous network structure with uniform pore distribution. The DPPH free radical scavenging rate of the nanofiber mask prepared in this comparative example was tested, and the test structure is shown below. Figure 2As shown in the figure, the DPPH free radical scavenging rate of the nanofiber mask prepared in this comparative example was 78%, but it dropped sharply to 52% after 24 hours, indicating that the synthetic substrate is not conducive to the stable and sustained release of active ingredients. The transdermal tyrosinase inhibition rate of the nanofiber mask prepared in this comparative example was tested, and the test structure is shown in the figure. Figure 3 As shown in the figure, the tyrosinase inhibition rate of the transdermal solution of the nanofiber mask in this comparative example was 77%. Soil degradation rate testing was conducted on the nanofiber mask prepared in this comparative example, and the results are as follows. Figure 4 As shown, tests revealed that the nanofiber mask prepared in this comparative example had a soil degradation rate of 47% after 28 days. This contrasts sharply with the degradation rate of the all-natural substrate of this invention, fully revealing the serious shortcomings of synthetic materials in terms of environmental friendliness.
[0078] Test results show that: (1) Influence of process parameters: Under different process parameters (Examples 1-5), the core properties of the prepared masks (antioxidant, whitening, degradation and loading rate) remained excellent and stable, which proved the robustness of the process of the present invention.
[0079] (2) Common advantages of the present invention: All embodiments are significantly better than the comparative examples in terms of product performance, which fully verifies the advanced nature and effectiveness of the core invention concept of "all-natural nanofiber substrate + atomization anchoring", regardless of minor changes in specific process parameters.
[0080] (3) Deficiencies of traditional soaking method: Comparative Example 1 (soaking method) lagged far behind in all functional indicators (DPPH scavenging rate, tyrosinase inhibition rate, loading rate), proving the key role of the "atomization anchoring" process of the present invention in efficient loading and maintaining activity.
[0081] (4) Limitations of synthetic substrate: Although the loading rate and dry strength of Comparative Example 2 (polyimide substrate) are acceptable, the functionality (antioxidant, whitening) and environmental friendliness of the final product are far inferior to the all-natural substrate of this invention due to the bioinertness and non-degradability of the substrate.
[0082] The various embodiments of the present invention have been described above. These descriptions are exemplary and not exhaustive, nor are they limited to the disclosed embodiments. Many modifications and variations will be apparent to those skilled in the art without departing from the scope and spirit of the described embodiments. The terminology used herein is chosen to best explain the principles, practical application, or improvement of the technology in the market, or to enable others skilled in the art to understand the embodiments disclosed herein.
Claims
1. A nanofiber mask based on plant active ingredients, characterized in that, The nanofiber mask is composed of a plant active ingredient layer atomized and deposited to anchor on a nanofiber base layer; the composition of the plant active ingredient layer includes, in mass percentage: 10-30% of a plant active extract, 2-8% of a natural carrier, and the balance of water; the composition of the nanofiber base layer includes, in mass percentage: 50-80% of a natural plant nanofiber, 5-15% of a natural crosslinking agent, and 3-10% of a natural plasticizer; the loading amount of the plant active ingredient layer on the nanofiber base layer is 50-200 mg / m 2 .
2. The nanofiber mask based on plant active ingredients according to claim 1, characterized in that, The plant active extract is a combination of two or more of the following: saffron extract, snow lotus extract, fireweed extract, green prickly pear fruit extract, wild chrysanthemum extract, aloe vera extract, bletilla extract, notoginseng extract, artemisia extract, and purslane extract; the natural plant nanofiber is a cellulose nanofiber obtained by mechanical nano-sizing of wood pulp fiber, cotton fiber, or bamboo fiber, with a diameter of 50-100 nm.
3. The nanofiber mask based on plant active ingredients according to claim 1, characterized in that, The atomization deposition employs ultrasonic atomization or high-pressure micro-mist technology, with atomized droplet particle size of 10-50 μm; the natural carrier is β-cyclodextrin; the natural crosslinking agent is either genipin or tannic acid; and the natural plasticizer is either glycerol or citrate.
4. The method for preparing a nanofiber mask based on a plant active ingredient according to claim 1, characterized by, Specifically, the following steps are included: (1) Preparation of plant active extracts: Plant powder is placed in a solvent and cold soaked to obtain a mixture. The mixture is then subjected to ultrasonication, filtration, evaporation and concentration, and freeze drying to obtain plant active extract powder. (2) Preparation of natural plant nanofibers: Wood pulp fiber, cotton fiber or bamboo fiber is subjected to cyclic high-pressure homogenization under alkaline conditions to obtain a natural plant nanofiber suspension. (3) Preparation of nanofiber substrate: Natural crosslinking agent and natural plasticizer are placed in natural plant nanofiber suspension and dispersed to form a spinnable solution. The spinnable solution is electrospun to make nanofiber membrane. (4) Post-processing: The nanofiber membrane is vacuum dried and then cross-linked by ultraviolet irradiation to obtain the nanofiber substrate layer; (5) Active ingredient atomization and anchoring: The active ingredient loading solution is atomized and deposited on the surface of the nanofiber substrate using atomization deposition technology, and then dried and cured to obtain a nanofiber mask based on plant active ingredients.
5. The method for preparing a nanofiber facial mask based on plant active ingredients according to claim 4, characterized in that, In step (1), the solvent is prepared by mixing anhydrous ethanol and water in a volume ratio of 1:(3-5); the cold soaking conditions are: cold soaking at 4-8℃ for 24-48h; the amount of plant powder added to the mixture is 0.0667-0.125g / mL; the ultrasonic conditions are: ultrasonic treatment at a power of 300-500W and a temperature of 40-50℃ for 30-45min.
6. The method for preparing a nanofiber facial mask based on plant active ingredients according to claim 4, characterized in that, The conditions for the cyclic high-pressure homogenization treatment in step (2) are: homogenization and cyclic treatment for 5-8 times under a pressure of 80-100MPa; the content of natural plant nanofibers in the natural plant nanofiber suspension is 3-5% by mass percentage.
7. The method for preparing a nanofiber facial mask based on plant active ingredients according to claim 4, characterized in that, The dispersion conditions in step (3) are: dispersion for 20-30 minutes at a rotation speed of 10000-15000 rpm; the electrospinning conditions are: spinning for 8-12 hours at a voltage of 18-25 kV, a receiving distance of 12-18 cm, a spinning speed of 0.8-1.5 mL / h, an ambient temperature of 22-28℃, and an ambient relative humidity of 40-50%.
8. The method for preparing a nanofiber facial mask based on plant active ingredients according to claim 4, characterized in that, The conditions for vacuum drying in step (4) are: vacuum drying at 40-45℃ for 6-8 hours; and the time for ultraviolet irradiation crosslinking is 10-15 minutes.
9. The method for preparing a nanofiber facial mask based on plant active ingredients according to claim 4, characterized in that, In step (5), when ultrasonic atomization is used for atomization deposition, the atomization rate is 0.5-2 mL / min; the drying and curing temperature is 25-30℃; and the active ingredient loading solution is an aqueous solution of plant active extract powder and natural carrier.
10. The application of the plant-based active ingredient-based nanofiber mask as described in claim 1 in the field of medical aesthetics and cosmetics.